Processes for producing anti-inflammatory, antibacterial, antifungal, and bactericidal materials

Abstract

Provided herein are methods for preparing metal matrix composites by a deposition process. The metal matrix composites described herein are useful for anti-inflammatory, antibacterial, antifungal, and antiseptic applications.

Description

[Technical Field]

[0001] Cross-referencing of related technologies This application claims the benefits of U.S. Provisional Patent Application No. 63 / 006,044, filed on April 6, 2020, which is incorporated herein by reference in its entirety. [Overview of the Initiative]

[0002] This specification describes a method for preparing various metal matrix composite materials, the method comprising the step of depositing one or more metals and metal oxides from a source onto a substrate in a deposition chamber in the presence of water vapor and one or more gases including oxygen gas, wherein the said source is located at a distance of at least 5 cm from the substrate, and further the method involves maintaining an internal pressure of about 10 before and / or during deposition in the deposition chamber. -7 It does not include a step that drops below Torrell. In some embodiments, the base pressure during this deposition is about 10 -7 It is above 10. In some embodiments, this method raises the internal pressure of the deposit chamber to approximately 10 within 24 hours, 12 hours, 6 hours, and 3 hours before deposit. -7 The process does not involve dropping below the Torrell. In some embodiments, one or more gases further include inert gases. In some embodiments, liquid water is injected into an inert gas stream outside the deposit chamber and enters the deposit chamber as water vapor. In some embodiments, the oxygen gas includes molecular oxygen gas. In some embodiments, the molecular oxygen gas includes any form of molecular oxygen gas. In some embodiments, the molecular oxygen gas is O2, O3, O3 + , O2 + , O2 - , O3, O, O + , O -The group consists of ionized ozone, metastable excited oxygen, free electrons, H2O2, and OH. In some embodiments, liquid water is injected into the inert gas stream upstream of the inert gas mass flow controller. In some embodiments, the inert gas is present at a concentration of about 80% to about 100%, the oxygen gas at a concentration of about 1% to about 10%, and the water vapor at a concentration of about 1% to about 15% of the total molar composition of one or more gases. In some embodiments, the inert gas is present at a concentration of about 92% to about 94%, the oxygen gas at a concentration of about 3% to about 5%, and the water vapor at a concentration of about 2% to about 3% of the total molar composition of one or more gases. In some embodiments, the inert gas is present at a concentration of about 92.95%, the oxygen gas at a concentration of about 4.25%, and the water vapor at a concentration of about 2.8% of the total molar composition of one or more gases. In some embodiments, liquid water is injected into the inert gas stream by a syringe pump. In some embodiments, liquid water is injected into the inert gas stream by a syringe pump at a flow rate between approximately 0.5 μl / min and approximately 11 μl / min. In some embodiments, liquid water is injected into the inert gas stream by a syringe pump at a flow rate between approximately 7 μl / min and approximately 10 μl / min. In some embodiments, liquid water is injected into the inert gas stream by a syringe pump at a flow rate between approximately 9 μl / min. In some embodiments, liquid water is injected into the inert gas stream upstream of the inert gas mass flow controller. In some embodiments, liquid water is injected into the inert gas stream downstream of the inert gas mass flow controller when its composition exceeds 1.02% of the total composition. In some embodiments, vapor is injected directly into the deposit chamber. In some embodiments, the inert gas mass flow controller controls the flow rate of inert gas entering the deposit chamber between approximately 100 SCCM and approximately 600 SCCM. In some embodiments, an inert gas mass flow controller controls the flow rate of inert gas entering the loading chamber between approximately 350 SCCM and approximately 450 SCCM. In some embodiments, an oxygen gas mass flow controller controls the flow rate of oxygen gas entering the loading chamber between approximately 0.1 SCCM and approximately 100 SCCM.In some embodiments, the mass flow controller for oxygen gas controls the flow rate of the oxygen gas entering the deposition chamber to be between about 1 SCCM and about 20 SCCM. In some embodiments, the mass flow controller for oxygen gas controls the flow rate of the oxygen gas entering the deposition chamber to be between about 5 SCCM and about 10 SCCM. In some embodiments, the mass flow controller for oxygen gas controls the flow rate of the oxygen gas entering the deposition chamber to be about 8 SCCM. In some embodiments, the liquid water is heated to a temperature between about 20 °C and about 80 °C in the region between the syringe pump and the mass flow controller. In some embodiments, the liquid water is heated to a temperature between about 40 °C and about 60 °C in the region between the syringe pump and the mass flow controller. In some embodiments, the liquid water is heated to a temperature of about 50 °C in the region between the syringe pump and the mass flow controller. In some embodiments, the above distance is between about 1 cm and about 20 cm. In some embodiments, the above distance is between about 5 cm and about 15 cm. In some embodiments, the above distance is about 10 cm. In some embodiments, the above method is to control the internal pressure of the deposition chamber to be about 10. -7 , 10 -6 , 10 -5 , 10 -4 , 10 -3The process does not involve steps that reduce the pressure to below 0.01, 0.1, 1, 10, 100, 760 Torr, or atmospheric pressure. In some embodiments, the metal is a noble metal. In some embodiments, the noble metal is silver, gold, platinum, palladium, or a combination thereof. In some embodiments, the method includes the step of depositing at least two metals onto a substrate. In some embodiments, the at least two metals include silver and gold. In some embodiments, the at least two metals include silver and gold, with silver present at 65% and gold at 35%. In some embodiments, the at least two metals include silver and gold, with silver present at 35% and gold at 65%. In some embodiments, the method further includes the step of depositing additional metal or metal oxide onto the substrate. In some embodiments, the inert gas is argon. In some embodiments, the internal pressure of the deposit chamber during deposition is maintained between about 5 milliliters and about 50 milliliters. In some embodiments, the internal pressure of the deposit chamber during deposition is maintained between about 35 milliliters and about 45 milliliters. In some embodiments, the internal pressure of the deposition chamber during deposition is maintained at approximately 40 milliliters. In some embodiments, the substrate is solid. In some embodiments, the solid includes metal foil, glass, or silicon. In some embodiments, the substrate exhibits low gas emission. In some embodiments, the substrate is an implant. In some embodiments, the implant is a stent. In some embodiments, the stent is a metal stent. In some embodiments, the substrate includes a polymer. In some embodiments, the polymer is high-density polyethylene. In some embodiments, the substrate includes a mesh structure made from high-density polyethylene. In some embodiments, the bandage includes a mesh structure made from high-density polyethylene. In some embodiments, the bandage includes an absorbent layer between two of the mesh structures made from high-density polyethylene. In some embodiments, deposition includes sputtering. In some embodiments, sputtering includes DC magnetron sputtering. In some embodiments, the sputtering power is approximately 190 watts to approximately 950 watts.In some embodiments, the sputtering power is approximately 380 watts to approximately 760 watts. In some embodiments, the sputtering power is approximately 570 watts to approximately 684 watts. In some embodiments, the sputtering power density is approximately 0.7 watts / cm². 2 ~Approximately 3.3 watts / cm² 2 It is between approximately 1.3 and 2.7 watts / cm². In some embodiments, the sputtering power density is approximately 1.3 to 2.7 watts / cm². 2 In some embodiments, the sputtering power density is approximately 2.0 to approximately 2.4 watts / cm². 2 In some embodiments, the sputtering power density is approximately 2.4 watts / cm³. 2 In some embodiments, the inert gas is present at a concentration of approximately 95-96%, the oxygen gas at a concentration of approximately 1-4.5%, the water vapor at a concentration of approximately 2.8%, and the sputtering power density is approximately 2.4 W / cm². 2 In some embodiments, the metal matrix composite material is exposed to a carbon dioxide environment of at least 200 ppm after deposition.

[0003] This specification describes a method for preparing a metal matrix composite material, the method comprising the step of depositing one or more metals and metal oxides onto a substrate in a deposition chamber in the presence of one or more gases including oxygen gas, the method wherein the internal pressure of the deposition chamber is set to about 10 before and / or during deposition. -7 It does not include any processes that reduce the torque below a certain level.

[0004] This specification describes various metal matrix composite materials comprising metal intergrain atoms, metal oxides, and metal crystal grains, wherein the median diameter of the crystal grains is between approximately 2 nm and approximately 15 nm, and the intergrain atoms constitute approximately 50 to approximately 20% of the unit surface area of ​​the metal matrix composite material. In some embodiments, the composite material comprises metal intergrain atoms, metal oxides, oxygen, water, and metal crystal grains, wherein the median diameter of the crystal grains is between approximately 2 nm and approximately 15 nm, the intergrain atoms constitute approximately 50 to approximately 20% of the unit surface area of ​​the metal matrix composite material, and the oxygen constitutes at least 2% by weight of the metal matrix composite material. In some embodiments, the composite material comprises metal intergrain atoms, metal oxides, oxygen, water, and metal crystal grains, wherein the median diameter of the crystal grains is between approximately 2 nm and approximately 15 nm, the intergrain atoms constitute approximately 50 to approximately 20% of the unit surface area of ​​the metal matrix composite material, and the water constitutes less than 4% by weight of the metal matrix composite material. In some embodiments, the median diameter of the crystal grains is between approximately 2 nm and approximately 15 nm, and the metal grain boundary atoms comprise between approximately 50% and approximately 20% of the unit surface area of ​​the metal matrix composite. In some embodiments, the median diameter of the crystal grains is between approximately 5 nm and approximately 15 nm, and the metal grain boundary atoms comprise between approximately 40% and approximately 20% of the unit surface area of ​​the metal matrix composite. In some embodiments, there are second metal grain boundary atoms and second metal crystal grains with a median diameter between approximately 2 nm and approximately 15 nm, and the second metal grain boundary atoms comprise between approximately 50% and approximately 20% of the unit surface area of ​​the metal matrix composite. In some embodiments, the metal matrix composite contains Ag2CO3.

[0005] This specification describes various methods for preparing metal matrix composite materials, which include the step of depositing one or more metals and metal oxides onto a substrate in a deposition chamber in the presence of water vapor and one or more gases including oxygen gas, wherein the deposition of at least one metal and metal oxide is produced from a source at a distance of at least 5 cm from the substrate, and further, the method involves bringing the internal pressure of the deposition chamber to approximately 10°C within 24, 12, 6, and 3 hours prior to deposition. -7 It does not include any processes that reduce the torque below a certain level.

[0006] This specification describes various metal matrix composite materials comprising metal grain boundary atoms, metal oxides, oxygen, water, and metal crystal grains with a median diameter between approximately 2 nm and 15 nm, wherein the grain boundary atoms constitute approximately 50 to 20% of the unit surface area of ​​the metal matrix composite material, and the metal matrix composite material is prepared by a method comprising the step of depositing one or more metals and metal oxides on a substrate in a deposition chamber in the presence of water vapor and one or more gases including oxygen gas, wherein the deposition of at least one metal and metal oxide originates from a source at a distance of at least 5 cm from the substrate, and furthermore, this method involves adjusting the internal pressure of the deposition chamber to approximately 10 within 24 hours, 12 hours, 6 hours, and 3 hours prior to deposition. -7 The process does not involve dropping below Torr. In some embodiments, the internal pressure of the deposit chamber during deposit is maintained between about 5 milliliters and about 50 milliliters. In some embodiments, the internal pressure of the deposit chamber during deposit is maintained between about 35 milliliters and about 45 milliliters. In some embodiments, the internal pressure of the deposit chamber during deposit is maintained at about 40 milliliters. In some embodiments, the oxygen gas includes molecular oxygen gas. In some embodiments, the molecular oxygen gas includes any form of molecular oxygen gas. In some embodiments, the molecular oxygen gas is O2, O3, O3 + , O2 + , O2 - , O3, O, O + , O - The group is selected from ionized ozone, metastable excited oxygen, free electrons, H2O2, and OH.

[0007] Citation by reference All publications, patents, and patent applications referenced herein are cited by reference to the same extent as individual publications, patents, or patent applications are specifically and individually cited. [Brief explanation of the drawing]

[0008] Novel features of the present invention are described in detail in the appended claims. The features and advantages of the present invention will be better understood by referring to the following detailed description and accompanying drawings, which describe exemplary embodiments in which the principles of the present invention are utilized.

[0009] [Figure 1] This figure shows a bandage made from two mesh layers surrounding an absorbent layer. The mesh layers are covered with a metal matrix composite. The bandage is integrally bonded by ultrasonic welding. [Figure 2A] This figure shows the effect of water added to argon working gas on ammonium hydroxide-soluble silver and sputtering power of 684 watts (1.8 amperes at 380 volts). [Figure 2B] This figure shows the performance of an antimicrobial assay. [Figure 3A] This figure shows the effect of water added to argon working gas on ammonium hydroxide-soluble silver and sputtering power of 571 watts (1.5 amperes at 380 volts). [Figure 3B] This figure shows the effect of water added to argon working gas on the antibacterial activity of a silver thin film. [Figure 4] This figure shows the effect of adding various concentrations of water and 2% oxygen to argon working gas on the amount of ammonium-soluble silver produced. [Figure 5A] This figure shows the effect of water and oxygen added to argon working gas on ammonium hydroxide-soluble Ag and sputtering power of 571 watts (1.5 amperes at 380 volts). [Figure 5B] This figure shows the performance of an antimicrobial assay. [Figure 6A] This figure shows the effect of water added to argon working gas on the antibacterial activity of a metal matrix composite composed of an alloy in which 35% silver and 65% gold are deposited on oxygen-free argon, at various flow rates of liquid water. [Figure 6B] This figure shows the effect of water added to argon working gas on the antimicrobial activity of a metal matrix composite composed of an alloy in which 35% silver and 65% gold are deposited in oxygen at various concentrations, with and without water. [Figure 7A] This figure shows the results for materials using the aqueous sputtering process described herein. All of these materials were observed to reduce erythema considerably more rapidly than Acticoat bandages, as shown in Figure 7A. Similar results were observed for edema, as shown in Figure 7B. [Figure 7B] This figure shows the results for materials using the aqueous sputtering process described herein. All of these materials were observed to reduce erythema considerably more rapidly than Acticoat bandages, as shown in Figure 7A. Similar results were observed for edema, as shown in Figure 7B. [Figure 8A] This figure shows the X-ray diffraction spectrum of a commercially available nanocrystalline material. [Figure 8B] This figure shows the X-ray diffraction spectrum of a metal matrix composite material synthesized by the method described herein. [Figure 8C] This figure shows the X-ray diffraction spectrum of a metal matrix composite material synthesized by the method described herein. [Modes for carrying out the invention]

[0010] 1.Overview This specification provides a method for preparing metal matrix composites by a deposition process. The metal matrix composites disclosed herein are useful for anti-inflammatory, antimicrobial, antifungal, and bactericidal applications. In wound dressings, solutions, and kits, the metal matrix composites described herein can be used in applications involving dressings, solutions, and kits for the treatment of inflammatory skin diseases, including burns, chronic wounds, surgical scars, psoriatic eczema, and atopic dermatitis. The bandages, coatings, solutions, and kits, including the preparation of solutions, are useful for site-specific applications including bladder diseases (e.g., urinary tract infections, ureteral biofilms, and interstitial cystitis), lungs (e.g., acute respiratory distress syndrome, viral and bacterial pneumonia), eyes (e.g., viral conjunctivitis, chronic eye infections, and eye surgery), general surgery (e.g., orthopedic surgery, surgical adhesions, laparoscopy, and robotic surgery), warts, heart, traumatic injuries, implants, and infection implants.

[0011] This specification discloses various methods, including physical vapor deposition processes using complex working gas mixtures. In some embodiments, the working gas composition includes argon (80–99.9%), oxygen (0–20%), and water vapor. In some embodiments, the water vapor is controlled by a water temperature of 0–100°C in an argon flow line, which controls the water vapor pressure and allows for increasing or decreasing the amount of water drawn into the working gas flow as needed. Generally, a water temperature of 50–90°C is used. Alternatively, even lower water temperatures can be used with a sparger to introduce small bubbles and draw more water into the working gas flow.

[0012] In certain embodiments, methods utilizing a deposition process are disclosed herein. In some embodiments, this deposition process is a sputtering process, which involves the intrinsic structure and composition of a metallic plasma, forming a metallic matrix with intrinsic nanostructures. In some embodiments, the metallic matrix composite can consist of silver, silver oxide, and silver hydroxide. In various embodiments, the oxides and hydroxides formed during the deposition process limit the adatomic diffusion of incident silver atoms, effectively trapping the incident silver atoms at higher energy locations as nanostructures. In some embodiments, this has the additional advantage of generating a large number of grain boundary atoms. Generally, these atoms are found in all materials, but as the grain size of the crystal decreases below 20 nm, the atoms become more prominent because the number of grain boundaries increases. In some embodiments, as the grain size approaches 5 nm, grain boundary atoms can approach 40-50% of the matrix composition. The amount of grain boundary atoms affects the chemical and physical properties of the material, dramatically altering its biological properties.

[0013] This specification describes a method for preparing metal matrix composite materials that does not require the system to be pumped down to low pressure (high vacuum) to remove water. In some embodiments, water is included in the deposition process. In addition to altering the biological properties of the material, the various methods described herein are significantly less expensive to implement than other physical vapor deposition processes. In these other physical vapor deposition processes, which do not include the methods described herein, the target such as Al or Ta is "poisoned" by forming oxides on the surface, so the deposition chamber is evacuated before the start of the process to remove water from the system. -7The pressure is set to Torr. In this example, the Ag-O bond is weaker than the Ag-Ag bond and is sputtered from the surface as it is formed, so the target is never poisoned. For this reason, by including water in some embodiments of the various methods described herein, it is possible to reduce the exhaust of the deposition chamber (to a higher base pressure) before the start of sputtering because the removal of water is not required. In some embodiments, reducing the exhaust of the deposition chamber before deposition makes the process less expensive.

[0014] II. Definition As used herein and in the appended claims, the singular forms "a," "an," and "the" include plural forms unless otherwise evident from the context. For example, a reference to "method" includes one or more methods and / or processes of the types described herein, which would be obvious to those skilled in the art by reading this disclosure, etc.

[0015] As used herein, "about" is intended to include variations of ±20%, ±10%, ±5%, or even ±1% from a specified value when referring to measurable values ​​such as quantity or duration, because such variations are appropriate for the composition of the disclosure or for the implementation of the methods disclosed herein. In certain embodiments, methods are disclosed herein.

[0016] A metal-matrix composite (MMC) is a composite material comprising at least two components, one of which is necessarily a metal, and the other component may be a different metal, or another material such as a ceramic or organic compound. When at least three materials are present, it is called a hybrid composite (https: / / en.wikipedia.org / wiki / Metal_matrix_composite).

[0017] Plasma is a quasi-neutral ionized gas. Therefore, plasma consists of cations, anions, electrons, free radicals, photons, metastable atoms, as well as excited and neutral atoms and molecules (Fatemeh Rezaei,1). * Patrick Vanraes,2 Anton Nikiforov,1 Rino Morent,1 and Nathalie De Geyter1.Applications of Plasma-Liquid Systems:A Review.Materials(Basel).2019 Sep;12(17):2751.Pub.online 2019 Aug 27.doi:10.3390 / ma12172751, PMCID:PMC674778,PMID:31461960 https: / / www.ncbi.nlm.nih.gov / pmc / articles / PMC6747786 / ).

[0018] Oxygen species are generated in the plasma (O2+, O2-, O3, O, O+, O-, ionized ozone, metastable excited oxygen, and free electrons (https: / / allwin21.com / plasma-cleaning / )).

[0019] Water is known to decompose mainly into hydrogen atoms and hydroxyl radicals, and hydroxyl radicals can further form hydrogen and oxygen atoms (Shuaibov, AK & Shimon, L. & Dashchenko, AI & Shevera, Igor. (2001). Optical characteristics of the plasma of a glow discharge in a He / H2O mixture. Plasma Physics Reports. 27.897-900.10.1134 / 1.1409723.).

[0020] "SCCM" stands for standard cubic centimeters per minute.

