Oxygen-deficient wrinkle M x Mg 1-x Oxide antibacterial material, preparation and use thereof

Abstract

The application belongs to the field of antibacterial materials, and particularly relates to an oxygen-defect wrinkle M x Mg 1‑x Oxide antibacterial material, preparation and application thereof, the preparation method is as follows: obtaining a metal solution dispersed with Mg source and M source, then carrying out atomization treatment to obtain metal raw material particles, then carrying out first-stage calcination on the metal raw material particles in an oxygen-free atmosphere at a temperature of 500-1000 DEG C, then in an oxygen-containing atmosphere, the oxygen-defect wrinkle M x Mg 1‑x Oxide antibacterial material; the M x Mg 1‑x In the oxide, the M includes at least one of Li or rare earth elements; x is 0.01-0.4. The material prepared by the preparation method can unexpectedly and significantly improve antibacterial performance.

Description

Technical Field

[0001] This invention relates to the preparation of antibacterial materials, and more particularly to a magnesium oxide-modified antibacterial material. Background Technology

[0002] Harmful microorganisms, especially common bacteria such as Escherichia coli and Helicobacter pylori, have significantly impacted human life and health. Therefore, addressing the adverse effects of harmful microorganisms on human life has become a hot topic and an urgent problem to be solved. Against this backdrop, antimicrobial materials have come into the public eye and quickly become a focus of attention. Developing new, safe, environmentally friendly, and effective antimicrobial materials, and how to achieve large-scale industrial production and utilization of these new antimicrobial materials, have become key areas of focus.

[0003] MgO, as an emerging inorganic antibacterial material, has gained attention and gradually become a hot topic in antibacterial material research due to its environmental friendliness, low cost, and non-toxicity. However, compared with traditional inorganic antibacterial materials, such as Ag-based materials and photocatalytic antibacterial materials like TiO2 and ZnO, magnesium oxide has two drawbacks: firstly, pure magnesium oxide has relatively weak antibacterial properties, and its application requires consideration of whether the addition of large doses of antibacterial materials will affect the product; secondly, although reinforced magnesium oxide materials exist, their production costs are high and the process is complex, affecting the economic benefits of the product. Therefore, it is necessary to develop a magnesium oxide material that possesses both high antibacterial properties and an industrially feasible production method.

[0004] To address the issue of unsatisfactory antibacterial activity of magnesium oxide, existing technologies have several improvement solutions. For example, Chinese patent document CN116463103A discloses an antibacterial and antifungal sealant and its preparation method, specifically disclosing a Zn, Ce, and Cu co-doped MgO. It also discloses a preparation method involving calcining raw materials of zinc, cerium, copper, magnesium, and PEG400 at 450–550°C. Additionally, US patent document US20220279794A1 discloses a co-doped magnesium oxide nanocomposite material composition. Chinese patent document CN112088897A discloses a nano-magnesium oxide inorganic antibacterial agent and its preparation method, specifically describing a preparation process involving the calcination of lithium salt, magnesium salt, and a complexing agent.

[0005] In summary, the existing main approach to addressing the unsatisfactory antibacterial properties of magnesium oxide is to dope it with elements. However, this method is unlikely to further improve its antibacterial properties and efficiency, especially against difficult-to-treat Gram-negative bacteria, where its antibacterial ability and efficiency need to be improved. Summary of the Invention

[0006] To address the unsatisfactory antibacterial efficiency and effectiveness of existing magnesium oxide-based antibacterial materials, particularly their difficulty in exhibiting high-efficiency antibacterial activity against Gram-negative bacteria, the primary objective of this invention is to provide an oxygen-deficient wrinkled M... x Mg 1-x The preparation method of oxide antibacterial materials aims to prepare M with suitable oxygen-deficient wrinkle morphology and excellent antibacterial efficiency and effect. x Mg 1-x Oxide antibacterial materials.

[0007] The second objective of this invention is to provide an oxygen-deficient fold M prepared by the aforementioned method. x Mg 1-x Oxide antibacterial materials and their applications.

[0008] A third objective of the present invention is to provide a system comprising the oxygen-deficient fold M. x Mg 1-x Preparation of antibacterial oxide antibacterial materials.