[0021] "CFU" stands for Colony Forming Unit.

[0022] "AAS" stands for atomic absorption spectrometry.

[0023] Unless otherwise specified, all technical and scientific terms used herein have the same meanings as those commonly understood by those skilled in the art to which this invention pertains.

[0024] III. Process This specification describes a method for preparing a metal matrix composite material, the method comprising the step of depositing one or more metals and metal oxides from a source onto a substrate in a deposition chamber in the presence of water vapor and one or more gases including oxygen gas, wherein the source is located at a distance of at least 5 cm from the substrate, and further the method involves maintaining an internal pressure of about 10°C in the deposition chamber during deposition. -7 The process does not involve dropping below the Torrell. In some embodiments, this method involves reducing the internal pressure of the deposit chamber to about 10 before depositing. -7 The process does not involve any steps that reduce the pressure below the threshold. In some embodiments, this method reduces the internal pressure of the deposit chamber to approximately 10 within 24, 12, 6, and 3 hours prior to deposit. -7 It does not include any processes that reduce the torque below a certain level.

[0025] This specification describes various methods for preparing metal matrix composite materials, wherein liquid water is injected into an inert gas flow outside the deposition chamber and enters the deposition chamber as water vapor. In some embodiments, the liquid water is injected into an inert gas flow upstream of an inert gas mass flow controller. In some embodiments, the liquid water is injected into the inert gas flow by a syringe pump. In some embodiments, the liquid water is injected into the inert gas flow by a syringe pump at a flow rate between approximately 0.5 μl / min and approximately 11 μl / min. In some embodiments, the liquid water is injected into the inert gas flow by a syringe pump at a flow rate between approximately 7 μl / min and approximately 10 μl / min. In some embodiments, the liquid water is injected into the inert gas flow by a syringe pump at a flow rate of approximately 9 μl / min.

[0026] This specification describes various methods for preparing metal matrix composite materials, wherein liquid water is heated to a temperature between about 20°C and about 90°C in the region between the syringe pump and the mass flow controller. In some embodiments, the liquid water is heated to a temperature between about 40°C and about 60°C in the region between the syringe pump and the mass flow controller. In some embodiments, the liquid water is heated to a temperature of about 50°C in the region between the syringe pump and the mass flow controller.

[0027] This specification describes various methods for preparing metal matrix composite materials, wherein one or more gases are present in a deposition chamber. In some embodiments, one or more gases are inert gases. In some embodiments, the inert gas is argon. In some embodiments, an inert gas mass flow controller controls the flow rate of the inert gas entering the deposition chamber between about 100 SCCM and about 600 SCCM. In some embodiments, an inert gas mass flow controller controls the flow rate of the inert gas entering the deposition chamber between about 350 SCCM and about 450 SCCM. In some embodiments, an oxygen gas mass flow controller controls the flow rate of the oxygen gas entering the deposition chamber between about 0.1 SCCM and about 100 SCCM. In some embodiments, an oxygen gas mass flow controller controls the flow rate of the oxygen gas entering the deposition chamber between about 1 SCCM and about 20 SCCM. In some embodiments, an oxygen gas mass flow controller controls the flow rate of the oxygen gas entering the deposition chamber between about 5 SCCM and about 10 SCCM. In some embodiments, the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber to approximately 8 SCCM.

[0028] This specification describes various methods for preparing metal matrix composite materials, wherein one or more gases are present in a deposition chamber. In some embodiments, one or more gases are inert gases. In some embodiments, the inert gas is argon. In some embodiments, a mass flow controller for the inert gas controls the flow rate of the inert gas entering the deposition chamber between approximately 100 SCCM and approximately 600 SCCM, and the target active region is approximately 100 cm². 2 ~1000cm 2 It is between these two ranges. In some embodiments, the inert gas mass flow controller controls the flow rate of the inert gas entering the deposit chamber between approximately 350 SCCM and approximately 450 SCCM, and the target active area is approximately 100 cm². 2 ~1000cm 2 It is between. In some embodiments, the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 0.1 SCCM and approximately 100 SCCM, and the target active area is approximately 100 cm. 2 ~1000cm 2 It is between. In some embodiments, the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 1 SCCM and approximately 20 SCCM, and the target active area is approximately 100 cm. 2 ~1000cm 2 It is between. In some embodiments, the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 5 SCCM and approximately 10 SCCM, and the target active area is approximately 100 cm. 2 ~1000cm 2 In some embodiments, the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber to approximately 8 SCCM, and the target active area is approximately 100 cm². 2 ~1000cm 2 It is between these two points.

[0029] This specification describes various methods for preparing metal matrix composite materials, wherein one or more gases are present in a deposition chamber. In some embodiments, one or more gases are inert gases. In some embodiments, the inert gas is argon. In some embodiments, a mass flow controller for the inert gas controls the flow rate of the inert gas entering the deposition chamber between approximately 100 SCCM and approximately 600 SCCM, and the target active region is approximately 250 cm². 2 ~about 300cm 2 It is between these two ranges. In some embodiments, the inert gas mass flow controller controls the flow rate of the inert gas entering the deposit chamber between approximately 350 SCCM and approximately 450 SCCM, and the target active area is approximately 250 cm². 2 ~about 300cm 2 It is between. In some embodiments, the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 0.1 SCCM and approximately 100 SCCM, and the target active area is approximately 250 cm². 2 ~about 300cm 2 It is between. In some embodiments, the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 1 SCCM and approximately 20 SCCM, and the target active area is approximately 250 cm². 2 ~about 300cm 2 It is between. In some embodiments, the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 5 SCCM and approximately 10 SCCM, and the target active area is approximately 250 cm². 2 ~about 300cm 2 In some embodiments, the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber to approximately 8 SCCM, and the target active area is approximately 250 cm². 2 ~about 300cm 2 It is between these two points.

[0030] This specification describes various methods for preparing metal matrix composite materials, wherein one or more gases are present in a deposition chamber. In some embodiments, one or more gases are inert gases. In some embodiments, the inert gas is argon. In some embodiments, a mass flow controller for the inert gas controls the flow rate of the inert gas entering the deposition chamber between approximately 100 SCCM and approximately 600 SCCM, and the target active region is approximately 284 cm². 2 In some embodiments, the inert gas mass flow controller controls the flow rate of the inert gas entering the deposit chamber between approximately 350 SCCM and 450 SCCM, and the target active region is approximately 284 cm². 2 In some embodiments, the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 0.1 SCCM and approximately 100 SCCM, and the target active area is approximately 284 cm². 2 In some embodiments, the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 1 SCCM and approximately 20 SCCM, and the target active area is approximately 284 cm². 2 In some embodiments, the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 5 SCCM and approximately 10 SCCM, and the target active area is approximately 284 cm². 2 In some embodiments, the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber to approximately 8 SCCM, and the target active area is approximately 284 cm³. 2 That is the case.

[0031] This specification describes various methods for preparing metal matrix composite materials, wherein the source and the substrate are separated by a certain distance. In some embodiments, the source is a target containing a metal. In some embodiments, the distance is between about 1 cm and about 20 cm. In some embodiments, the distance is between about 5 cm and about 15 cm. In some embodiments, the distance is about 10 cm.

[0032] This specification provides a method for preparing a metal matrix composite material, wherein the internal pressure of the deposition chamber is set to approximately 1 × 10⁻⁶. -7 , 1 x 10 -6 , 1 x 10 -5 , 1 x 10 -4 , 1 x 10 -3 Methods are described that do not involve steps that reduce pressure to below 0.01, 0.1, 1, 10, 100, 760 Torrell, or atmospheric pressure.

[0033] In some embodiments, the above method involves reducing the internal pressure of the loading chamber to approximately 1 × 10⁻¹⁰ within 24, 12, 6, and 3 hours prior to loading. -8 The process does not include steps that reduce the pressure below the Torrell. In some embodiments, the above method reduces the internal pressure of the loading chamber to approximately 1 × 10⁻¹⁰ within 24, 12, 6, and 3 hours prior to loading. -7 The process does not include steps that reduce the pressure below the Torrell. In some embodiments, the above method reduces the internal pressure of the loading chamber to approximately 1 × 10⁻¹⁰ within 24, 12, 6, and 3 hours prior to loading. -6 The process does not include steps that reduce the pressure below the Torrell. In some embodiments, the above method reduces the internal pressure of the loading chamber to approximately 1 × 10⁻¹⁰ within 24, 12, 6, and 3 hours prior to loading. -5 The process does not include steps that reduce the pressure below the Torrell. In some embodiments, the above method reduces the internal pressure of the loading chamber to approximately 1 × 10⁻¹⁰ within 24, 12, 6, and 3 hours prior to loading. -5 The process does not include steps that reduce the pressure below the Torrell. In some embodiments, the above method reduces the internal pressure of the loading chamber to approximately 1 × 10⁻¹⁰ within 24, 12, 6, and 3 hours prior to loading. -4 The process does not include steps that reduce the pressure below the Torrell. In some embodiments, the above method reduces the internal pressure of the loading chamber to approximately 1 × 10⁻¹⁰ within 24, 12, 6, and 3 hours prior to loading. -3 The process does not include steps that reduce the pressure below the Torrell. In some embodiments, the above method reduces the internal pressure of the loading chamber to approximately 1 × 10⁻¹⁰ within 24, 12, 6, and 3 hours prior to loading. -2The method does not include a step of reducing the pressure below Torr. In some embodiments, the method does not include a step of reducing the internal pressure of the deposit chamber to below approximately 0.1 Torr within 24, 12, 6, or 3 hours prior to deposit. In some embodiments, the method does not include a step of reducing the internal pressure of the deposit chamber to below approximately 1 Torr within 24, 12, 6, or 3 hours prior to deposit. In some embodiments, the method does not include a step of reducing the internal pressure of the deposit chamber to below approximately 10 Torr within 24, 12, 6, or 3 hours prior to deposit. In some embodiments, the method does not include a step of reducing the internal pressure of the deposit chamber to below approximately 100 Torr within 24, 12, 6, or 3 hours prior to deposit. In some embodiments, the method does not include a step of reducing the internal pressure of the deposit chamber to below approximately 760 Torr within 24, 12, 6, or 3 hours prior to deposit. In some embodiments, the method does not include a step of reducing the internal pressure of the deposit chamber to below atmospheric pressure within 24, 12, 6, or 3 hours prior to deposit.

[0034] This specification describes methods for depositing metals. In some embodiments, the metals are precious metals. In some embodiments, the precious metals are silver, gold, platinum, palladium, or a combination thereof. In some embodiments, the method includes the step of depositing at least two metals onto a substrate. In some embodiments, the at least two metals include silver and gold. In some embodiments, the at least two metals include silver and gold, with silver present at 65% and gold present at 35%. In some embodiments, the at least two metals include silver and gold, with silver present at 35% and gold present at 65%.

[0035] In some embodiments, the method further includes the step of depositing additional metal or metal oxide onto the substrate.

[0036] This specification describes various methods for preparing a metal matrix material, wherein one or more gases are introduced into a deposition chamber. In some embodiments, one or more gases include inert gases. In some embodiments, the inert gas is argon. In some embodiments, the internal pressure of the deposition chamber during deposition is maintained between about 5 milliliters and about 50 milliliters. In some embodiments, the internal pressure of the deposition chamber during deposition is maintained between about 35 milliliters and about 45 milliliters. In some embodiments, the internal pressure of the deposition chamber during deposition is maintained at about 40 milliliters. In some embodiments, the internal pressure of the deposition chamber is between about 1 milliliter and about 100 milliliters. In some embodiments, the internal pressure of the deposit chamber is approximately 1 milliliter to 10 milliliters, approximately 1 milliliter to 20 milliliters, approximately 1 milliliter to 30 milliliters, approximately 1 milliliter to 40 milliliters, approximately 1 milliliter to 50 milliliters, approximately 1 milliliter to 100 milliliters, approximately 10 milliliters to 20 milliliters, approximately 10 milliliters to 30 milliliters, approximately 10 milliliters to 40 milliliters, approximately 10 milliliters to 50 milliliters, and approximately 10 milliliters. The pressures are approximately 1 milliliter to 100 milliliters, approximately 20 to 30 milliliters, approximately 20 to 40 milliliters, approximately 20 to 50 milliliters, approximately 20 to 100 milliliters, approximately 30 to 40 milliliters, approximately 30 to 50 milliliters, approximately 30 to 100 milliliters, approximately 40 to 50 milliliters, approximately 40 to 100 milliliters, or approximately 50 to 100 milliliters. In some embodiments, the internal pressure of the deposit chamber is approximately 1 milliliter, approximately 10 milliliters, approximately 20 milliliters, approximately 30 milliliters, approximately 40 milliliters, approximately 50 milliliters, or approximately 100 milliliters. In some embodiments, the internal pressure of the deposit chamber is at least approximately 1 milliliter, approximately 10 milliliters, approximately 20 milliliters, approximately 30 milliliters, approximately 40 milliliters, or approximately 50 milliliters. In some embodiments, the internal pressure of the deposit chamber is at most about 10 milliliters, about 20 milliliters, about 30 milliliters, about 40 milliliters, about 50 milliliters, or about 100 milliliters.

[0037] This specification describes various methods for preparing metal matrix composite materials deposited on a substrate. In some embodiments, the substrate is solid. In some embodiments, the solid includes metal foil, glass, or silicon. In some embodiments, the substrate exhibits low gas emission. In some embodiments, the substrate is an implant. In some embodiments, the implant is a stent. In some embodiments, the stent is a metal stent. In some embodiments, the substrate includes a polymer. In some embodiments, the polymer is high-density polyethylene. In some embodiments, the substrate includes a mesh structure made from high-density polyethylene. In some embodiments, the bandage includes a mesh structure made from high-density polyethylene. In some embodiments, the bandage includes an absorbent layer between two of the mesh structures made from high-density polyethylene. In some embodiments, the substrate moves linearly within the deposition chamber. In some embodiments, the substrate moves rotationally within the deposition chamber.

[0038] This specification describes a method for preparing a metal matrix composite, comprising the step of depositing a metal. In some embodiments, the deposition includes sputtering. In some embodiments, the sputtering includes DC magnetron sputtering. In some embodiments, the sputtering power is about 190 watts to about 950 watts (0.5 to 2.5 amperes at 380 volts). In some embodiments, the sputtering power is about 380 watts to about 760 watts (1 to 2 amperes at 380 V). In some embodiments, the sputtering power is about 571 watts (1.5 amperes at 380 volts). In some embodiments, the sputtering power is about 10 watts to about 1000 watts. In some embodiments, the sputtering power is approximately 10 watts to 100 watts, approximately 10 watts to 200 watts, approximately 10 watts to 500 watts, approximately 10 watts to 1000 watts, approximately 100 watts to 200 watts, approximately 100 watts to 500 watts, approximately 100 watts to 1000 watts, approximately 200 watts to 500 watts, approximately 200 watts to 1000 watts, or approximately 500 watts to 1000 watts. In some embodiments, the sputtering power is approximately 10 watts, approximately 100 watts, approximately 200 watts, approximately 500 watts, or approximately 1000 watts. In some embodiments, the sputtering power is at least approximately 10 watts, approximately 100 watts, approximately 200 watts, or approximately 500 watts. In some embodiments, the sputtering power is at most approximately 100 watts, approximately 200 watts, approximately 500 watts, or approximately 1000 watts.

[0039] This specification describes a method for preparing a metal matrix composite, comprising the step of depositing a metal. In some embodiments, the deposition includes sputtering. In some embodiments, the sputtering is DC magnetron sputtering. 2 In some embodiments, the sputtering power density is approximately 0.1 W / cm². 2 ~About 3W / cm 2 In some embodiments, the power density is approximately 0.1 W / cm². 2~about 0.9 W / cm 2 、about 0.1 W / cm 2 ~about 1.5 W / cm 2 、about 0.1 W / cm 2 ~about 1.8 W / cm 2 、about 0.1 W / cm 2 ~about 2 W / cm 2 、about 0.1 W / cm 2 ~about 2.5 W / cm 2 、about 0.1 W / cm 2 ~about 3 W / cm 2 、about 0.9 W / cm 2 ~about 1.5 W / cm 2 、about 0.9 W / cm 2 ~about 1.8 W / cm 2 、about 0.9 W / cm 2 ~about 2 W / cm 2 、about 0.9 W / cm 2 ~about 2.5 W / cm 2 、about 0.9 W / cm 2 ~about 3 W / cm 2 、about 1.5 W / cm 2 ~about 1.8 W / cm 2 、about 1.5 W / cm 2 ~about 2 W / cm 2 、about 1.5 W / cm 2 ~about 2.5 W / cm 2 、about 1.5 W / cm 2 ~about 3 W / cm 2 、about 1.8 W / cm 2 ~about 2 W / cm 2 、about 1.8 W / cm 2 ~about 2.5 W / cm 2 、about 1.8 W / cm 2 ~about 3 W / cm 2 、about 2 W / cm 2 ~about 2.5 W / cm 2 、about 2 W / cm 2 ~about 3 W / cm 2 、or about 2.5 W / cm 2 ~about 3 W / cm 2 is. In some embodiments, the power density is about 0.1 W / cm 2 、about 0.9 W / cm 2 、about 1.5 W / cm 2 、about 1.8 W / cm 2 、about 2 W / cm2 , about 2.5W / cm 2 , or approximately 3W / cm 2 In some embodiments, the power density is at least about 0.1 W / cm². 2 , about 0.9W / cm 2 , about 1.5W / cm 2 Approximately 1.8 W / cm² 2 , about 2W / cm 2 , or approximately 2.5 W / cm² 2 In some embodiments, the power density is at most about 0.9 W / cm². 2 , about 1.5W / cm 2 Approximately 1.8 W / cm² 2 , about 2W / cm 2 , about 2.5W / cm 2 , or approximately 3W / cm 2 That is the case.

[0040] This specification describes a method for preparing a metal matrix composite material, the method comprising the step of depositing one or more metals and metal oxides onto a substrate in a deposition chamber in the presence of one or more gases including oxygen gas, the method wherein the internal pressure of the deposition chamber is about 10 -7 It does not include any processes that reduce the torque below a certain level.

[0041] This specification describes a method for preparing a metal matrix composite material, the method comprising the steps of depositing one or more metals and metal oxides onto a substrate in a deposition chamber, pressurizing the deposition chamber with a combination of one or more inert gases and oxygen gases, wherein the deposition of at least one metal and metal oxide occurs from a source located at a distance of at least 5 cm from the substrate.

[0042] This specification describes a method for preparing a metal matrix composite material, comprising the step of depositing one or more metals and metal oxides onto a substrate in a deposition chamber, wherein the composite working gas mixture includes an inert gas, oxygen gas, and water vapor.

[0043] In some embodiments, the duration of the deposit is approximately 0.01 hours to approximately 100 hours. In some embodiments, the duration of the deposit is approximately 0.01 hours to approximately 0.1 hours, approximately 0.01 hours to approximately 1 hour, approximately 0.01 hours to approximately 50 hours, approximately 0.01 hours to approximately 100 hours, approximately 0.1 hours to approximately 1 hour, approximately 0.1 hours to approximately 50 hours, approximately 0.1 hours to approximately 100 hours, approximately 1 hour to approximately 50 hours, approximately 1 hour to approximately 100 hours, or approximately 50 hours to approximately 100 hours. In some embodiments, the duration of the deposit is approximately 0.01 hours, approximately 0.1 hours, approximately 1 hour, approximately 50 hours, or approximately 100 hours. In some embodiments, the duration of the deposit is at least approximately 0.01 hours, approximately 0.1 hours, approximately 1 hour, or approximately 50 hours. In some embodiments, the duration of deposition is at most about 0.1 hours, about 1 hour, about 50 hours, or about 100 hours.

[0044] In some embodiments, the deposition time exceeds 100 hours. In some embodiments, the length is 50 hours in a machine equipped with 20 cathodes, where the substrate is moved at a linear speed of 20.8 m / hour in a roll-to-roll process.

[0045] In some embodiments, water is used together with oxygen and an inert gas to deposit nanocrystalline precious metals onto a substrate. In some embodiments, the above method utilizes the synergistic relationship between water and oxygen in the presence of an inert gas.

[0046] In some embodiments, the presence of water and oxygen makes it possible to deposit the metal matrix composite materials described herein at a much higher power than that possible when using oxygen alone. In such embodiments, the higher power results in a higher reaction rate. In such embodiments, argon is present at 95.75% and oxygen at 4.25% at 2.4 watts / cm³. 2 It is used.

[0047] In some embodiments, a low base pressure is obtained before sputtering. In such embodiments, the process is initiated by introducing oxygen into the working gas before it strikes the plasma.

[0048] This specification describes methods for preparing metal matrix composite materials. In some embodiments, the metal matrix composite material is exposed to a carbon dioxide environment after the deposition step of the method described herein. In some embodiments, carbon dioxide is present in the carbon dioxide environment at a concentration of about 100 ppm to about 1,000,000 ppm. In some embodiments, carbon dioxide is present in the carbon dioxide environment at concentrations of approximately 100 ppm to 200 ppm, 100 ppm to 400 ppm, 100 ppm to 1,000 ppm, 100 ppm to 1,000,000 ppm, 200 ppm to 400 ppm, 200 ppm to 1,000 ppm, 200 ppm to 1,000 ppm, 400 ppm to 1,000 ppm, 400 ppm to 1,000,000 ppm, or 1,000 ppm to 1,000,000 ppm. In some embodiments, carbon dioxide is present in the carbon dioxide environment at a concentration of at least about 100 ppm, about 200 ppm, about 400 ppm, or about 1,000 ppm. In some embodiments, carbon dioxide is present in the carbon dioxide environment at a concentration of at most about 200 ppm, about 400 ppm, about 1,000 ppm, or about 1,000,000 ppm. In some embodiments, the carbon dioxide environment is pure carbon dioxide.

[0049] A. Assays regarding antibacterial effects This specification describes various methods for assaying the antimicrobial effects of metal matrix composite materials. In some embodiments, the antimicrobial effect of the coating was tested using a logarithmic reduction test. In some embodiments, a bacterial inoculum was prepared by inoculating 50 mL of calf serum with a 16-hour culture of Pseudomonas aeruginosa and incubating for 16 hours. In some embodiments, this method yielded 1.05 × 10⁻⁶ 9 CFU inoculum was produced. In some embodiments, bandages were prepared from two silver-coated HDPE pieces (2.5 × 2.5 cm) with a piece of cotton gauze (2.5 × 2.5 cm) in between. In some embodiments, the bandage was placed on a sterile plastic piece (3.2 × 3.2 cm) with the lid of a petri dish inverted in a Class 2 laminar-flow hood. In some embodiments, 200 μL of inoculum was applied to the bandage in the petri dish, then covered with a second plastic piece (3.2 × 3.2 cm), and incubated at 37°C for 1 hour. In some embodiments, the bandage, containing the plastic base piece and the coating piece with bacteria, was then inactivated in 1.8 mL of sodium thioglycolate saline (STS), then diluted in a dish with peptone water, and inoculated onto Mueller-Hinton agar. In some embodiments, the plates were examined 24 hours after incubation, and the total number of bacterial colony-forming units was calculated. In some embodiments, the following equation was used:

[0050] Equation 1.

[0051] 1 / (IDxSDxFD)X50XCFU=CFU / mL

[0052] In the formula, ID is the initial dilution, SD is the later dilution, FD is the final dilution, 50 is converted to mL, and CFU is the colony-forming unit counted at the dilution used in the calculation.

[0053] In some embodiments, the CFU / mL was then converted to a logarithmic number. The logarithmic reduction was calculated by subtracting the logarithm of the recovered CFU from the logarithm of the inoculum. A logarithmic reduction of more than 3 was considered bactericidal.

[0054] B. Determining the total amount of silver in the bandage This specification describes various methods for determining the total amount of silver in a bandage. In some embodiments, one square inch of bandage was dissolved in 20 mL of a 50% solution of nitric acid in distilled water over 20 minutes, then diluted in an additional 20 mL of distilled water, and analyzed using an atomic absorption spectrophotometer (AAS).

[0055] C. Determination of the amount of ammonium hydroxide-soluble silver in the bandage. This specification describes various methods for determining the amount of ammonium hydroxide-soluble silver. In some embodiments, the amount of silver oxide in a bandage was estimated by dissolving a metal matrix composite material. In some embodiments, one square inch of the bandage was immersed in 20 mL of 14.5 moles of ammonium hydroxide for 10 minutes. In some embodiments, 10 mL of this solution was diluted in 40 mL of water and analyzed using atomic absorption spectroscopy (AAS).

[0056] Overall, the method of this disclosure includes the step of preparing a metal matrix composite. Generally, the metal matrix composite is dissolved in ammonium hydroxide and characterized by analyzing the dissolved material using AAS. Figure 2A shows the effect of water on ammonium hydroxide-soluble silver and 684 watts (1.8 amperes at 380 volts). The y-axis plots the percentage of ammonium hydroxide-soluble silver characterized by ASS. The x-axis plots the flow rate of the liquid water used in the above method to form water vapor upon or before entry into the deposition chamber. Figure 2B shows the effect of water on the antimicrobial activity of the metal matrix composite when 684 watts is used, and liquid water is introduced at various flow rates of microliters per minute. The y-axis plots the logarithmic decrease of CFU / mL. The x-axis plots the flow rate of the liquid water used in the above method to form water vapor upon or before entry into the deposition chamber.

[0057] In various examples described herein, the methods of the disclosure include the step of preparing a metal matrix composite. Generally, the metal matrix composite is characterized by dissolving it in ammonium hydroxide and analyzing the dissolved material using AAS. Figure 3A shows the effect of water on ammonium hydroxide-soluble silver and 571 watts (1.5 amperes at 380 volts). The y-axis plots the percentage of ammonium hydroxide-soluble silver characterized by ASS. The x-axis plots the flow rate of the liquid water used in the above method to form water vapor upon or before entry into the deposition chamber. Figure 3B shows the effect of water on the antimicrobial activity of the metal matrix composite when sputtering power of 685 watts (1.8 amperes at 380 volts) is used and liquid water is introduced at various flow rates of microliters per minute. The y-axis plots the logarithmic decrease of CFU / mL. The x-axis plots the flow rate of the liquid water used in the above method to form water vapor upon or before entry into the deposition chamber.

[0058] In various examples described herein, the methods of this disclosure include the step of preparing a metal matrix composite. Generally, the metal matrix composite is dissolved in ammonium hydroxide and characterized by analyzing the dissolved material using AAS. Figure 4 shows the effect of various concentrations of water and 2% oxygen used in each run on the amount of ammonium-soluble silver produced. The y-axis plots the percentage of ammonium-soluble silver characterized by ASS. The x-axis plots the flow rate of liquid water used in the above method, which forms water vapor upon or before entry into the deposit chamber.

[0059] This specification describes various methods for preparing metal matrix complexes. In some embodiments, the metal matrix complexes are characterized with respect to the amount of ammonium hydroxide-soluble silver. Figure 5A shows the effects of H2O and O2 on ammonium hydroxide-soluble Ag and 571 watts (1.5 amperes at 380 volts). The y-axis plots the percentage of ammonium hydroxide-soluble silver characterized by ASS. The x-axis plots the percentages of oxygen flowing into the deposition chamber. The solid trace plots data obtained from metal matrix complexes formed using a sputtering power of 571 watts and a liquid water flow rate of 9 μL / min in some embodiments of this method. The dashed trace plots data obtained from metal matrix complexes formed using a sputtering power of 571 watts but without the use of liquid water in some embodiments of this method. Figure 5B shows the logarithmic decrease of Pseudomonas aeruginosa with and without water concentration. The y-axis plots the logarithmic decrease in CFU / mL. The x-axis plots the various percentages of oxygen flowing into the deposition chamber. The dashed line plots data obtained from metal matrix composites formed using 571 watts of sputtering power but without the use of liquid water, in some embodiments of this method. The solid trace plots data obtained from metal matrix composites formed using 571 watts of sputtering power and a liquid water flow rate of 9 μL / min, in some embodiments of this method.

[0060] Figure 6A shows the effect of water on the antimicrobial activity of Ag / Au (35% / 65%) alloy deposited in argon. The y-axis plots the logarithmic decrease in CFU / mL. The x-axis plots the amount of liquid water used at various flow rates in microliters per minute. Figure 6B shows the effect of water on the antimicrobial activity of a metal matrix composite composed of 35% silver and 65% gold thin films deposited at various oxygen concentrations. The y-axis plots the logarithmic decrease in CFU / mL. The x-axis plots the percentage of oxygen present in the deposition chamber. The solid line represents the assay performance of the metal matrix composite containing 35% silver and 65% gold at a liquid water flow rate of 8 microliters per minute. The dashed line represents the assay performance of the metal matrix composite containing 35% silver and 65% gold without the use of water.

[0061] IV. Material This specification describes various compositions of metal matrix composites. In some embodiments, the metal matrix composite contains metal grain boundary atoms, where the median diameter of the metal grains is between approximately 2 nm and approximately 15 nm, and the grain boundary atoms comprise approximately 50% to approximately 20% of the unit surface area of ​​the metal matrix composite. In some embodiments, the median diameter of the grains is between approximately 2 nm and approximately 15 nm, and the metal grain boundary atoms comprise approximately 50% to approximately 20% of the unit surface area of ​​the metal matrix composite. In some embodiments, the median diameter of the grains is between approximately 5 nm and approximately 15 nm, and the metal grain boundary atoms comprise approximately 40% to approximately 20% of the unit surface area of ​​the metal matrix composite.

[0062] In some embodiments, the grain boundary atoms of the second metal are such that the median diameter of the crystal grains of the second metal is between approximately 2 nm and approximately 15 nm, and the grain boundary atoms of the second metal constitute approximately 50 to approximately 20% per unit surface area of ​​the metal matrix composite material.

[0063] In some embodiments, the metal is silver or gold. In some embodiments, the metal is an alloy of silver and gold. In some embodiments, the film of the metal matrix composite material contains the metal, reaction products, unreacted oxygen, and water. In some embodiments, the reaction products are metal oxides. In some embodiments, the metal is a precious metal.

[0064] In some embodiments, the metal matrix composite contains less than 20% oxygen. In some embodiments, the metal matrix composite contains more than 1% oxygen. In some embodiments, the metal matrix composite contains less than 6% oxygen. In some embodiments, the metal matrix composite contains more than 2% oxygen. In some embodiments, the silver composite contains less than 6% oxygen. In some embodiments, the silver matrix composite contains 6% oxygen, of which 4% is contained in silver oxide and the remainder is from water and molecular oxygen. In some embodiments, the silver matrix composite contains 60% material soluble in ammonia, where about 38% to about 40% silver is contained in silver metal and about 52% to about 56% silver is contained in silver oxide. In such embodiments, the silver matrix composite contains about 4% to 6% oxygen in the form of silver oxide, water, and molecular oxygen. In some embodiments, the metal matrix composite contains at least 2% oxygen obtained from silver oxide, water, and molecular oxygen.

[0065] This specification describes various methods for preparing metal matrix composite materials. In some embodiments, the metal matrix composite material is used as a bandage for applications including wound healing. In some embodiments, the bandage includes a mesh structure made from high-density polyethylene. In some embodiments, the bandage includes an absorbent layer between two of the mesh structures made from high-density polyethylene. In some embodiments, the substrate includes a polymer. In some embodiments, the polymer is high-density polyethylene. In some embodiments, the substrate includes a mesh structure made from high-density polyethylene. Figure 1 shows a bandage made from two mesh layers surrounding a cotton absorbent layer. The mesh layers are coated with a metal matrix composite. The bandage is integrally bonded by ultrasonic welding.

[0066] This specification describes various methods for preparing metal matrix composite materials. In some embodiments, the metal matrix composite is removed from a substrate. In some embodiments, the metal matrix composite is removed by at least partial dissolution in a solution. In some embodiments, the metal matrix composite is removed by at least partial dissolution in an aqueous solution. In some embodiments, the aqueous solution has a pH of about 3 to 10. In some embodiments, the aqueous solution has a pH range of about 4 to 9. In some embodiments, the aqueous solution has a pH range of about 6 to 8. In some embodiments, the aqueous solution has a pH of about 7. In some embodiments, the aqueous solution is administered to a patient by a delivery device applied to the lungs. In some embodiments, the delivery device is a nebulizer. In some embodiments, the aqueous solution is used for bronchoalveolar lavage (BAL).

[0067] This specification describes various methods for preparing metal matrix composites for the treatment of erythema and edema. In some embodiments, metal matrix composites prepared by various methods and compositions described herein are used to treat erythema or edema. The results of such treatments are summarized in Figures 7A and 7B. Various metal matrix composites produced by the methods described herein, containing varying amounts of gold, silver, or combinations thereof, were found to reduce erythema considerably more rapidly than Acticoat bandages, as shown in Figure 7A. In Figure 7A, the y-axis plots the erythema score and the x-axis plots time in days. The erythema score ranges from 1 to 4, with higher numbers indicating greater disease severity. The first treatment uses a saline control and is represented by a thick line. The second treatment uses Acticoat and is represented by a short dashed line. The third treatment uses a metal matrix composite prepared by the methods described herein, with a higher percentage of gold than silver, and is represented by a long dashed line. The fourth treatment uses a metal matrix composite material prepared according to the method herein, in which the percentage of gold is less than that of silver, and is represented as a long, large-dash-spot dashed line series. The fifth treatment uses a metal matrix composite material prepared according to the method herein, containing silver, oxygen, argon, water, or a combination thereof, and is represented as a medium-dash dashed line series. Figure 7B plots the results of applying various bandages for the treatment of edema, containing various embodiments of the metal matrix composites prepared according to the method herein. The results are presented in the same form as described in Figure 7A.

[0068] In some embodiments, X-ray diffraction is used to characterize the materials. Figure 8A shows the X-ray diffraction spectrum for a commercially available nanocrystalline material. Figures 8B and 8C show the X-ray diffraction spectra for a metal matrix composite material synthesized by the method described herein.