[0009] Existing magnesium oxide-based antibacterial materials exhibit unsatisfactory antibacterial activity and efficiency, particularly against Gram-negative bacteria that are difficult to inhibit. While existing doping methods can improve antibacterial activity to some extent, the modified materials still fall short of optimal antibacterial efficiency and effectiveness against Gram-negative bacteria. To address this issue, this invention, after in-depth research, provides the following improvement scheme:

[0010] An oxygen-deficient fold M x Mg 1-x A method for preparing oxide antibacterial materials involves obtaining a metal solution (also known as a metal salt solution) dispersed with Mg and M sources, followed by atomization to obtain metal raw material particles (also known as precursor particles). These metal raw material particles are then subjected to a first-stage calcination at 500–1000°C in an oxygen-free atmosphere to obtain the oxygen-deficient wrinkled M source. x Mg 1-x Oxide antibacterial materials;

[0011] The M mentioned x Mg 1-x In the oxide, M includes at least one of Li or rare earth elements; x is 0.01 to 0.4.

[0012] Unlike conventional doping processes that require organic assistance, this invention directly atomizes a metal solution without adding a conventional carbon source, followed by calcination in an oxygen-free atmosphere. This unexpectedly creates a gradient of oxygen defects on the surface and enables particle shrinkage to form a suitable wrinkled surface. Research in this invention shows that the material prepared using this method unexpectedly exhibits significantly improved antibacterial properties, particularly against recalcitrant Gram-negative bacteria, demonstrating excellent short-term and highly effective antibacterial activity.

[0013] In this invention, the Mg source and the M source are water-soluble salts of various metal elements, such as at least one of inorganic acid salts and acetates.

[0014] Preferably, the rare earth element comprises at least one of Ce and La. Most preferably, M is Li. Research in this invention indicates that the preferred M, when combined with the process of this invention, helps to further achieve synergy and can further optimize the antibacterial activity of the material against Gram-negative bacteria in a short time.

[0015] Preferably, x is 0.05 to 0.2, and more preferably 0.1 to 0.15. Research in this invention indicates that, at the preferred x value, its combination with the process of this invention helps to achieve further synergy, and can further optimize the antibacterial activity of the material against Gram-negative bacteria in a short time.

[0016] In this invention, the inlet air temperature for the atomization process is 180–240°C, and the outlet air temperature is 100–160°C. Further, the inlet air temperature for the atomization process is 200–240°C, and the outlet air temperature is 100–120°C.

[0017] Preferably, the particle size of the metal raw material particles is 1–5 μm.

[0018] In this invention, the oxygen-free atmosphere is at least one of nitrogen and an inert gas. For example, the inert gas is Ar.

[0019] In this invention, the temperature of the first calcination stage can be 550–800°C, and more preferably 600–700°C.

[0020] In this invention, the holding time at the first calcination temperature is 2 to 6 hours; preferably 4 to 6 hours.

[0021] Preferably, in this invention, after the first stage of calcination, a second stage of calcination is carried out in an oxygen-containing atmosphere at a temperature above 300°C, preferably above 350°C, to obtain the oxygen-deficient folds M. x Mg 1-xOxide antibacterial materials. This invention demonstrates that subjecting the product after the first calcination stage to subsequent calcination in an oxygen-containing atmosphere unexpectedly further optimizes the material's deep antibacterial activity against Gram-negative bacteria.

[0022] In this invention, the temperature of the second calcination stage is 350–450°C.

[0023] In this invention, the holding time at the second calcination temperature is 1 to 4 hours, preferably 1 to 2 hours.

[0024] The present invention also provides an oxygen-deficient fold M prepared by the aforementioned method. x Mg 1-x Oxide antibacterial materials.

[0025] The preparation method described in this invention can endow the prepared material with special physicochemical properties, and the material with the aforementioned properties obtained by the preparation method can unexpectedly and significantly enhance antibacterial properties, especially against Gram-negative bacteria that are difficult to inhibit, it can also obtain excellent antibacterial activity in a short time.

[0026] The oxygen-deficient folds M of the present invention x Mg 1-x The oxide antibacterial materials are blackish-gray or grayish-white in color, with particle sizes ranging from 10 nm to 1 μm.