[0069] Numbered Embodiments The following embodiments list non-limiting permutations of combinations of features disclosed herein. Other permutations of combinations of features are also contemplated. Specifically, each of these numbered embodiments is contemplated to be dependent on or related to all preceding or succeeding embodiments, regardless of the order in which they are enumerated. 1. A method for preparing various metal matrix composite materials, the method comprising the step of depositing one or more metals and metal oxides from a source onto a substrate in a deposition chamber in the presence of water vapor and one or more gases including oxygen gas, wherein the source is located at a distance of at least 5 cm from the substrate, and further the method does not include the step of reducing the internal pressure of the deposition chamber below about 10⁻⁷ Torre before and / or during deposition. 2. The method according to Embodiment 1, wherein the base pressure during deposition is about 10⁻⁷ Torre or greater. 3. The method according to Embodiment 1 or 2, which does not include the step of reducing the internal pressure of the deposition chamber below about 10⁻⁷ Torre within 24 hours, 12 hours, 6 hours, and 3 hours before deposition. 4. The method according to any one of Embodiments 1 to 3, wherein 4.1 or more gases further include an inert gas. 5. The method according to any one of Embodiments 1 to 4, wherein liquid water is injected into an inert gas stream outside the deposit chamber and enters the deposit chamber as water vapor. 6. The method according to any one of Embodiments 1 to 5, wherein the oxygen gas includes molecular oxygen gas. 7. The method according to any one of Embodiments 1 to 6, wherein the molecular oxygen gas includes any form of molecular oxygen gas. 8. The method according to any one of Embodiments 1 to 6, wherein the molecular oxygen gas is selected from the group consisting of O2, O3, O3+, O2+, O2-, O3, O, O+, O-, ionized ozone, metastable excited oxygen, free electrons, H2O2, and OH. 9. The method according to any one of Embodiments 1 to 8, wherein liquid water is injected into an inert gas stream upstream of a mass flow controller of the inert gas. 10. The method according to any one of Embodiments 1 to 9, wherein an inert gas is present at a concentration of approximately 90% to approximately 99%, an oxygen gas at a concentration of approximately 1% to approximately 10%, and water vapor at a concentration of approximately 0.1% to approximately 5% of the total molar composition of one or more gases.11. The method according to any one of Embodiments 1 to 10, wherein the inert gas is present at a rate of about 94% to about 96%, the oxygen gas at a rate of about 1% to about 5%, and the water vapor at a rate of about 0.01% to about 2% of the total molar composition of one or more gases. 12. The method according to any one of Embodiments 1 to 11, wherein the inert gas is present at a rate of about 95% to about 96%, the oxygen gas at a rate of about 1% to about 4.5%, and the water vapor at a rate of about 0.03% to about 1.02% of one or more gases. 13. The method according to any one of Embodiments 1 to 12, wherein liquid water is injected into the inert gas stream by a syringe pump. 14. The method according to any one of Embodiments 1 to 13, wherein liquid water is injected into the inert gas stream by a syringe pump at a flow rate of about 0.5 μl / min to about 11 μl / min. 15. The method according to any one of Embodiments 1 to 14, wherein liquid water is injected into the inert gas stream by a syringe pump at a flow rate between approximately 7 μl / min and approximately 10 μl / min. 16. The method according to any one of Embodiments 1 to 15, wherein liquid water is injected into the inert gas stream by a syringe pump at a flow rate between approximately 9 μl / min. 17. The method according to any one of Embodiments 1 to 16, wherein liquid water is injected into the inert gas stream upstream of the inert gas mass flow controller. 18. The method according to any one of Embodiments 1 to 17, wherein liquid water is injected into the inert gas stream downstream of the inert gas mass flow controller. 19. The method according to any one of Embodiments 1 to 18, wherein liquid water is injected into the inert gas stream downstream of the inert gas mass flow controller when the composition exceeds 1.02% of the total composition. 20. The method according to any one of Embodiments 1 to 19, wherein steam is injected directly into the deposit chamber. 21. The method according to any one of Embodiments 1 to 20, wherein the inert gas mass flow controller controls the flow rate of the inert gas entering the deposit chamber between approximately 100 SCCM and approximately 600 SCCM. 22. The method according to any one of Embodiments 1 to 21, wherein the inert gas mass flow controller controls the flow rate of the inert gas entering the deposit chamber between approximately 350 SCCM and approximately 450 SCCM.23. The method according to any one of Embodiments 1 to 22, wherein the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 0.1 SCCM and approximately 100 SCCM. 24. The method according to any one of Embodiments 1 to 23, wherein the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 1 SCCM and approximately 20 SCCM. 25. The method according to any one of Embodiments 1 to 24, wherein the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 5 SCCM and approximately 10 SCCM. 26. The method according to any one of Embodiments 1 to 25, wherein the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber to approximately 8 SCCM. 27. The method according to any one of Embodiments 1 to 26, wherein liquid water is heated to a temperature between approximately 20°C and approximately 80°C in the region between the syringe pump and the mass flow controller. 28. The method according to any one of Embodiments 1 to 27, wherein liquid water is heated to a temperature between about 40°C and about 60°C in the region between the syringe pump and the mass flow controller. 29. The method according to any one of Embodiments 1 to 28, wherein liquid water is heated to a temperature between about 50°C in the region between the syringe pump and the mass flow controller. 30. The method according to any one of Embodiments 1 to 29, wherein the distance is between about 1 cm and about 20 cm. 31. The method according to any one of Embodiments 1 to 30, wherein the distance is between about 5 cm and about 15 cm. 32. The method according to any one of Embodiments 1 to 31, wherein the distance is about 10 cm. 33. The method according to any one of Embodiments 1 to 32, wherein the step of reducing the internal pressure of the deposit chamber to below about 10⁻⁷, 10⁻⁶, 10⁻⁵, 10⁻⁴, 10⁻³, 0.01, 0.1, 1, 10, 100, 760 Torr, or atmospheric pressure. 34. The method according to any one of Embodiments 1 to 33, wherein the metal is a precious metal. 35. The method according to any one of Embodiments 1 to 34, wherein the precious metal is silver, gold, platinum, palladium, or a combination thereof. 36. The method according to any one of Embodiments 1 to 35, further comprising the step of depositing at least two metals onto a substrate. 37. The method according to any one of Embodiments 1 to 36, wherein at least two metals include silver and gold.38. The method according to any one of Embodiments 1 to 37, wherein at least two metals include silver and gold, with silver present at 65% and gold at 35%. 39. The method according to any one of Embodiments 1 to 37, wherein at least two metals include silver and gold, with silver present at 35% and gold at 65%. 40. The method according to any one of Embodiments 1 to 39, further comprising the step of depositing an additional metal or metal oxide on a substrate. 41. The method according to any one of Embodiments 1 to 40, wherein the inert gas is argon. 42. The method according to any one of Embodiments 1 to 41, wherein the internal pressure of the deposit chamber during deposition is maintained between about 5 milliliters and about 50 milliliters. 43. The method according to any one of Embodiments 1 to 42, wherein the internal pressure of the deposit chamber during deposition is maintained between about 35 milliliters and about 45 milliliters. 44. The method according to any one of Embodiments 1 to 43, wherein the internal pressure of the deposit chamber during deposition is maintained at about 40 milliliters. 45. The method according to any one of Embodiments 1 to 44, wherein the substrate is solid. 46. The method according to any one of Embodiments 1 to 45, wherein the solid comprises metal foil, glass, or silicon. 47. The method according to any one of Embodiments 1 to 46, wherein the substrate exhibits low gas emission. 48. The method according to any one of Embodiments 1 to 47, wherein the substrate is an implant. 49. The method according to any one of Embodiments 1 to 48, wherein the implant is a stent. 50. The method according to any one of Embodiments 1 to 49, wherein the stent is a metal stent. 51. The method according to any one of Embodiments 1 to 50, wherein the substrate comprises a polymer. 52. The method according to any one of Embodiments 1 to 51, wherein the polymer is high-density polyethylene. 53. The method according to any one of Embodiments 1 to 52, wherein the substrate comprises a mesh structure made from high-density polyethylene. 54. The method according to any one of Embodiments 1 to 53, wherein the bandage comprises a mesh structure made from high-density polyethylene. 55. The method according to any one of Embodiments 1 to 54, wherein the bandage comprises an absorbent layer between two mesh structures made of high-density polyethylene. 56. The method according to any one of Embodiments 1 to 55, wherein the deposition comprises sputtering.57. The method according to any one of Embodiments 1 to 56, wherein the sputtering is DC magnetron sputtering. 58. The method according to any one of Embodiments 1 to 57, wherein the sputtering power is approximately 190 watts to approximately 950 watts. 59. The method according to any one of Embodiments 1 to 58, wherein the sputtering power is approximately 380 watts to approximately 760 watts. 60. The method according to any one of Embodiments 1 to 59, wherein the sputtering power is approximately 570 watts to approximately 684 watts. 61. The method according to any one of Embodiments 1 to 60, wherein the sputtering power density is between approximately 0.7 watts / cm² and approximately 3.3 watts / cm². 62. The method according to any one of Embodiments 1 to 61, wherein the sputtering power density is between approximately 1.3 to approximately 2.7 watts / cm². 63. The method according to any one of Embodiments 1 to 62, wherein the sputtering power density is between approximately 2.0 to approximately 2.4 watts / cm². 64. The method according to any one of Embodiments 1 to 63, wherein the sputtering power density is about 2.4 watts / cm². 65. The method according to any one of Embodiments 1 to 64, wherein the inert gas is present at a concentration of about 95% to about 96%, the oxygen gas is present at a concentration of about 1% to about 4.5%, the water vapor is present at a concentration of about 2.8%, and the sputtering power density is about 2.4 watts / cm². 66. The method according to any one of Embodiments 1 to 65, wherein the metal matrix composite is exposed to a carbon dioxide environment of at least 200 ppm after deposition. 67. A method for preparing a metal matrix composite, comprising the step of depositing one or more metals and metal oxides on a substrate in a deposition chamber in the presence of one or more gases including oxygen gas, but without the step of reducing the internal pressure of the deposition chamber below about 10⁻⁷ torre before and / or during deposition. 68. The method according to Embodiment 67, further comprising the step of reducing the internal pressure of the deposition chamber below about 10⁻⁷ milliliters before deposition. 69. The method according to Embodiment 67 or 68, which does not include the step of reducing the internal pressure of the loading chamber to below about 10⁻⁷ milliliters within 24, 12, 6, or 3 hours prior to loading. 70. The method according to any one of Embodiments 67 to 69, wherein liquid water is injected into an inert gas flow outside the loading chamber and enters the loading chamber as water vapor.71. The method according to any one of embodiments 67 to 70, wherein liquid water is injected into an inert gas stream upstream of an inert gas mass flow controller. 72. The method according to any one of embodiments 67 to 71, wherein liquid water is injected into an inert gas stream by a syringe pump. 73. The method according to any one of embodiments 67 to 72, wherein liquid water is injected into an inert gas stream by a syringe pump at a flow rate between approximately 0.5 μl / min and approximately 11 μl / min. 74. The method according to any one of embodiments 67 to 73, wherein liquid water is injected into an inert gas stream by a syringe pump at a flow rate between approximately 7 μl / min and approximately 10 μl / min. 75. The method according to any one of embodiments 67 to 74, wherein liquid water is injected into an inert gas stream by a syringe pump at a flow rate between approximately 9 μl / min. 76. Inert gas mass flow controller. 77. The method according to any one of embodiments 67 to 75, wherein the Trolla controls the flow rate of inert gas entering the deposit chamber between approximately 100 SCCM and approximately 600 SCCM. 78. The method according to any one of embodiments 67 to 77, wherein the inert gas mass flow controller controls the flow rate of inert gas entering the deposit chamber between approximately 350 SCCM and approximately 450 SCCM. 79. The method according to any one of embodiments 67 to 78, wherein the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 0.1 SCCM and approximately 100 SCCM. 80. The method according to any one of embodiments 67 to 79, wherein the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 1 SCCM and approximately 20 SCCM. 81. The method according to any one of embodiments 67 to 80, wherein the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber to about 8 SCCM. 82. The method according to any one of embodiments 67 to 81, wherein liquid water is heated to a temperature between about 20°C and about 80°C in the region between the syringe pump and the mass flow controller. 83. The method according to any one of embodiments 67 to 82, wherein liquid water is heated to a temperature between about 40°C and about 60°C in the region between the syringe pump and the mass flow controller. 84. The method according to any one of embodiments 67 to 83, wherein liquid water is heated to a temperature of about 50°C in the region between the syringe pump and the mass flow controller. 85. The method according to any one of embodiments 67 to 84, wherein the distance between the supply source and the substrate is between about 1 cm and about 20 cm. 86. The method according to any one of embodiments 67 to 85, wherein the distance is between about 5 cm and about 15 cm. 87. The method according to any one of embodiments 67 to 86, wherein the distance is approximately 10 cm. 88. The method according to any one of embodiments 67 to 87, wherein the step of reducing the internal pressure of the deposit chamber to approximately 10⁻⁷, 10⁻⁶, 10⁻⁵, 10⁻⁴, 10⁻³, 0.01, 0.1, 1, 10, 100, 760 Torr, or below atmospheric pressure.89. The method according to any one of embodiments 67 to 88, wherein the metal is a precious metal. 90. The method according to any one of embodiments 67 to 89, wherein the precious metal is silver, gold, platinum, palladium, or a combination thereof. 91. The method according to any one of embodiments 67 to 90, comprising the step of depositing at least two metals on a substrate. 92. The method according to any one of embodiments 67 to 91, wherein at least two metals include silver and gold. 93. The method according to any one of embodiments 67 to 92, wherein at least two metals include silver and gold, with silver present at 65% and gold at 35%. 94. The method according to any one of embodiments 67 to 92, wherein at least two metals include silver and gold, with silver present at 35% and gold at 65%. 95. The method according to any one of embodiments 67 to 94, further comprising the step of depositing an additional metal or metal oxide on a substrate. 96. The method according to any one of embodiments 67 to 95, wherein one or more gases further include an inert gas. 97. The method according to any one of embodiments 67 to 96, wherein the inert gas is argon. 98. The method according to any one of embodiments 67 to 97, wherein the internal pressure of the deposition chamber during deposition is maintained between about 5 milliliters and about 50 milliliters. 99. The method according to any one of embodiments 67 to 98, wherein the internal pressure of the deposition chamber during deposition is maintained between about 35 milliliters and about 45 milliliters. 100. The method according to any one of embodiments 67 to 99, wherein the internal pressure of the deposition chamber during deposition is maintained at about 40 milliliters. 101. The method according to any one of embodiments 67 to 100, wherein the substrate is solid. 102. The method according to any one of embodiments 67 to 101, wherein the solid comprises metal foil, glass, or silicon. 103. The method according to any one of embodiments 67 to 102, wherein the substrate exhibits low gas emission. 104. The method according to any one of embodiments 67 to 103, wherein the substrate is implantable. 105. The method according to any one of embodiments 67 to 104, wherein the implant is a stent. 106. The method according to any one of embodiments 67 to 105, wherein the stent is a metal stent. 107. The method according to any one of embodiments 67 to 106, wherein the substrate comprises a polymer.108. The method according to any one of embodiments 67 to 107, wherein the polymer is high-density polyethylene. 109. The method according to any one of embodiments 67 to 108, wherein the substrate includes a mesh structure made from high-density polyethylene. 110. The method according to any one of embodiments 67 to 109, wherein the bandage includes a mesh structure made from high-density polyethylene. 111. The method according to any one of embodiments 67 to 110, wherein the bandage includes an absorbent layer between two mesh structures made from high-density polyethylene. 112. The method according to any one of embodiments 67 to 111, wherein the deposition includes sputtering. 113. The method according to any one of embodiments 67 to 112, wherein the sputtering is DC magnetron sputtering. 114. The method according to any one of embodiments 67 to 113, wherein the sputtering power is about 190 watts to about 950 watts. 115. The method according to any one of embodiments 67 to 114, wherein the sputtering power is about 380 watts to about 760 watts. 116. The method according to any one of embodiments 67 to 115, wherein the sputtering power is approximately 571 watts. 117. A method for preparing a metal matrix composite material, comprising the step of depositing one or more metals and metal oxides on a substrate in a deposition chamber in the presence of one or more combinations of inert gases and oxygen gases, wherein the deposition of at least one metal and metal oxide originates from a source, the source being at least 5 cm away from the substrate. 118. The method according to embodiment 117, comprising the step of evacuating the deposition chamber before deposition. 119. The method according to embodiment 117 or 118, wherein the evacuating step comprises reducing the internal pressure of the deposition chamber to approximately 10⁻⁷, 10⁻⁶, 10⁻⁵, 10⁻⁴, 10⁻³, 0.01, 0.1, 1, 10, 100, 760 tors, or below atmospheric pressure. 120. The method according to any one of embodiments 117 to 119, further comprising the step of repressurizing the deposit chamber to between approximately 5 milliliters and approximately 50 milliliters. 121. The method according to any one of embodiments 117 to 120, further comprising the step of repressurizing the deposit chamber to between approximately 35 milliliters and approximately 45 milliliters. 122. The method according to any one of embodiments 117 to 121, further comprising the step of repressurizing the deposit chamber to approximately 40 milliliters.123. The method according to any one of embodiments 117 to 122, wherein liquid water is injected into an inert gas flow outside the deposit chamber and enters the deposit chamber as water vapor. 124. The method according to any one of embodiments 117 to 123, wherein liquid water is injected into an inert gas flow upstream of a mass flow controller of inert gas. 125. The method according to any one of embodiments 117 to 124, wherein liquid water is injected into the inert gas flow by a syringe pump. 126. The method according to any one of embodiments 117 to 125, wherein liquid water is injected into the inert gas flow by a syringe pump at a flow rate between approximately 0.5 μl / min and approximately 11 μl / min. 127. The method according to any one of embodiments 117 to 126, wherein liquid water is injected into the inert gas flow by a syringe pump at a flow rate between approximately 7 μl / min and approximately 10 μl / min. 128. The method according to any one of embodiments 117 to 127, wherein liquid water is injected into the inert gas flow at a flow rate of approximately 9 μl / min by a syringe pump. 129. The method according to any one of embodiments 117 to 128, wherein the inert gas mass flow controller controls the flow rate of the inert gas entering the deposit chamber between approximately 100 SCCM and approximately 600 SCCM. 130. The method according to any one of embodiments 117 to 129, wherein the inert gas mass flow controller controls the flow rate of the inert gas entering the deposit chamber between approximately 350 SCCM and approximately 450 SCCM. 131. The method according to any one of embodiments 117 to 130, wherein the oxygen gas mass flow controller controls the flow rate of the oxygen gas entering the deposit chamber between approximately 0.1 SCCM and approximately 100 SCCM. 132. The method according to any one of embodiments 117 to 131, wherein the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 1 SCCM and approximately 20 SCCM. 133. The method according to any one of embodiments 117 to 132, wherein the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 5 SCCM and approximately 10 SCCM. 134. The method according to any one of embodiments 117 to 133, wherein the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber to approximately 8 SCCM.135. The method according to any one of embodiments 117 to 134, wherein the liquid water is heated to a temperature between approximately 20°C and approximately 80°C in the region between the syringe pump and the mass flow controller. 136. The method according to any one of embodiments 117 to 135, wherein the liquid water is heated to a temperature between approximately 40°C and approximately 60°C in the region between the syringe pump and the mass flow controller. 137. The method according to any one of embodiments 117 to 136, wherein the liquid water is heated to a temperature between approximately 50°C in the region between the syringe pump and the mass flow controller. 138. The method according to any one of embodiments 117 to 137, wherein the distance is between approximately 1 cm and approximately 20 cm. 139. The method according to any one of embodiments 117 to 138, wherein the distance is between approximately 5 cm and approximately 15 cm. 140. The method according to any one of embodiments 117 to 139, wherein the distance is approximately 10 cm. 141. The method according to any one of embodiments 117 to 140, wherein the step of reducing the internal pressure of the deposition chamber to about 10⁻⁷, 10⁻⁶, 10⁻⁵, 10⁻⁴, 10⁻³, 0.01, 0.1, 1, 10, 100, 760 Torr, or below atmospheric pressure. 142. The method according to any one of embodiments 117 to 141, wherein the metal is a precious metal. 143. The method according to any one of embodiments 117 to 142, wherein the precious metal is silver, gold, platinum, palladium, or a combination thereof. 144. The method according to any one of embodiments 117 to 143, comprising the step of depositing at least two metals on a substrate. 145. The method according to any one of embodiments 117 to 144, wherein at least two metals include silver and gold. 146. The method according to any one of embodiments 117 to 145, wherein at least two metals include silver and gold, with silver present in a 65% proportion and gold present in a 35% proportion. 147. The method according to any one of embodiments 117 to 145, wherein at least two metals include silver and gold, with silver present in a 35% proportion and gold present in a 65% proportion. 148. The method according to any one of embodiments 117 to 147, further comprising the step of depositing an additional metal or metal oxide on a substrate. 149. The method according to any one of embodiments 117 to 148, wherein one or more gases further include an inert gas.150. The method according to any one of Embodiments 117 to 149, wherein the inert gas is argon. 151. The method according to any one of Embodiments 117 to 150, wherein the internal pressure of the deposition chamber during deposition is maintained between about 5 milliliters and about 50 milliliters. 152. The method according to any one of Embodiments 117 to 151, wherein the internal pressure of the deposition chamber during deposition is maintained between about 35 milliliters and about 45 milliliters. 153. The method according to any one of Embodiments 117 to 152, wherein the internal pressure of the deposition chamber during deposition is maintained at about 40 milliliters. 154. Any of Embodiments 117 to 153, wherein the substrate is solid. or one method thereof. 155. The method according to any one of embodiments 117 to 154, wherein the solid comprises a metal foil, glass, or silicon. 156. The method according to any one of embodiments 117 to 155, wherein the substrate exhibits low gas emission. 157. The method according to any one of embodiments 117 to 156, wherein the substrate is an implant. 158. The method according to any one of embodiments 117 to 157, wherein the implant is a stent. 159. The method according to any one of embodiments 117 to 158, wherein the stent is a metal stent. 160. The method according to any one of embodiments 117 to 159, wherein the substrate comprises a polymer. 161. The method according to any one of embodiments 117 to 160, wherein the polymer is high-density polyethylene. 162. The method according to any one of embodiments 117 to 161, wherein the substrate comprises a mesh structure made from high-density polyethylene. 163. The method according to any one of embodiments 117 to 162, wherein the bandage comprises a mesh structure made from high-density polyethylene. 164. The method according to any one of embodiments 117 to 163, wherein the bandage comprises an absorbent layer between two mesh structures made of high-density polyethylene. 165. The method according to any one of embodiments 117 to 164, wherein the deposition comprises sputtering. 166. The method according to any one of embodiments 117 to 165, wherein the sputtering is DC magnetron sputtering. 167. The method according to any one of embodiments 117 to 166, wherein the sputtering power is approximately 190 watts to approximately 950 watts. 168. The method according to any one of embodiments 117 to 167, wherein the sputtering power is approximately 380 watts to approximately 760 watts. 169. The method according to any one of embodiments 117 to 168, wherein the sputtering power is approximately 571 watts. 170. A method for preparing a metal matrix composite material, comprising the step of depositing one or more metals and metal oxides on a substrate in a deposition chamber in the presence of an inert gas, oxygen gas, and water vapor. 171. The method according to Embodiment 170, wherein water vapor is produced as liquid water injected into an inert gas flow outside the deposit chamber. 172. The method according to Embodiment 170 or 171, wherein the injection is performed upstream of the deposit chamber.173. The method according to any one of embodiments 170 to 172, wherein liquid water is injected into an inert gas stream upstream of a mass flow controller. 174. The method according to any one of embodiments 170 to 173, wherein the mass flow controller is configured for the inert gas. 175. The method according to any one of embodiments 170 to 174, wherein liquid water is injected into the inert gas stream by a syringe pump. 176. The method according to any one of embodiments 170 to 175, wherein liquid water is injected into the inert gas stream by a syringe pump at a flow rate between approximately 0.5 μl / min and approximately 11 μl / min. 177. The method according to any one of embodiments 170 to 176, wherein liquid water is injected into the inert gas stream by a syringe pump at a flow rate between approximately 7 μl / min and approximately 10 μl / min. 178. The method according to any one of embodiments 170 to 177, wherein liquid water is injected into the inert gas flow at a flow rate of approximately 9 μl / min by a syringe pump. 179. The method according to any one of embodiments 170 to 178, wherein the inert gas mass flow controller controls the flow rate of the inert gas entering the deposit chamber between approximately 100 SCCM and approximately 600 SCCM. 180. The method according to any one of embodiments 170 to 179, wherein the inert gas mass flow controller controls the flow rate of the inert gas entering the deposit chamber between approximately 350 SCCM and approximately 450 SCCM. 181. The method according to any one of embodiments 170 to 180, wherein the oxygen gas mass flow controller controls the flow rate of the oxygen gas entering the deposit chamber between approximately 0.1 SCCM and approximately 100 SCCM. 182. The method according to any one of embodiments 170 to 181, wherein the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 1 SCCM and approximately 20 SCCM. 183. The method according to any one of embodiments 170 to 182, wherein the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber between approximately 5 SCCM and approximately 10 SCCM. 184. The method according to any one of embodiments 170 to 183, wherein the oxygen gas mass flow controller controls the flow rate of oxygen gas entering the deposit chamber to approximately 8 SCCM.185. The method according to any one of embodiments 170 to 184, wherein the liquid water is heated to a temperature between approximately 20°C and approximately 80°C in the region between the syringe pump and the mass flow controller. 186. The method according to any one of embodiments 170 to 185, wherein the liquid water is heated to a temperature between approximately 40°C and approximately 60°C in the region between the syringe pump and the mass flow controller. 187. The method according to any one of embodiments 170 to 186, wherein the liquid water is heated to a temperature between approximately 50°C in the region between the syringe pump and the mass flow controller. 188. The method according to any one of embodiments 170 to 187, wherein the distance is between approximately 1 cm and approximately 20 cm. 189. The method according to any one of embodiments 170 to 188, wherein the distance is between approximately 5 cm and approximately 15 cm. 190. The method according to any one of embodiments 170 to 189, wherein the distance is approximately 10 cm. 191. The method according to any one of Embodiments 170 to 190, wherein the step of reducing the internal pressure of the deposition chamber to about 10⁻⁷, 10⁻⁶, 10⁻⁵, 10⁻⁴, 10⁻³, 0.01, 0.1, 1, 10, 100, 760 Torr, or below atmospheric pressure. 192. The method according to any one of Embodiments 170 to 191, wherein the metal is a precious metal. 193. The method according to any one of Embodiments 170 to 192, wherein the precious metal is silver, gold, platinum, palladium, or a combination thereof. 194. The method according to any one of Embodiments 170 to 193, comprising the step of depositing at least two metals on a substrate. 195. The method according to any one of Embodiments 170 to 194, wherein at least two metals include silver and gold. 196. The method according to any one of Embodiments 170 to 195, wherein at least two metals include silver and gold, with silver present in a 65% proportion and gold present in a 35% proportion. 197. The method according to any one of Embodiments 170 to 195, wherein at least two metals include silver and gold, with silver present in a 35% proportion and gold present in a 65% proportion. 198. The method according to any one of Embodiments 170 to 197, further comprising the step of depositing an additional metal or metal oxide on a substrate. 199. The method according to any one of Embodiments 170 to 198, wherein one or more gases further include an inert gas.200. The method according to any one of Embodiments 170 to 199, wherein the inert gas is argon. 201. The method according to any one of Embodiments 170 to 200, wherein the internal pressure of the deposition chamber during deposition is maintained between about 5 milliliters and about 50 milliliters. 202. The method according to any one of Embodiments 170 to 201, wherein the internal pressure of the deposition chamber during deposition is maintained between about 35 milliliters and about 45 milliliters. 203. The method according to any one of Embodiments 170 to 202, wherein the internal pressure of the deposition chamber during deposition is maintained at about 40 milliliters. 204. The method according to any one of Embodiments 170 to 203, wherein the substrate is solid. 205. The method according to any one of Embodiments 170 to 204, wherein the solid comprises metal foil, glass, or silicon. 206. The method according to any one of Embodiments 170 to 205, wherein the substrate exhibits low gas emission. 207. The method according to any one of Embodiments 170 to 206, wherein the substrate is implantable. 208. The method according to any one of Embodiments 170 to 207, wherein the implant is a stent. 209. The method according to any one of Embodiments 170 to 208, wherein the stent is a metal stent. 210. The method according to any one of Embodiments 170 to 209, wherein the substrate comprises a polymer. 211. The method according to any one of Embodiments 170 to 210, wherein the polymer is high-density polyethylene. 212. The method according to any one of Embodiments 170 to 211, wherein the substrate comprises a mesh structure made from high-density polyethylene. 213. The method according to any one of Embodiments 170 to 212, wherein the bandage comprises a mesh structure made from high-density polyethylene. 214. The method according to any one of Embodiments 170 to 213, wherein the bandage comprises an absorbent layer between two mesh structures made from high-density polyethylene. 215. The method according to any one of Embodiments 170 to 214, wherein the deposition comprises sputtering. 216. The method according to any one of embodiments 170 to 215, wherein the sputtering is DC magnetron sputtering. 217. The method according to any one of embodiments 170 to 216, wherein the sputtering power is about 190 watts to about 950 watts. 218. The method according to any one of embodiments 170 to 217, wherein the sputtering power is about 380 watts to about 760 watts.219. The method according to any one of embodiments 170 to 218, wherein the sputtering power is approximately 571 watts. 220. A metal matrix composite material comprising metallic grain boundary atoms, a metal oxide, and metallic crystal grains, wherein the median diameter of the crystal grains is between approximately 2 nm and approximately 15 nm, and the grain boundary atoms constitute approximately 50 to approximately 20% per unit surface area of ​​the metal matrix composite material. 221. The metal matrix composite material according to embodiment 220, comprising metallic grain boundary atoms, a metal oxide, oxygen, water, and metallic crystal grains, wherein the median diameter of the crystal grains is between approximately 2 nm and approximately 15 nm, the grain boundary atoms constitute approximately 50 to approximately 20% per unit surface area of ​​the metal matrix composite material, and the oxygen constitutes at least 2% by weight of the metal matrix composite material. 222. A metal matrix composite material according to Embodiment 220 or 221, comprising metal grain boundary atoms, metal oxides, oxygen, water, and metal crystal grains, wherein the median diameter of the crystal grains is between approximately 2 nm and approximately 15 nm, the grain boundary atoms constitute approximately 50% to approximately 20% per unit surface area of ​​the metal matrix composite material, and the water constitutes less than 4% by weight of the metal matrix composite material. 223. A metal matrix composite material according to any one of Embodiments 220 to 222, wherein the median diameter of the crystal grains is between approximately 2 nm and approximately 15 nm, and the metal grain boundary atoms constitute approximately 50% to approximately 20% per unit surface area of ​​the metal matrix composite material. 224. A metal matrix composite material according to any one of Embodiments 220 to 223, wherein the median diameter of the crystal grains is between approximately 5 nm and approximately 15 nm, and the metal grain boundary atoms constitute approximately 40% to approximately 20% per unit surface area of ​​the metal matrix composite material. 225. A metal matrix composite material according to any one of embodiments 220 to 224, comprising grain boundary atoms of a second metal and crystal grains of a second metal having a median diameter between approximately 2 nm and approximately 15 nm, wherein the grain boundary atoms of the second metal constitute approximately 50 to approximately 20% per unit surface area of ​​the metal matrix composite material. 226. A metal matrix composite material according to any one of embodiments 220 to 225, comprising Ag2CO3.227. A method for preparing a metal matrix composite material, comprising the step of depositing one or more metals and metal oxides on a substrate in a deposition chamber in the presence of water vapor and one or more gases including oxygen gas, wherein the deposition of at least one metal and metal oxide is generated from a source at a distance of at least 5 cm from the substrate, and further comprising the step of reducing the internal pressure of the deposition chamber to below about 10⁻⁷ Torr within 24 hours, 12 hours, 6 hours, and 3 hours prior to deposition. 228. A metal matrix composite material comprising metal grain boundary atoms, metal oxides, oxygen, water, and metal crystal grains with a median diameter between about 2 nm and about 15 nm, wherein the grain boundary atoms comprise about 50 to about 20% per unit surface area of ​​the metal matrix composite material. A metal matrix composite material comprising a step of depositing one or more metals and metal oxides onto a substrate in a deposition chamber in the presence of water vapor and one or more gases including oxygen gas, wherein the deposition of at least one metal and metal oxide originates from a source at a distance of at least 5 cm from the substrate, and further, the method does not include a step of reducing the internal pressure of the deposition chamber to below about 10⁻⁷ Torr within 24 hours, 12 hours, 6 hours, or 3 hours prior to deposition. 229. The metal matrix composite material according to Embodiment 228, wherein the internal pressure of the deposition chamber during deposition is maintained between about 5 milliliters and about 50 milliliters. 230. The metal matrix composite material according to Embodiment 228 or 229, wherein the internal pressure of the deposition chamber during deposition is maintained between about 35 milliliters and about 45 milliliters. 231. The metal matrix composite material according to any one of Embodiments 228 to 230, wherein the internal pressure of the deposition chamber during deposition is maintained at about 40 milliliters. 232. A metal matrix composite material according to any one of embodiments 228 to 231, wherein the oxygen gas comprises molecular oxygen gas. 233. A metal matrix composite material according to embodiment 232, wherein the molecular oxygen gas comprises any form of molecular oxygen gas. 234. A metal matrix composite material according to embodiment 233, wherein the molecular oxygen gas is selected from the group consisting of O2, O3, O3+, O2+, O2-, O3, O, O+, O-, ionized ozone, metastable excited oxygen, free electrons, H2O2, and OH. [Examples]

[0070] The following examples are provided for illustrative purposes only and are not intended to limit the scope of the present invention.

[0071] Example 1 Working gas: 96% argon with water vapor (water column was 20°C), 4% oxygen

[0072] Power: 0.9 amps

[0073] Target: 99.99% silver

[0074] Target dimensions: 20.25”X5”X0.25”

[0075] Sputtering distance (cathode to substrate): 10cm

[0076] Gas flow rate: Ar + water vapor 384 SCCM, O2 16 SCCM

[0077] Operating gas pressure: 40 mtorr

[0078] Water temperature: 20℃

[0079] Plasma generation color: Purple

[0080] Test conditions: A bandage (3) was prepared by sandwiching a 1 square inch piece around a 1 square inch single layer of woven cotton gauze (Figure 1). A 6-hour culture (1.6 × 10⁶) of Gram-negative enterobacteria grown in TSB at 37°C was placed in this bandage. 8 250 μL of CFU was inoculated. The bandage was incubated at 37°C for 30 minutes. Then, the bandage was placed in 2.25 mL of saline thioglycolic acid solution to inactivate the silver, and diluted for enumeration. 5 × 10 4 The sample was collected. The logarithmic decrease was 8.2 - 4.7 = 3.5. This indicates that the bandage was antiseptic, meaning the logarithmic decrease was greater than 3.

[0081] III. Process

[0082] This is a physical vapor deposition process using a composite working gas mixture. Working gas composition: argon (80-99.9%), oxygen (0-20%), and water vapor. The water vapor is controlled by a water temperature of 20°C in an argon flow line, which controls the water vapor pressure and allows for increasing or decreasing the amount of water involved in the operation as needed.

[0083] Example 2 Process parameters:

[0084] Working gas: 96% argon with water vapor (water column was 20°C), 4% oxygen

[0085] Power: 0.9 amps

[0086] Target: 99.99% silver

[0087] Target dimensions: 20.25”X5”X0.25”

[0088] Sputtering distance (cathode to substrate): 10cm

[0089] Gas flow rate: Ar + water vapor 384 SCCM, O2 16 SCCM

[0090] Operating gas pressure: 40 mtorr

[0091] Water temperature: 70℃

[0092] Plasma generation color: Pink

[0093] Test conditions: A bandage (3) was prepared by sandwiching a 1 square inch piece around a 1 square inch single layer of woven cotton gauze (Figure 1). A 6-hour culture (1.6 × 10⁶) of Gram-negative enterobacteria grown in TSB at 37°C was placed in this bandage. 8250 μL of CFU was inoculated. The bandage was incubated at 37°C for 30 minutes. Then, the bandage was placed in 2.25 mL of saline thioglycolic acid solution to inactivate the silver, and diluted for enumeration. 7 × 10 5 The group was collected. The logarithmic decrease was 3.4. This indicates that the bandage was antibacterial, meaning the logarithmic decrease was greater than 3.

[0094] This is a physical vapor deposition process using a composite working gas mixture. Working gas composition: argon (80-99.9%), oxygen (0-20%), and water vapor. The water vapor is controlled by a water temperature of 70°C in an argon flow line, which controls the water vapor pressure and allows for increasing or decreasing the amount of water involved in the operation as needed.

[0095] Example 3: Effect of water on the concentration of ammonium hydroxide-soluble silver This embodiment is included to demonstrate that an antimicrobial coating cannot be applied to a commercially available high-density polyethylene (HDPE) mesh by DC magnetron sputtering of silver when water is injected into the deposition chamber. The mesh was coated on the surface by DC magnetron sputtering of 99.9% Ag under the following conditions: The working gas used was high-purity water (final concentration 100 wt%) added directly to the vacuum chamber via a microvalve. Water was injected into the chamber at 35 μL / min. The sputtering power was 1.5 amperes and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular and measured 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The run time was 15 minutes and the HDPE mesh was static.

[0096] The antibacterial effect of the coating was tested using a logarithmic reduction test. A bacterial inoculum was prepared by inoculating 50 mL of calf serum with a 16-hour culture of Pseudomonas aeruginosa, and this was incubated for 16 hours. This resulted in a bacterial count of 1.05 × 10⁻⁶. 9CFU inoculum was produced. A bandage was prepared from two silver-coated HDPE pieces (2.5 × 2.5 cm) with a piece of cotton gauze (2.5 × 2.5 cm) in between. The bandage was placed on a sterile plastic piece (3.2 × 3.2 cm) with the lid of a petri dish inverted in a Class 2 laminar-flow hood. 200 μL of inoculum was applied to the bandage in the petri dish, then covered with the second plastic piece (3.2 × 3.2 cm), and incubated at 37°C for 1 hour. The bandage, containing the plastic base piece and the coating piece with bacteria, was then inactivated by placing it in 1.8 mL of sodium thioglycolate saline (STS), then diluted in a dish with peptone water, and seeded onto Mueller-Hinton agar. The plate was examined after 24 hours of incubation, and the total bacterial colony-forming units were calculated.

[0097] Equation 1.

[0098] 1 / (IDxSDxFD)X50XCFU=CFU / mL

[0099] In the formula, ID is the initial dilution, SD is the later dilution, FD is the final dilution, 50 is converted to mL, and CFU is the colony-forming unit counted at the dilution used in the calculation.

[0100] Next, the CFU / mL values ​​were converted to logarithmic numbers. The logarithmic reduction was calculated by subtracting the logarithm of the recovered CFU from the logarithm of the inoculated material. A logarithmic reduction of more than 3 was considered bactericidal.

[0101] To determine the total amount of silver in the bandage, one square inch of bandage was dissolved in 20 mL of a 50% nitric acid solution in distilled water over 20 minutes, then diluted in an additional 20 mL of distilled water, and analyzed using an atomic absorption spectrometer (AAS).

[0102] To estimate the amount of silver oxide in the bandage, and to determine the amount of ammonium hydroxide-available silver, one square inch of the bandage was dissolved in 20 mL of ammonium hydroxide over 10 minutes. 10 mL of this solution was then diluted in 40 mL of water and analyzed using AAS.

[0103] Bandages prepared with 35 μL / min of water contained a total of 1012 μg / square inch of Ag, including 220 μg / square inch of ammonium hydroxide-soluble Ag, equivalent to 22% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was less than 2, and the silver coating deposited in a moist environment was found to be non-bactericidal in calf serum.

[0104] Simple sputtering in water does not produce high concentrations of ammonium hydroxide-available silver or antimicrobial activity.

[0105] Example 4: Effect of water (0-8 μL / min) and argon on the concentration of ammonium hydroxide-available silver This embodiment is included to demonstrate that an antimicrobial coating cannot be applied to a commercially available high-density polyethylene (HDPE) mesh by silver DC magnetron sputtering when water is injected into Ar upstream of the MFC via a syringe pump before being placed in the deposition chamber. The mesh was coated on the surface by DC magnetron sputtering of 99.9% Ag under the following conditions: The working gas used was high-purity commercially available Ar (100 wt% final concentration) added to the vacuum chamber via a mass flow controller. Water was injected into the Ar stream at flow rates of 0, 2, 4, 6, and 8 μL / min. A stainless steel pipe was heated to 50°C between the inlet and the MFC to maintain the water in a gaseous state. The sputtering power was 1.8 amps, the argon flow rate was 400 SCCM, and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular and measured 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The execution time was 30 minutes, during which the HDPE mesh moved at a rate of 15 cm / min.

[0106] The antibacterial effect of the coating was tested using a logarithmic reduction test. A bacterial inoculum was prepared by inoculating 50 mL of calf serum with a 16-hour culture of Pseudomonas aeruginosa, and this was incubated for 16 hours. This resulted in a bacterial count of 1.05 × 10⁻⁶. 9CFU inoculum was produced. A bandage was prepared from two silver-coated HDPE pieces (2.5 × 2.5 cm) with a piece of cotton gauze (2.5 × 2.5 cm) in between. The bandage was placed on a sterile plastic piece (3.2 × 3.2 cm) with the lid of a petri dish inverted in a Class 2 laminar-flow hood. 200 μL of inoculum was applied to the bandage in the petri dish, then covered with the second plastic piece (3.2 × 3.2 cm), and incubated at 37°C for 1 hour. The bandage, containing the plastic base piece and the coating piece with bacteria, was then inactivated by placing it in 1.8 mL of sodium thioglycolate saline (STS), then diluted in a dish with peptone water, and seeded onto Mueller-Hinton agar. The plate was examined after 24 hours of incubation, and the total bacterial colony-forming units were calculated.

[0107] Equation 1.

[0108] 1 / (IDxSDxFD)X50XCFU=CFU / mL

[0109] In the formula, ID is the initial dilution, SD is the later dilution, FD is the final dilution, 50 is converted to mL, and CFU is the colony-forming unit counted at the dilution used in the calculation.

[0110] Next, the CFU / mL values ​​were converted to logarithmic numbers. The logarithmic reduction was calculated by subtracting the logarithm of the recovered CFU from the logarithm of the inoculated material. A logarithmic reduction of more than 3 was considered bactericidal.

[0111] To determine the total amount of silver in the bandage, one square inch of bandage was dissolved in 20 mL of a 50% nitric acid solution in distilled water over 20 minutes, then diluted in an additional 20 mL of distilled water, and analyzed using an atomic absorption spectrometer (AAS).

[0112] To estimate the amount of silver oxide in the bandage, and to determine the amount of ammonium hydroxide-available silver, one square inch of the bandage was dissolved in 20 mL of ammonium hydroxide over 10 minutes. 10 mL of this solution was then diluted in 40 mL of water and analyzed using AAS.

[0113] The results are summarized in Figures 2A and 2B.

[0114] Bandages prepared with 0% O2 and 8 μL / min of water contained a total of 4320 μg / m² of Ag, including 136 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 3.2% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 2.2, indicating that the silver coating deposited in a moist environment was not bactericidal in calf serum.

[0115] Bandages prepared with 0% O2 and 6 μL / min of water contained a total of 4160 μg / m² of Ag, including 150 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 2.4% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 2.1, indicating that the silver coating deposited in a moist environment was not bactericidal in calf serum.

[0116] Bandages prepared with 0% O2 and 4 μL / min of water contained a total of 4800 μg / square inch of Ag, including 102 μg / square inch of ammonium hydroxide-soluble Ag, equivalent to 2.1% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 2.1, indicating that the silver coating deposited in a moist environment was not bactericidal in calf serum.

[0117] Bandages prepared with 0% O2 and 2 μL / min of water contained a total of 4960 μg / m² of Ag, including 104 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 2.1% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 2.7, indicating that the silver coating deposited in a moist environment was not bactericidal in calf serum.

[0118] Bandages prepared with 0% O2 and 0 μL / min of water contained a total of 5040 μg / m² of Ag, including 168 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 3.3% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 2.8, indicating that the silver coating deposited in a moist environment was not bactericidal in calf serum.

[0119] Simple sputtering in a mixture of argon and water does not produce high concentrations of ammonium hydroxide-available silver or antimicrobial activity.

[0120] Example 5: Effect of water (9-33 μL / min) and argon on the concentration of ammonium hydroxide-available silver This embodiment is included to demonstrate that an antimicrobial coating cannot be applied to a commercially available high-density polyethylene (HDPE) mesh by silver DC magnetron sputtering when water is injected into Ar upstream of the MFC via a syringe pump before being placed in the deposition chamber. The mesh was coated on the surface by DC magnetron sputtering of 99.9% Ag under the following conditions: The working gas used was high-purity commercially available Ar (100 wt% final concentration) added to the vacuum chamber via a mass flow controller. Water was injected into the Ar stream at flow rates of 9, 20, and 33 μL / min. A stainless steel pipe was heated to 50°C between the inlet and the MFC to maintain the water in a gaseous state. The sputtering power was 1.5 amps, the argon flow rate was 400 SCCM, and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular and measured 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The execution time was 30 minutes, and the HDPE mesh moved at a rate of 15 cm / minute.

[0121] The antibacterial effect of the coating was tested using a logarithmic reduction test. A bacterial inoculum was prepared by inoculating 50 mL of calf serum with a 16-hour culture of Pseudomonas aeruginosa, and this was incubated for 16 hours. This resulted in a bacterial count of 1.05 × 10⁻⁶. 9CFU inoculum was produced. A bandage was prepared from two silver-coated HDPE pieces (2.5 × 2.5 cm) with a piece of cotton gauze (2.5 × 2.5 cm) in between. The bandage was placed on a sterile plastic piece (3.2 × 3.2 cm) with the lid of a petri dish inverted in a Class 2 laminar-flow hood. 200 μL of inoculum was applied to the bandage in the petri dish, then covered with the second plastic piece (3.2 × 3.2 cm), and incubated at 37°C for 1 hour. The bandage, containing the plastic base piece and the coating piece with bacteria, was then inactivated by placing it in 1.8 mL of sodium thioglycolate saline (STS), then diluted in a dish with peptone water, and seeded onto Mueller-Hinton agar. The plate was examined after 24 hours of incubation, and the total bacterial colony-forming units were calculated.

[0122] Equation 1.

[0123] 1 / (IDxSDxFD)X50XCFU=CFU / mL

[0124] In the formula, ID is the initial dilution, SD is the later dilution, FD is the final dilution, 50 is converted to mL, and CFU is the colony-forming unit counted at the dilution used in the calculation.

[0125] Next, the CFU / mL values ​​were converted to logarithmic numbers. The logarithmic reduction was calculated by subtracting the logarithm of the recovered CFU from the logarithm of the inoculated material. A logarithmic reduction of more than 3 was considered bactericidal.

[0126] To determine the total amount of silver in the bandage, one square inch of bandage was dissolved in 20 mL of a 50% nitric acid solution in distilled water over 20 minutes, then diluted in an additional 20 mL of distilled water, and analyzed using an atomic absorption spectrometer (AAS).

[0127] To estimate the amount of silver oxide in the bandage, and to determine the amount of ammonium hydroxide-available silver, one square inch of the bandage was dissolved in 20 mL of ammonium hydroxide over 10 minutes. 10 mL of this solution was then diluted in 40 mL of water and analyzed using AAS.

[0128] The results are summarized in Figures 3A and 3B.

[0129] Bandages prepared with 0% O2 and 9 μL / min of water contained a total of 4320 μg / m² of Ag, including 136 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 1% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was less than 2, indicating that the silver coating deposited in a moist environment was not bactericidal in calf serum.

[0130] Bandages prepared with 0% O2 and 20 μL / min of water contained a total of 4160 μg / square inch of Ag, including 150 μg / square inch of ammonium hydroxide-soluble Ag, equivalent to 3% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was less than 2, and the silver coating deposited in a moist environment was found to be non-bactericidal in calf serum.

[0131] Bandages prepared with 0% O2 and 33 μL / min of water contained a total of 4800 μg / square inch of Ag, including 102 μg / square inch of ammonium hydroxide-soluble Ag, equivalent to 8% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was less than 2, indicating that the silver coating deposited in a moist environment was not bactericidal in calf serum.

[0132] Simple sputtering in a mixture of argon and water does not produce high concentrations of ammonium hydroxide-available silver or antimicrobial activity.

[0133] Example 6: Effect of water (1-9 μL / min) and argon on the concentration of ammonium hydroxide-available silver This embodiment is included to demonstrate that an antimicrobial coating can be applied to a commercially available high-density polyethylene (HDPE) mesh by DC magnetron sputtering of silver when water is injected into Ar upstream of the MFC via a syringe pump before being placed in the deposition chamber. The mesh was coated on the surface by DC magnetron sputtering of 99.9% Ag under the following conditions: The working gas used was high-purity commercially available Ar / O2 (final concentration 98 / 2 wt%) added to the vacuum chamber via a mass flow controller. Water was injected into the Ar stream at flow rates of 1, 3, 5, 7, and 9 μL / min. A stainless steel pipe was heated to 50°C between the inlet and the MFC to maintain the water in a gaseous state. The sputtering power was 570 watts (1.5 amps at 380 volts), the argon / O2 flow rate was 392 / 8 SCCM, and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular, with measurements of 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The run time was 30 minutes, during which the HDPE mesh moved at a rate of 15 cm / min.

[0134] The antibacterial effect of the coating was tested using a logarithmic reduction test. Bacterial inoculum was prepared by inoculating 50 mL of calf serum with a 16-hour culture of Pseudomonas aeruginosa, and this was incubated for 16 hours. This produced 1.05 × 10⁹ CFU of inoculum. A bandage was prepared from two silver-coated HDPE pieces (2.5 × 2.5 cm) with a piece of cotton gauze (2.5 × 2.5 cm) in between. The bandage was placed on a sterile plastic piece (3.2 × 3.2 cm) with the lid of a petri dish inverted in a Class 2 laminar-flow hood. 200 μL of inoculum was applied to the bandage in the petri dish, and then the second plastic piece (3.2 × 3.2 cm) was placed over it, and the mixture was incubated at 37°C for 1 hour. Next, bandages containing a plastic base piece and a covering piece with bacteria were placed in 1.8 mL of sodium thioglycolate saline (STS) to inactivate the silver, then diluted in peptone water and inoculated onto Mueller-Hinton agar. After 24 hours of incubation, the plates were examined and the total bacterial colony-forming units were calculated.

[0135] Equation 1.

[0136] 1 / (IDxSDxFD)X50XCFU=CFU / mL

[0137] In the formula, ID is the initial dilution, SD is the later dilution, FD is the final dilution, 50 is converted to mL, and CFU is the colony-forming unit counted at the dilution used in the calculation.

[0138] Next, the CFU / mL values ​​were converted to logarithmic numbers. The logarithmic reduction was calculated by subtracting the logarithm of the recovered CFU from the logarithm of the inoculated material. A logarithmic reduction of more than 3 was considered bactericidal.

[0139] To determine the total amount of silver in the bandage, one square inch of bandage was dissolved in 20 mL of a 50% nitric acid solution in distilled water over 20 minutes, then diluted in an additional 20 mL of distilled water, and analyzed using an atomic absorption spectrometer (AAS).

[0140] To estimate the amount of silver oxide in the bandage, and to determine the amount of ammonium hydroxide-available silver, one square inch of the bandage was dissolved in 20 mL of ammonium hydroxide over 10 minutes. 10 mL of this solution was then diluted in 40 mL of water and analyzed using AAS.

[0141] The results are summarized in Figure 4.

[0142] Bandages prepared with 2% O2 and 9 μL / min of water contained a total of 6672 μg / square inch of Ag, including 1290 μg / square inch of ammonium hydroxide-soluble Ag, equivalent to 19% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa exceeded 7, and the silver coating deposited in a moist environment was found to be bactericidal in calf serum.

[0143] Bandages prepared with 2% O2 and 7 μL / min of water contained a total of 4032 μg / m² of Ag, including 1050 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 26% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was greater than 7, and the silver coating deposited in a moist environment was found to be bactericidal in calf serum.

[0144] Bandages prepared with 2% O2 and 5 μL / min of water contained a total of 5664 μg / square inch of Ag, including 1270 μg / square inch of ammonium hydroxide-soluble Ag, equivalent to 22% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa exceeded 7, and the silver coating deposited in a moist environment was found to be bactericidal in calf serum.

[0145] Bandages prepared with 2% O2 and 3 μL / min of water contained a total of 6856 μg / square inch of Ag, including 1620 μg / square inch of ammonium hydroxide-soluble Ag, equivalent to 24% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa exceeded 7, and the silver coating deposited in a moist environment was found to be bactericidal in calf serum.

[0146] Bandages prepared with 2% O2 and 1 μL / min of water contained a total of 4704 μg / square inch of Ag, including 1140 μg / square inch of ammonium hydroxide-soluble Ag, equivalent to 24% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa exceeded 7, and the silver coating deposited in a moist environment was found to be bactericidal in calf serum.

[0147] When water is added to a mixture of 98% argon and 2% oxygen, higher concentrations of silver-available ammonium hydroxide are not produced.

[0148] Example 7: Effects of water, oxygen, and argon on the concentration of ammonium hydroxide-soluble silver This embodiment is included to demonstrate that various antimicrobial activity can be generated on a commercially available high-density polyethylene (HDPE) mesh by DC magnetron sputtering of silver when water is injected into Ar upstream of the MFC via a syringe pump before being placed in the deposition chamber. Antimicrobial activity is determined from the ratio of Ar, O2, and water. The mesh surface was coated by DC magnetron sputtering of 99.9% Ag under the following conditions. The working gas used was high-purity commercially available Ar / O2 (final concentrations of 100 / 0, 99 / 2, 98 / 2, 97 / 3, and 96 / 4 wt%) added to the vacuum chamber via a mass flow controller (one for Ar, the other for O2). Water was injected into the Ar stream at a flow rate of 0 or 9 μL / min. A stainless steel pipe was heated to 50°C between the inlet and the MFC to maintain the water in a gaseous state. The sputtering power was 570 watts (1.5 amps at 380 volts), the argon / O2 flow rates were 396 / 4, 392 / 8, 388 / 12, and 384 / 16 SCCM, and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular, with measurements of 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The run time was 30 minutes, and the HDPE mesh moved at 15 cm / min.

[0149] The antibacterial effect of the coating was tested using a logarithmic reduction test. A bacterial inoculum was prepared by inoculating 50 mL of calf serum with a 16-hour culture of Pseudomonas aeruginosa, and this was incubated for 16 hours. This resulted in a bacterial count of 1.05 × 10⁻⁶. 9CFU inoculum was produced. A bandage was prepared from two silver-coated HDPE pieces (2.5 × 2.5 cm) with a piece of cotton gauze (2.5 × 2.5 cm) in between. The bandage was placed on a sterile plastic piece (3.2 × 3.2 cm) with the lid of a petri dish inverted in a Class 2 laminar-flow hood. 200 μL of inoculum was applied to the bandage in the petri dish, then covered with the second plastic piece (3.2 × 3.2 cm), and incubated at 37°C for 1 hour. The bandage, containing the plastic base piece and the coating piece with bacteria, was then inactivated by placing it in 1.8 mL of sodium thioglycolate saline (STS), then diluted in a dish with peptone water, and seeded onto Mueller-Hinton agar. The plate was examined after 24 hours of incubation, and the total bacterial colony-forming units were calculated.

[0150] Equation 1.

[0151] 1 / (IDxSDxFD)X50XCFU=CFU / mL

[0152] In the formula, ID is the initial dilution, SD is the later dilution, FD is the final dilution, 50 is converted to mL, and CFU is the colony-forming unit counted at the dilution used in the calculation.

[0153] Next, the CFU / mL values ​​were converted to logarithmic numbers. The logarithmic reduction was calculated by subtracting the logarithm of the recovered CFU from the logarithm of the inoculated material. A logarithmic reduction of more than 3 was considered bactericidal.

[0154] To determine the total amount of silver in the bandage, one square inch of bandage was dissolved in 20 mL of a 50% nitric acid solution in distilled water over 20 minutes, then diluted in an additional 20 mL of distilled water, and analyzed using an atomic absorption spectrometer (AAS).

[0155] To estimate the amount of silver oxide in the bandage, and to determine the amount of ammonium hydroxide-available silver, one square inch of the bandage was dissolved in 20 mL of ammonium hydroxide over 10 minutes. 10 mL of this solution was then diluted in 40 mL of water and analyzed using AAS.

[0156] The results are summarized in Figures 5A and 5B.

[0157] Bandages prepared with 0% O2 and 9 μL / min of water contained a total of 3212 μg / m² of Ag, including 56 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 1% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 2.4, indicating that the silver coating deposited in a moist environment was not bactericidal in calf serum.

[0158] Bandages prepared with 1% O2 and 9 μL / min of water contained a total of 2472 μg / m² of Ag, including 812 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 32% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 6.2, and the silver coating deposited in a moist environment was found to be bactericidal in calf serum.

[0159] Bandages prepared with 2% O2 and 9 μL / min of water contained a total of 3292 μg / m² of Ag, including 1290 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 39% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 6.0, and the silver coating deposited in a moist environment was found to be bactericidal in calf serum.

[0160] Bandages prepared with 3% O2 ​​and 9 μL / min of water contained a total of 2736 μg / m² of Ag, including 1730 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 65% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 6.3, and the silver coating deposited in a moist environment was found to be bactericidal in calf serum.

[0161] Bandages prepared with 4% O2 and 9 μL / min of water contained a total of 2988 μg / m² of Ag, including 2210 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 74% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 6.6, and the silver coating deposited in a moist environment was found to be bactericidal in calf serum.

[0162] Bandages prepared with 0% O2 and 0 μL / min of water contained a total of 2520 μg / square inch of Ag, including 85 μg / square inch of ammonium hydroxide-soluble Ag, equivalent to 3% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 2.1, indicating that the silver coating deposited in a moist environment was not bactericidal in calf serum.

[0163] Bandages prepared with 1% O2 and 0 μL / min of water contained a total of 2832 μg / m² of Ag, including 267 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 9% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 4.9, and the silver coating deposited in a moist environment was found to be bactericidal in calf serum.

[0164] Bandages prepared with 2% O2 and 0 μL / min of water contained a total of 2320 μg / m² of Ag, including 495 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 21% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 4.9, and the silver coating deposited in a moist environment was found to be bactericidal in calf serum.

[0165] Bandages prepared with 3% O2 ​​and 0 μL / min of water contained a total of 2932 μg / m² of Ag, including 653 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 22% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 5.0, and the silver coating deposited in a moist environment was found to be bactericidal in calf serum.

[0166] Bandages prepared with 4% O2 and 0 μL / min of water contained a total of 2644 μg / m² of Ag, including 698 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 26% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 5.0, and the silver coating deposited in a moist environment was found to be bactericidal in calf serum.

[0167] Increasing the amount of water added to the argon-oxygen mixture significantly increases the production of ammonium hydroxide-soluble silver. This increase far exceeds the additional results that might be predicted from the activity produced by sputtering with water alone or a mixture of water and Ar. Such changes in the chemical composition of the thin film, induced by the presence of water, result in a more than tenfold increase in antimicrobial activity, creating an unexpected synergistic effect.

[0168] Example 8: Column heated by adding water upstream of the MFC This embodiment is included to demonstrate an antimicrobial coating formed on a commercially available high-density polyethylene (HDPE) mesh containing water in the working gas by DC magnetron sputtering. The mesh surface was coated by DC magnetron sputtering with 99.9% pure silver under the following conditions. The working gas used was high-purity commercially available Ar and O2 (final concentration 99 / 1 wt%) added to a vacuum chamber via a separate mass flow controller. Argon was bubbled by passing it through a long stainless steel column (134 cm × 4.8 cm) heated with 1400 mls of HPLC-grade H2O before the mass flow controller. A thermostat-controlled electric heater was installed at the base of the column. The ambient temperature was maintained at 65°C ± 3°C, and the internal water temperature was 88°C ± 3°C. The sputtering power was 570 watts (1.5 amps at 380 volts), the argon flow rate was 396 SCCM, the O2 flow rate was 4 SCCM, and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular, with measured dimensions of 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The run time was 30 minutes, and the HDPE mesh remained stationary.

[0169] The antibacterial effect of the coating was tested using a logarithmic reduction test. Bacterial inoculum was prepared by inoculating 50 mL of calf serum with a 16-hour culture of Pseudomonas aeruginosa, and this was incubated for 16 hours. This produced 1 × 10⁹ CFU of inoculum. Bandages were prepared from two silver-coated HDPE pieces (2.5 × 2.5 cm) with a piece of cotton gauze (2.5 × 2.5 cm) in between. The bandages were placed on a sterile plastic piece (3.2 × 3.2 cm) with the lid of a petri dish inverted in a Class 2 laminar-flow hood. 200 μL of inoculum was applied to the bandage in the petri dish, and then the second plastic piece (3.2 × 3.2 cm) was placed over it, and the mixture was incubated at 37°C for 1 hour. Next, bandages containing a plastic base piece and a covering piece with bacteria were placed in 1.8 mL of sodium thioglycolate saline (STS) to inactivate the silver, then diluted in peptone water and inoculated onto Mueller-Hinton agar. After 24 hours of incubation, the plates were examined and the total bacterial colony-forming units were calculated.

[0170] Equation 1.

[0171] 1 / (IDxSDxFD)X50XCFU=CFU / mL

[0172] In the formula, ID is the initial dilution, SD is the later dilution, FD is the final dilution, 50 is converted to mL, and CFU is the colony-forming unit counted at the dilution used in the calculation.

[0173] Next, the CFU / mL values ​​were converted to logarithmic numbers. The logarithmic reduction was calculated by subtracting the logarithm of the recovered CFU from the logarithm of the inoculated material. A logarithmic reduction of more than 3 was considered bactericidal.

[0174] To determine the total amount of silver in the bandage, one square inch of bandage was dissolved in 20 mL of a 50% nitric acid solution in distilled water over 20 minutes, then diluted in an additional 20 mL of distilled water, and analyzed using an atomic absorption spectrometer (AAS).

[0175] To estimate the amount of silver oxide in the bandage, and to determine the amount of ammonium hydroxide-available silver, one square inch of the bandage was dissolved in 20 mL of ammonium hydroxide over 10 minutes. 10 mL of this solution was then diluted in 40 mL of water and analyzed using AAS.

[0176] The bandage contained a total of 5144 μg / m² of silver (Ag), equivalent to 2109 μg / m² of ammonium hydroxide-soluble silver (Ag), which is 41% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 6.9, and the silver coating was found to be bactericidal in calf serum.

[0177] Example 9: Column heated by adding water upstream of the MFC This embodiment is included to demonstrate that an antimicrobial coating formed on a commercially available high-density polyethylene (HDPE) mesh by DC magnetron sputtering was unaffected by the volume of water passing through before the argon entered the deposition chamber. The mesh surface was coated by DC magnetron sputtering of 99.9% pure silver under the following conditions. The working gases used were high-purity commercially available argon and O2 (final concentration 99 / 1 wt%) added to the vacuum chamber via a separate mass flow controller. Before the mass flow controller, argon was bubbled by passing it through a long stainless steel column (134 cm × 4.8 cm) heated with 1500 mls of HPLC-grade H2O. A thermostat-controlled electric heater was placed at the base of the column. The ambient temperature was maintained at 65°C ± 3°C, and the internal water temperature was 88°C ± 3°C. The sputtering power was 571 watts (1.5 amps at 380 volts), the argon flow rate was 396 SCCM, the O2 flow rate was 4 SCCM, and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular, with measured dimensions of 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The run time was 30 minutes, and the HDPE mesh remained stationary.

[0178] The antibacterial effect of the coating was tested using a logarithmic reduction test. A bacterial inoculum was prepared by inoculating 50 mL of calf serum with a 16-hour culture of Pseudomonas aeruginosa, and this was incubated for 16 hours. This resulted in a bacterial count of 1 × 10⁻⁶. 9 CFU inoculum was produced. Bandages were prepared from two silver-coated HDPE pieces (2.5 × 2.5 cm) with a piece of cotton gauze (2.5 × 2.5 cm) in between. The bandages were placed on a sterile plastic piece (3.2 × 3.2 cm) with the lid of a petri dish inverted in a Class 2 laminar-flow hood. 200 μL of inoculum was applied to the bandage in the petri dish, then covered with the second plastic piece (3.2 × 3.2 cm), and incubated at 37°C for 1 hour. The bandages containing the plastic base piece and coating piece with bacteria were then inactivated in 1.8 mL of sodium thioglycolate saline (STS), then diluted in a dish with peptone water, and seeded onto Mueller-Hinton agar. The plates were examined after 24 hours of incubation, and the total bacterial colony-forming units were calculated.

[0179] Equation 1.

[0180] 1 / (IDxSDxFD)X50XCFU=CFU / mL

[0181] In the formula, ID is the initial dilution, SD is the later dilution, FD is the final dilution, 50 is converted to mL, and CFU is the colony-forming unit counted at the dilution used in the calculation.

[0182] Next, the CFU / mL values ​​were converted to logarithmic numbers. The logarithmic reduction was calculated by subtracting the logarithm of the recovered CFU from the logarithm of the inoculated material. A logarithmic reduction of more than 3 was considered bactericidal.

[0183] To determine the total amount of silver in the bandage, one square inch of bandage was dissolved in 20 mL of a 50% nitric acid solution in distilled water over 20 minutes, then diluted in an additional 20 mL of distilled water, and analyzed using an atomic absorption spectrometer (AAS).

[0184] To estimate the amount of silver oxide in the bandage, and to determine the amount of ammonium hydroxide-available silver, one square inch of the bandage was dissolved in 20 mL of ammonium hydroxide over 10 minutes. 10 mL of this solution was then diluted in 40 mL of water and analyzed using AAS.

[0185] The bandage contained a total of 5320 μg / square inch of Ag, equivalent to 2430 μg / square inch of ammonium hydroxide-soluble Ag, which is 46% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was greater than 6, and the silver coating was found to be bactericidal in calf serum.

[0186] Example 10: Water injection downstream of MFC via microvalve This embodiment is included to demonstrate an antimicrobial coating formed on a commercially available high-density polyethylene (HDPE) mesh by DC magnetron sputtering when water is added via a microvalve after MFC and before entering the deposition chamber. The mesh surface was coated by DC magnetron sputtering with 99.9% pure silver under the following conditions. The working gas used was high-purity commercially available Ar and O2 (final concentration 98 / 2 wt%) added to the vacuum chamber via a separate mass flow controller. HPLC-grade water at 21°C was added to the Ar / O2 at a flow rate of 51.6 μL / min via a burette equipped with a microvalve. The sputtering power was 571 watts (1.5 amps at 380 volts), the argon flow rate was 392 SCCM, the O2 flow rate was 8 SCCM, and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular and measured 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The execution time was 30 minutes, and the HDPE mesh remained stationary.

[0187] The antibacterial effect of the coating was tested using a logarithmic reduction test. A bacterial inoculum was prepared by inoculating 50 mL of calf serum with a 16-hour culture of Pseudomonas aeruginosa, and this was incubated for 16 hours. This resulted in a bacterial count of 1 × 10⁻⁶. 9CFU inoculum was produced. Bandages were prepared from two silver-coated HDPE pieces (2.5 × 2.5 cm) with a piece of cotton gauze (2.5 × 2.5 cm) in between. The bandages were placed on a sterile plastic piece (3.2 × 3.2 cm) with the lid of a petri dish inverted in a Class 2 laminar-flow hood. 200 μL of inoculum was applied to the bandage in the petri dish, then covered with the second plastic piece (3.2 × 3.2 cm), and incubated at 37°C for 1 hour. The bandages containing the plastic base piece and coating piece with bacteria were then inactivated in 1.8 mL of sodium thioglycolate saline (STS), then diluted in a dish with peptone water, and seeded onto Mueller-Hinton agar. The plates were examined after 24 hours of incubation, and the total bacterial colony-forming units were calculated.

[0188] Equation 1.

[0189] 1 / (IDxSDxFD)X50XCFU=CFU / mL

[0190] In the formula, ID is the initial dilution, SD is the later dilution, FD is the final dilution, 50 is converted to mL, and CFU is the colony-forming unit counted at the dilution used in the calculation.

[0191] Next, the CFU / mL values ​​were converted to logarithmic numbers. The logarithmic reduction was calculated by subtracting the logarithm of the recovered CFU from the logarithm of the inoculated material. A logarithmic reduction of more than 3 was considered bactericidal.

[0192] To determine the total amount of silver in the bandage, one square inch of bandage was dissolved in 20 mL of a 50% nitric acid solution in distilled water over 20 minutes, then diluted in an additional 20 mL of distilled water, and analyzed using an atomic absorption spectrometer (AAS).

[0193] To estimate the amount of silver oxide in the bandage, and to determine the amount of ammonium hydroxide-available silver, one square inch of the bandage was dissolved in 20 mL of ammonium hydroxide over 10 minutes. 10 mL of this solution was then diluted in 40 mL of water and analyzed using AAS.

[0194] The bandage contained a total of 4108 μg / m² of silver (Ag), equivalent to 710 μg / m² of ammonium hydroxide-soluble silver (Ag), which is 17.2% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 7.5, and the silver coating was found to be bactericidal in calf serum.

[0195] Example 11: Water injection downstream of MFC via microvalve This embodiment is included to demonstrate an antimicrobial coating formed on a commercially available high-density polyethylene (HDPE) mesh by DC magnetron sputtering when water is added via a microvalve after MFC and before entering the deposition chamber. The mesh surface was coated by DC magnetron sputtering with 99.9% pure silver under the following conditions: The working gas used was high-purity commercially available Ar and O2 (final concentration 98 / 2 wt%) added to the vacuum chamber via a separate mass flow controller. HPLC-grade water at 21°C was added to the Ar / O2 at a flow rate of 9.1 μL / min via a burette equipped with a microvalve. The sputtering power was 571 watts (1.5 amps at 380 volts), the argon flow rate was 392 SCCM, the O2 flow rate was 8 SCCM, and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular and measured 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The execution time was 30 minutes, and the HDPE mesh remained stationary.

[0196] The antibacterial effect of the coating was tested using a logarithmic reduction test. Bacterial inoculum was prepared by inoculating 50 mL of calf serum with a 16-hour culture of Pseudomonas aeruginosa, and this was incubated for 16 hours. This produced 1 × 10⁹ CFU of inoculum. Bandages were prepared from two silver-coated HDPE pieces (2.5 × 2.5 cm) with a piece of cotton gauze (2.5 × 2.5 cm) in between. The bandages were placed on a sterile plastic piece (3.2 × 3.2 cm) with the lid of a petri dish inverted in a Class 2 laminar-flow hood. 200 μL of inoculum was applied to the bandage in the petri dish, and then the second plastic piece (3.2 × 3.2 cm) was placed over it, and the mixture was incubated at 37°C for 1 hour. Next, bandages containing a plastic base piece and a covering piece with bacteria were placed in 1.8 mL of sodium thioglycolate saline (STS) to inactivate the silver, then diluted in peptone water and inoculated onto Mueller-Hinton agar. After 24 hours of incubation, the plates were examined and the total bacterial colony-forming units were calculated.

[0197] Equation 1.

[0198] 1 / (IDxSDxFD)X50XCFU=CFU / mL

[0199] In the formula, ID is the initial dilution, SD is the later dilution, FD is the final dilution, 50 is converted to mL, and CFU is the colony-forming unit counted at the dilution used in the calculation.

[0200] Next, the CFU / mL values ​​were converted to logarithmic numbers. The logarithmic reduction was calculated by subtracting the logarithm of the recovered CFU from the logarithm of the inoculated material. A logarithmic reduction of more than 3 was considered bactericidal.

[0201] To determine the total amount of silver in the bandage, one square inch of bandage was dissolved in 20 mL of a 50% nitric acid solution in distilled water over 20 minutes, then diluted in an additional 20 mL of distilled water, and analyzed using an atomic absorption spectrometer (AAS).

[0202] To estimate the amount of silver oxide in the bandage, and to determine the amount of ammonium hydroxide-available silver, one square inch of the bandage was dissolved in 20 mL of ammonium hydroxide over 10 minutes. 10 mL of this solution was then diluted in 40 mL of water and analyzed using AAS.

[0203] The bandage contained a total of 3196 μg / m² of silver (Ag), equivalent to 830 μg / m² of ammonium hydroxide-soluble silver (Ag), which is 26% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa was 7.5, and the silver coating was found to be bactericidal in calf serum.

[0204] Example 12: Water injection upstream of MFC via syringe pump This embodiment is included to demonstrate an antimicrobial coating formed on a commercially available high-density polyethylene (HDPE) mesh by DC magnetron sputtering when water is injected into Ar upstream of an MFC via a syringe pump before being placed in the deposition chamber. The mesh surface was coated by DC magnetron sputtering with 99.9% pure silver under the following conditions: The working gases used were high-purity commercially available Ar and O2 (final concentration 98 / 2 wt%) added to the vacuum chamber via a separate mass flow controller. Water was injected into the Ar stream at flow rates of 1, 3, 5, 7, and 9 μL / min. A stainless steel pipe was heated to 50°C between the inlet and the MFC to maintain the water in a gaseous state. The sputtering power was 571 watts (1.5 amps at 380 volts), the argon flow rate was 392 SCCM, the O2 flow rate was 8 SCCM, and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular, with measurements of 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The run time was 30 minutes, and the HDPE mesh remained stationary.

[0205] The antibacterial effect of the coating was tested using a logarithmic reduction test. A bacterial inoculum was prepared by inoculating 50 mL of calf serum with a 16-hour culture of Pseudomonas aeruginosa, and this was incubated for 16 hours. This resulted in a bacterial count of 1 × 10⁻⁶. 9CFU inoculum was produced. Bandages were prepared from two silver-coated HDPE pieces (2.5 × 2.5 cm) with a piece of cotton gauze (2.5 × 2.5 cm) in between. The bandages were placed on a sterile plastic piece (3.2 × 3.2 cm) with the lid of a petri dish inverted in a Class 2 laminar-flow hood. 200 μL of inoculum was applied to the bandage in the petri dish, then covered with the second plastic piece (3.2 × 3.2 cm), and incubated at 37°C for 1 hour. The bandages containing the plastic base piece and coating piece with bacteria were then inactivated in 1.8 mL of sodium thioglycolate saline (STS), then diluted in a dish with peptone water, and seeded onto Mueller-Hinton agar. The plates were examined after 24 hours of incubation, and the total bacterial colony-forming units were calculated.

[0206] Equation 1.

[0207] 1 / (IDxSDxFD)X50XCFU=CFU / mL

[0208] In the formula, ID is the initial dilution, SD is the later dilution, FD is the final dilution, 50 is converted to mL, and CFU is the colony-forming unit counted at the dilution used in the calculation.

[0209] Next, the CFU / mL values ​​were converted to logarithmic numbers. The logarithmic reduction was calculated by subtracting the logarithm of the recovered CFU from the logarithm of the inoculated material. A logarithmic reduction of more than 3 was considered bactericidal.

[0210] To determine the total amount of silver in the bandage, one square inch of bandage was dissolved in 20 mL of a 50% nitric acid solution in distilled water over 20 minutes, then diluted in an additional 20 mL of distilled water, and analyzed using an atomic absorption spectrometer (AAS).

[0211] To estimate the amount of silver oxide in the bandage, and to determine the amount of ammonium hydroxide-available silver, one square inch of the bandage was dissolved in 20 mL of ammonium hydroxide over 10 minutes. 10 mL of this solution was then diluted in 40 mL of water and analyzed using AAS.

[0212] Bandages prepared with 9 μL / min of water contained a total of 6672 μg / m² of Ag, including 1050 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 19% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa exceeded 8.3, and the silver coating was found to be bactericidal in calf serum.

[0213] Bandages prepared with 7 μL / min of water contained a total of 4032 μg / m² of Ag, including 1050 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 26% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa exceeded 8.3, and the silver coating was found to be bactericidal in calf serum.

[0214] Bandages prepared with 5 μL / min of water contained a total of 5664 μg / m² of Ag, including 1270 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 22% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa exceeded 8.3, and the silver coating was found to be bactericidal in calf serum.

[0215] Bandages prepared with 3 μL / min of water contained a total of 6856 μg / m² of Ag, including 1620 μg / m² of ammonium hydroxide-soluble Ag, equivalent to 24% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa exceeded 8.3, and the silver coating was found to be bactericidal in calf serum.

[0216] Bandages prepared with 1 μL / min of water contained a total of 4704 μg / square inch of Ag, including 1140 μg / square inch of ammonium hydroxide-soluble Ag, equivalent to 24% ammonium hydroxide-soluble silver. The logarithmic reduction of Pseudomonas aeruginosa exceeded 8.3, and the silver coating was found to be bactericidal in calf serum.

[0217] Example 13: Water injection upstream of MFC via syringe pump data using a 65% Ag / 35% Au alloy. This embodiment is included to demonstrate an antimicrobial coating formed on a commercially available high-density polyethylene (HDPE) mesh by DC magnetron sputtering of a silver / gold alloy when water is injected into Ar upstream of an MFC via a syringe pump before being placed in the deposition chamber. The mesh was coated on the surface by DC magnetron sputtering of 65% Ag / 35% Au using the following conditions: The working gases used were high-purity commercially available Ar and O2 (final concentration of 96 / 4 wt% or 95.5 / 4.5 wt%) added to the vacuum chamber via a separate mass flow controller. Water was injected into the Ar stream at a flow rate of 8 μL / min. A stainless steel pipe was heated to 50°C between the inlet and the MFC to maintain the water in a gaseous state. The sputtering power was 1.8 amps, the argon flow rate was 384 SCCM, the O2 flow rate was 16 SCCM or 382 SCCM, the O2 flow rate was 18 SCCM, and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular, with measurements of 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The execution time was 30 minutes, and the HDPE mesh moved at a rate of 1.5 cm / min.

[0218] The antibacterial effect of the coating was tested using a logarithmic reduction test. A bacterial inoculum was prepared by inoculating 50 mL of calf serum with a 16-hour culture of Pseudomonas aeruginosa, and this was incubated for 16 hours. This resulted in a bacterial count of 1.05 × 10⁻⁶. 9CFU inoculum was produced. Bandages were prepared from two HDPE silver / gold alloy coated pieces (2.5 × 2.5 cm) with a piece of cotton gauze (2.5 × 2.5 cm) in between. The bandages were placed on a sterile plastic piece (3.2 × 3.2 cm) with the lid of a petri dish inverted in a Class 2 laminar flow hood. 200 μL of inoculum was applied to the bandage in the petri dish, then covered with the second plastic piece (3.2 × 3.2 cm), and incubated at 37°C for 1 hour. The bandages containing the plastic base piece and coating piece with bacteria were then inactivated in 1.8 mL of sodium thioglycolate saline (STS), then diluted in a dish with peptone water and seeded on Mueller-Hinton agar. The plates were examined after 24 hours of incubation, and the total bacterial colony-forming units were calculated.

[0219] Equation 1.

[0220] 1 / (IDxSDxFD)X50XCFU=CFUmL

[0221] In the formula, ID is the initial dilution, SD is the later dilution, FD is the final dilution, 50 is converted to mL, and CFU is the colony-forming unit counted at the dilution used in the calculation.

[0222] Next, the CFU / mL values ​​were converted to logarithmic numbers. The logarithmic reduction was calculated by subtracting the logarithm of the recovered CFU from the logarithm of the inoculated material. A logarithmic reduction of more than 3 was considered bactericidal.

[0223] To determine the total amount of silver in the bandage, one square inch of bandage was dissolved in 20 mL of a 50% nitric acid solution in distilled water over 20 minutes, then diluted in an additional 20 mL of distilled water, and analyzed using an atomic absorption spectrometer (AAS).

[0224] To estimate the amount of silver oxide in the bandage, and to determine the amount of ammonium hydroxide-available silver, one square inch of the bandage was dissolved in 20 mL of ammonium hydroxide over 10 minutes. 10 mL of this solution was then diluted in 40 mL of water and analyzed using AAS.

[0225] To determine the total amount of gold in the bandage, 1 square inch of the bandage was dissolved in 20 mL of aqua regia of nitric acid in distilled water for 20 minutes, then diluted with an additional 20 mL of distilled water and analyzed using an atomic absorption spectrometer (AAS).

[0226] The bandage made with 4% O2 and 8 μL / min of water contained a total of 2956 μg / square inch of Ag and 1150 μg / square inch of ammonium hydroxide-available Ag, corresponding to 38.9% ammonium hydroxide-available silver. The amount of gold in the bandage was 1520 μg / square inch, or 34% of the coating. The logarithmic reduction of Pseudomonas aeruginosa was 5.4, and it was found that the silver / gold coating deposited in a moist environment was bactericidal in calf serum.

[0227] The bandage made with 4.5% O2 and 8 μL / min of water contained a total of 2896 μg / square inch of Ag and 1740 μg / square inch of ammonium hydroxide-available Ag, corresponding to 60% ammonium hydroxide-available silver. The amount of gold in the bandage was 1488 μg / square inch, or 34% of the coating. The logarithmic reduction of Pseudomonas aeruginosa was 5.4, and it was found that the silver / gold coating deposited in a moist environment was bactericidal in calf serum.

[0228] Example 14. Water injection upstream of MFC via syringe pump data using a 35% Ag / 65% Au alloy This embodiment is included to demonstrate an antimicrobial coating formed on a commercially available high-density polyethylene (HDPE) mesh by DC magnetron sputtering of a silver / gold alloy when water is injected into Ar upstream of an MFC via a syringe pump before being placed in a deposition chamber. The mesh was coated on the surface by DC magnetron sputtering of 35% Ag / 65% Au using the following conditions: The working gases used were high-purity commercially available Ar and O2 (final concentrations of 99 / 1, 97.5 / 2.5, and 95.75 wt%) added to the vacuum chamber via a separate mass flow controller. Water was injected into the Ar stream at a flow rate of 2, 4, or 8 μL / min. A stainless steel pipe was heated to 50°C between the inlet and the MFC to maintain the water in a gaseous state. The sputtering power was 684 watts (1.8 amps at 380 volts), the argon flow rates were 396, 390, and 383 SCCM, the O2 flow rates were 4, 10, and 17 SCCM, and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular, with measurements of 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The execution time was 30 minutes of dynamic execution (web speed 1.56 cm / min).

[0229] The antibacterial effect of the coating was tested using a logarithmic reduction test. A bacterial inoculum was prepared by inoculating 50 mL of calf serum with a 16-hour culture of Pseudomonas aeruginosa, and this was incubated for 16 hours. This resulted in a bacterial count of 3.5 × 10⁻⁶. 9CFU inoculum was produced. Bandages were prepared from two HDPE silver / gold alloy coated pieces (2.5 × 2.5 cm) with a piece of cotton gauze (2.5 × 2.5 cm) in between. The bandages were placed on a sterile plastic piece (3.2 × 3.2 cm) with the lid of a petri dish inverted in a Class 2 laminar flow hood. 250 μL of inoculum was applied to the bandage in the petri dish, then covered with the second plastic piece (3.2 × 3.2 cm), and incubated at 37°C for 1 hour. The bandages containing the plastic base piece and coating piece with bacteria were then inactivated in 2.25 mL of sodium thioglycolate saline (STS), then diluted in a dish with peptone water and seeded on Mueller-Hinton agar. The plates were examined after 24 hours of incubation, and the total bacterial colony-forming units were calculated.

[0230] Equation 1.

[0231] 1 / (IDxSDxFD)X50XCFU=CFUmL

[0232] In the formula, ID is the initial dilution, SD is the later dilution, FD is the final dilution, 50 is converted to mL, and CFU is the colony-forming unit counted at the dilution used in the calculation.

[0233] Next, the CFU / mL values ​​were converted to logarithmic numbers. The logarithmic reduction was calculated by subtracting the logarithm of the recovered CFU from the logarithm of the inoculated material. A logarithmic reduction of more than 3 was considered bactericidal.

[0234] The data is summarized in Figures 6A and 6B.

[0235] The logarithmic reduction of bandages prepared with 1% O2 and 0 μL / min of water was 0.9 against Pseudomonas aeruginosa, indicating that silver / gold coating deposited in a moist environment was not bactericidal against calf serum.

[0236] The logarithmic reduction of bandages prepared with 2.5% O2 and 0 μL / min of water was 1.0 against Pseudomonas aeruginosa, indicating that silver / gold coating deposited in a moist environment was not bactericidal against calf serum.

[0237] The logarithmic reduction of bandages prepared with 4.25% O2 and 0 μL / min of water was 4.2 against Pseudomonas aeruginosa, indicating that the silver / gold coating deposited in a moist environment was bactericidal against calf serum.

[0238] The logarithmic reduction of bandages prepared with 0% O2 and 2 μL / min of water was 1.0 against Pseudomonas aeruginosa, indicating that silver / gold coating deposited in a moist environment was not bactericidal against calf serum.

[0239] The logarithmic reduction of bandages prepared with 0% O2 and 4 μL / min of water was 0.9 against Pseudomonas aeruginosa, indicating that silver / gold coating deposited in a moist environment was not bactericidal against calf serum.

[0240] The logarithmic reduction of bandages prepared with 0% O2 and 8 μL / min of water was 0.9 against Pseudomonas aeruginosa, indicating that silver / gold coating deposited in a moist environment was not bactericidal against calf serum.

[0241] The logarithmic reduction of bandages prepared with 1% O2 and 8 μL / min of water was 1.2 against Pseudomonas aeruginosa, indicating that silver / gold coating deposited in a moist environment was not bactericidal against calf serum.

[0242] The logarithmic reduction of bandages prepared with 2.5% O2 and 8 μL / min of water was 4.4 against Pseudomonas aeruginosa, indicating that the silver / gold coating deposited in a moist environment was bactericidal against calf serum.

[0243] The logarithmic reduction of bandages prepared with 4.25% O2 and 8 μL / min of water was 5.5 against Pseudomonas aeruginosa, indicating that the silver / gold coating deposited in a moist environment was bactericidal against calf serum.

[0244] While water alone has very limited effects, higher concentrations (4.25%) of oxygen exhibit some antibacterial activity. When water (8 μL / min) is added to the Ar / O2 working gas, a synergistic effect is observed, and the antibacterial activity of the resulting material is more than 10 times greater than that of the Ar / O2 working gas itself.

[0245] Example 15: Demonstration of various sputtering powers This embodiment is included to demonstrate an antimicrobial coating formed on a commercially available high-density polyethylene (HDPE) mesh by DC magnetron sputtering when water is injected into Ar upstream of an MFC via a syringe pump before being placed in the deposition chamber. The mesh was coated on the surface by DC magnetron sputtering with 99.9% pure silver under the following conditions: The working gases used were high-purity commercially available Ar and O2 (final concentration of 95.75 / 4.25 wt%) added to the vacuum chamber via a separate mass flow controller. Water was injected into the Ar stream at a flow rate of 6 μL / min. A stainless steel pipe was heated to 50°C between the inlet and the MFC to maintain the water in a gaseous state. Sputtering power was 684, 342, and 190 watts (1.8, 0.9, or 0.5 amperes at 380 volts), argon flow rate was 383 SCCM, O2 flow rate was 17 SCCM, and working gas pressure was 50, 40, or 13 mTorr in each run. The distance from the target to the substrate was 10 cm. The target was rectangular, and its measured dimensions were 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The execution time was 30 minutes, and the HDPE mesh remained stationary.

[0246] The antibacterial effect of the coating was tested using a logarithmic reduction test. A bacterial inoculum was prepared by inoculating 50 mL of calf serum with a 16-hour culture of Pseudomonas aeruginosa, and this was incubated for 16 hours. This resulted in a bacterial count of 1 × 10⁻⁶. 9An inoculum of CFU was produced. A bandage was prepared from two silver-coated pieces of HDPE (2.5×2.5 cm) with a piece of cotton gauze (2.5×2.5 cm) in between. In a Class 2 laminar flow hood, with the lid of the Petri dish facing upwards, the bandage was placed on a sterile plastic piece (3.2×3.2 cm). 200 μL of the inoculum was applied to the bandage in the Petri dish, then covered with a second plastic piece (3.2×3.2 cm) and incubated at 37 °C for 1 hour. Then, the bandage containing the plastic substrate piece and the coated piece with bacteria was placed in 1.8 mL of sodium thioglycollate saline solution (STS) to inactivate silver, then diluted in the dish using peptone water and seeded onto Mueller-Hinton agar medium. The plates were examined after 24 hours of incubation and the total bacterial colony forming units were calculated.

[0247] Equation 1.

[0248] 1 / (IDxSDxFD)X50XCFU=CFUmL

[0249] Where ID is the initial dilution, SD is the subsequent dilution, FD is the final dilution, 50 is converted to mL, and CFU is the colony forming unit counted at the dilution used for the calculation.

[0250] The CFU / mL was then converted to a logarithmic number. The log reduction was calculated by subtracting the log of the recovered CFU from the log of the inoculum. A log reduction greater than 3 is considered bactericidal.

[0251] The data for logarithmic reduction are summarized in Table 1. The most active bandages were those deposited at 40 mTorr, followed by 50 mTorr and 13 mTorr. The working gas pressure in the system achieved antimicrobial activity against the sputtered thin films, but in the range of 13–50 mTorr, all films were at least bactericidal (higher than 3-logarithmic reduction). In these examples, the power was reduced as the gas pressure decreased in order to maintain an ammonium hydroxide soluble silver content of over 35%. As the pressure decreases, the mean free distance between gas atoms increases, and if the sputtered flux is high, the deposited film will be mainly metallic. That is, a metallic film is deposited because there are no multiple collisions between the working gas and the sputtered flux, and the oxidation reaction time in the gas phase is shortened.

[0252] [Table 1]

[0253] Example 16: Demonstration of various target-substrate distances This embodiment is included to demonstrate the effect of cathode-substrate distance on antimicrobial coatings formed on commercially available high-density polyethylene (HDPE) mesh by DC magnetron sputtering when water is injected into Ar upstream of the MFC via a syringe pump before being placed in the deposition chamber. The mesh was coated on the surface by DC magnetron sputtering with 99.9% pure silver under the following conditions. The working gases used were high-purity commercially available Ar and O2 (final concentration of 95.75 / 4.25 wt%) added to the vacuum chamber via a separate mass flow controller. Water was injected into the Ar stream at a flow rate of 9 μL / min. A stainless steel pipe was heated to 50°C between the inlet and the MFC to maintain the water in a gaseous state. The sputtering power was 1.8 amps, the argon flow rate was 383 SCCM, the O2 flow rate was 17 SCCM, and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular, with measurements of 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The run time was 30 minutes, and the HDPE mesh remained stationary.

[0254] The antibacterial effect of the coating was tested using a logarithmic reduction test. A bacterial inoculum was prepared by inoculating 50 mL of calf serum with a 16-hour culture of Pseudomonas aeruginosa, and this was incubated for 16 hours. This resulted in a bacterial count of 1 × 10⁻⁶. 9CFU inoculum was produced. Bandages were prepared from two silver-coated HDPE pieces (2.5 × 2.5 cm) with a piece of cotton gauze (2.5 × 2.5 cm) in between. The bandages were placed on a sterile plastic piece (3.2 × 3.2 cm) with the lid of a petri dish inverted in a Class 2 laminar-flow hood. 200 μL of inoculum was applied to the bandage in the petri dish, then covered with the second plastic piece (3.2 × 3.2 cm), and incubated at 37°C for 1 hour. The bandages containing the plastic base piece and coating piece with bacteria were then inactivated in 1.8 mL of sodium thioglycolate saline (STS), then diluted in a dish with peptone water, and seeded onto Mueller-Hinton agar. The plates were examined after 24 hours of incubation, and the total bacterial colony-forming units were calculated.

[0255] Equation 1.

[0256] 1 / (IDxSDxFD)X50XCFU=CFU / mL

[0257] In the formula, ID is the initial dilution, SD is the later dilution, FD is the final dilution, 50 is converted to mL, and CFU is the colony-forming unit counted at the dilution used in the calculation.

[0258] Next, the CFU / mL values ​​were converted to logarithmic numbers. The logarithmic reduction was calculated by subtracting the logarithm of the recovered CFU from the logarithm of the inoculated material. A logarithmic reduction of more than 3 was considered bactericidal.

[0259] The data is summarized in Table 2. As the distance between the target and the substrate decreases, the average number of collisions between the sputtered atoms and argon decreases, and the flow velocity becomes more active. The absence of multiple collisions between the working gas and the sputtered flux, along with the shortened oxidation reaction time in the gas phase, allows for the deposition of a metal film. Combining these two challenges yields a web that is exposed to temperatures higher than the metalling point at which defects occur.

[0260] [Table 2]

[0261] Example 17: Anti-inflammatory effect This embodiment was included to demonstrate an anti-inflammatory coating formed on a commercially available high-density polyethylene (HDPE) mesh by DC magnetron sputtering when water is injected into Ar upstream of the MFC via a syringe pump before being placed in the deposition chamber. The mesh surface was coated by DC magnetron sputtering with 99.99% pure silver, 65% Ag / 35% Au, or 20% Ag / 80% Au under the following conditions. The working gases used were high-purity commercially available Ar and O2 (final concentration of 95.75 / 4.25 wt%) added to the vacuum chamber via a separate mass flow controller. Water was injected into the Ar stream at a flow rate of 9 μL / min. A stainless steel pipe was heated to 50°C between the inlet and the MFC to maintain the water in a gaseous state. The sputtering power was 1.8 amps, the argon flow rate was 383 SCCM, the O2 flow rate was 17 SCCM, and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular, with measurements of 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The run time was 6 hours, during which the HDPE mesh moved at 0.69 in / min.

[0262] The anti-inflammatory effect of the coating was tested in large white pigs using a DNCB (dinitrochlorobenzene)-induced inflammatory response. Bandages were prepared from two silver-coated HDPE pieces (8 × 12 in) with a piece of polyester gauze (8 × 12 in) in between.

[0263] Large white Yorkshire / Landrace animals (female, initial weight 10-15 kg) were selected for this study because they most closely resemble human skin and exhibit similar anti-inflammatory responses. Three animals were assigned to each test or control group, resulting in a total of nine different groups. The experiment was conducted in three variations. Briefly, animals were introduced to the experiment on day -17 to allow them to acclimate to the test facility. On day -13, the left side of the pigs' fur was shaved. Each treated pig was then treated with approximately 3 mL of 10% v / v 1,2-dinitrochlorobenzene (DNCB) in a 4:1 acetone-olive oil mixture on a shaved area of ​​approximately 25 cm x 15 cm. This shaved area was located caudally above the scapula running over the rib cage, 5 cm from the dorsal midline (representing approximately 5% of the total body surface area). This procedure was repeated on days -7 and -3. -On day 1, fentanyl patches were applied to all pigs to reduce discomfort without affecting skin inflammation. Animals in group "0", the control group, were administered a placebo of saline solution. To prevent injury to staff handling the animals and cross-contamination of the animals, the DNCB procedure was performed under complete anesthesia, and the treatment site was covered with Opsite® and secured with Elastoplast. After the final application of DNCB, the animals were placed under general anesthesia. On day 0, visual observation was performed using digital imaging. On days 1, 2, and 3, erythema and edema in the pigs were evaluated. The procedure was reapplied. All bandages were further secured with Opsite® to maintain moisture control and then secured with Elastoplast. Each animal was treated with a fentanyl patch for pain management. Evaluation and bandage changes were performed on days 1 and 2. On day 3, the pigs were slaughtered after evaluation and a complete autopsy was performed. Clinical observation was performed from day 0 to day 3, and photographs of the rash were taken. Erythema and edema were graded on a scale from 0 to 4. Control animals included saline without DNCB, saline with DNCB or Acticoat, and DNCB treatment.

[0264] The results are summarized in Figures 7A and 7B. All materials produced using the new water-based sputtering process reduced erythema much more rapidly than Acticoat bandages, as shown in Figure 7A. Similar results were observed for edema, as shown in Figure 7B.

[0265] Example 18: Treatment of herpesvirus This embodiment demonstrates the formation of an antimicrobial coating on a commercially available high-density polyethylene (HDPE) mesh by DC magnetron sputtering when water is injected into Ar upstream of the MFC via a syringe pump before being placed in the deposition chamber. The mesh surface was coated by DC magnetron sputtering with 99.9% pure silver under the following conditions: The working gases used were high-purity commercially available Ar and O2 (final concentration 95.75 / 4.25 wt%) added to the vacuum chamber via a separate mass flow controller. Water was injected into the Ar stream at a flow rate of 9 μL / min. A stainless steel pipe was heated to 50°C between the inlet and the MFC to maintain the water in a gaseous state. The sputtering power was 1.8 amps, the argon flow rate was 383 SCCM, the O2 flow rate was 17 SCCM, and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular and measured 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The execution time was 6 hours, and the HDPE mesh was moving at 0.69 in / min.

[0266] A solution was prepared by placing a 4-square-inch coated HDPE mesh in 15 mL of water and incubating it at 37°C for 6 hours. This solution was used to treat a resolving herpes simplex type 1 infection of the lips and nose. Blisters formed inside the nostrils, and the patient's lower lip showed burning and stinging, with new oral herpes lesions observed. The treatment was applied to the patient's lips and inside the nostrils with a cotton swab before bedtime. The treatment was repeated after 6 hours. After 12 hours, there was no burning or stinging on the lips, and the pain associated with contact inside the nose was dramatically reduced. The treatment was used more than twice, and after 24 hours, there was no pain on the lips or nose. This treatment controlled the herpes simplex type 1 outbreak in this patient, demonstrating the antiviral activity of the solution obtained from nanosilver particles.

[0267] Example 19: Treatment of human papillomavirus This embodiment is included to demonstrate an antimicrobial coating formed on a commercially available high-density polyethylene (HDPE) mesh by DC magnetron sputtering when water is injected into Ar upstream of an MFC via a syringe pump before being placed in the deposition chamber. The mesh surface was coated by DC magnetron sputtering with 99.9% pure silver under the following conditions: The working gases used were high-purity commercially available Ar and O2 (final concentration of 95.75 / 4.25 wt%) added to the vacuum chamber via a separate mass flow controller. Water was injected into the Ar stream at a flow rate of 9 μL / min. A stainless steel pipe was heated to 50°C between the inlet and the MFC to maintain the water in a gaseous state. The sputtering power was 1.8 amps, the argon flow rate was 383 SCCM, the O2 flow rate was 17 SCCM, and the working gas pressure was 40 mTorr. The distance from the target to the substrate was 10 cm. The target was rectangular and measured 12.7 cm × 51.4 cm. The target was cooled and maintained at 15°C using a chiller. The execution time was 6 hours, and the HDPE mesh was moving at 0.69 in / min.

[0268] The patient had recurrent plantar warts on the ball of the right foot. The affected area was treated with a bandage made of silver-clad HDPE and cotton gauze. The cotton gauze was moistened with sterile water and placed on top of the silver-clad HDPE over the infected area. This was then covered with a transparent film bandage to maintain moisture at the site of infection. The bandage was changed every three days for two weeks, after which the skin thickened by the plantar warts peeled off, leaving new healthy tissue. The warts did not return after six months, demonstrating that this bandage effectively controlled the human papillomavirus that caused the infection. The results are summarized in Figures 7A-7B. All materials produced using the new water-based sputtering process reduced erythema much more rapidly than Acticoat bandages. Similar results were observed for edema.

[0269] Example 20: Composition of working gas The purpose of this embodiment is to present various compositions of the working gas in the embodiments described herein. Table 3 shows the working gas compositions when the working gas flow rate is 400 SCCM.

[0270] [Table 3]

[0271] The water concentration used in the examples described herein ranged from approximately 2.8% to 11.2%, the oxygen concentration ranged from 1% to 4.5%, and the working gas flow rate was 400 SCCM. As oxygen increased, the ammonia-soluble content increased synergistically. Above 3% water, higher temperatures were required to maintain the water in gaseous form. However, the mass flow controllers used in these experiments could not withstand temperatures above 50°C. Instead of applying the high temperatures required to produce steam, steam was injected directly into the deposition chamber.

[0272] Example 21: Calculation of sputtering power density The objective of this embodiment is to demonstrate the calculation of sputtering power density at various values. The power of the sputtering system used in the embodiments described herein is controlled by varying the current. In the embodiments described, the current varied from 0.1 to 2.5 amperes (A). The system voltage was approximately 380 volts (V). The active area of ​​the sputtering target, or etch track ring area, was measured to be 284.39 cm². 2 The power in watts (W) was calculated by multiplying the voltage (V) by the current (A). The power density (W / cm²) was calculated by dividing the power (W) by the active area of ​​the target. 2 The following was calculated: Various power densities were calculated as shown in Table 4.

[0273] [Table 4]

[0274] Example 22: In this example, we demonstrate that the silver-based metal matrix composite material produced by the method described herein contains silver carbonate (Ag2CO3) when exposed to CO2. This is confirmed by X-ray diffraction comparison with other nanocrystalline materials. As an example, Acticoat, a commercially available nanocrystalline material, was characterized by X-ray diffraction as shown in Figure 8A. This material did not show a spectral peak indicating silver carbonate. However, the silver-based metal matrix composite material produced by the method described herein showed an X-ray diffraction spectral peak, confirming the presence of silver carbonate as seen in Figures 8B and 8C. Figure 8A shows the X-ray diffraction spectrum of a sample exposed to an atmosphere with 400 ppm CO2 for a period of less than 10 minutes after deposition and before X-ray diffraction. Water was injected into this sample upstream of a mass flow controller at 50°C, with the power set to 380V and 1.8A, and the water flow rate to 20 μL / min. The target active area, or etching track area, was measured to be 284.39 cm². 2The sample was determined to be 70% ammonia soluble. A prominent X-ray diffraction spectral peak indicating silver carbonate was observed at 32.8°C, as shown in Figure 8B. In the process described herein, a second sample was synthesized using a microvalve to inject 33 μL / min of water upstream of the mass flow controller, with oxygen gas present at 2% of the total working gas composition, and the sputtering power set to 380 V and 1.5 A. The target active area, or etching track area, was measured to be 284.39 cm². 2 Figure 8C shows two peaks, one at 32.2 confirming silver oxide and the other at 32.8 confirming silver carbonate. After exposure to a CO2 environment, the presence of silver carbonate in the material prepared by the method described herein suggests structural differences compared to commercially available silver nanocrystalline materials.

Claims

1. A method for preparing a metal matrix composite material, the method comprising the step of depositing one or more metals and metal oxides from a source onto a substrate in a deposition chamber in the presence of water vapor and one or more gases including oxygen gas, wherein the source is located at a distance of at least 5 cm from the substrate, and the method further comprises setting the internal pressure of the deposition chamber to 10 before and / or during the deposition. －７ A method comprising a step of reducing the temperature below the threshold, wherein the metal matrix composite material comprises metal grain boundary atoms, metal oxides, and metal crystal grains, the median diameter of the crystal grains is between 2 nm and 15 nm, and the grain boundary atoms constitute 50 to 20% of the unit surface area of ​​the metal matrix composite material.

2. The method according to claim 1, wherein the metal is a precious metal.

3. The method according to claim 2, wherein the precious metal is silver, gold, platinum, palladium, or a combination thereof.

4. The method according to claim 1, further comprising the step of depositing at least two metals on the substrate.

5. The method according to claim 4, wherein the at least two metals include silver and gold.

6. The method according to claim 4, wherein the at least two metals include silver and gold, with silver present in a 65% proportion and gold in a 35% proportion.

7. The method according to claim 4, wherein the at least two metals include silver and gold, with silver present in a 35% proportion and gold in a 65% proportion.

8. The method according to claim 1, further comprising the step of depositing an additional metal or metal oxide on the substrate.

9. The method according to claim 1, wherein the substrate is solid.

10. The method according to claim 9, wherein the solid comprises a metal foil, glass, or silicon.

11. The method according to claim 1, wherein the substrate includes a mesh structure made from high-density polyethylene.

12. The method according to claim 11, further comprising depositing one or more of the metal and metal oxides on the substrate, and then manufacturing a bandage including the mesh structure.

13. The method according to claim 12, wherein the bandage includes an absorbent layer between two mesh structures made of high-density polyethylene.

14. The method according to claim 1, wherein the oxygen gas is present in an amount between 1 and 4.5%.

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