[0027] The present invention also provides an oxygen-deficient fold M prepared by the above preparation method. x Mg 1-x The application of oxide antibacterial materials involves using them as antibacterial active ingredients to prepare antibacterial products that inhibit microorganisms.

[0028] Preferably, the microorganism is a bacterium, more preferably a Gram-positive bacterium and / or a Gram-negative bacterium; more preferably a Gram-negative bacterium.

[0029] The present invention also provides an antibacterial product, which contains oxygen-deficient wrinkle M prepared by the preparation method described in the present invention. x Mg 1-x Oxide antibacterial materials, and / or through the oxygen-deficient folds M x Mg 1-x Oxide antibacterial materials were prepared.

[0030] In the aforementioned antibacterial product, the oxygen-deficient folds M x Mg 1-x The content of oxide antibacterial materials can be adjusted reasonably as needed.

[0031] Beneficial effects

[0032] This invention directly atomizes a metal solution without the addition of a conventional carbon source, and then calcines it in an oxygen-free atmosphere. This unexpectedly creates a gradient oxygen defect on the surface and enables particle shrinkage to form a suitable wrinkled surface.

[0033] This invention demonstrates that the material prepared using the described method exhibits unexpectedly and significantly improved antibacterial properties, particularly demonstrating excellent antibacterial activity against Gram-negative bacteria within a short period. In particular, the combination of M-type, x-type, and calcination mechanisms contributes to further and unexpectedly optimizing the antibacterial activity of the prepared material against Gram-negative bacteria. Attached Figure Description

[0034] Figure 1 The images show the overall SEM image of the powder precursor material and a magnified image of a local part of the material during the preparation process in Comparative Example 1.

[0035] Figure 2 The images show the overall SEM images of the metal-doped magnesium oxide materials and the undoped magnesium oxide materials prepared in Comparative Examples 1, 1, and 2.

[0036] Figure 3 These are SEM magnified images and partial magnified images of the metal-doped magnesium oxide materials and undoped magnesium oxide materials prepared in Comparative Examples 1, 1, and 2.

[0037] Figure 4 Comparative Examples 1, 2, and 3: Metal-doped magnesium oxide materials and undoped magnesium oxide materials x X-ray diffraction pattern and magnified single peak image.

[0038] Figure 5 Comparative Examples 1, 2, and 3: Metal-doped magnesium oxide materials and undoped magnesium oxide materials XPS Peak distribution diagrams of O element in each material during the analysis.

[0039] Figure 6 This is an experimental diagram showing the minimum antibacterial concentration of the metal-doped magnesium oxide material and the undoped magnesium oxide material prepared in Comparative Example 1, Example 1, and Example 2. Detailed Implementation

[0040] The specific embodiments of the present invention will now be clearly and completely described with reference to the accompanying drawings. The pure magnesium oxide material used in the implementation of the present invention is commercially available nano-magnesium oxide material.

[0041] Comparative Example 1

[0042] Step 1. Dissolve magnesium acetate in 500 mL of deionized water and sonicate until completely dissolved to form a homogeneous and clear solution.

[0043] Step 2. Spray drying to prepare powder precursor: First, uniformly flow deionized water into the spray dryer at a constant flow rate. Set the spray dryer equipment parameters to an inlet air temperature of 220℃, adjust the spray airflow size, and wait for the outlet air temperature to stabilize. At this time, the outlet air temperature should be greater than 100℃. Then, uniformly flow the magnesium acetate solution from Step 1 into the spray dryer at a constant flow rate. After the solution has completely entered the spray dryer, turn off the heater. After the equipment temperature drops to room temperature, turn off the equipment and remove the collector to collect the precursor powder.

[0044] Step 3. First calcination: The precursor powder is calcined at 600℃ for 4 hours in an argon atmosphere to perform a first calcination. After the calcination is completed, the product is taken out and ground to obtain the intermediate product.

[0045] Step 4. Secondary calcination: The intermediate product is placed in a muffle furnace and calcined at 400℃ for 2 hours for a secondary calcination. After calcination, pure magnesium oxide powder (labeled as MgO) is obtained.

[0046] Example 1

[0047] Compared to Comparative Example 1, the only difference is that lithium acetate was added in step 1, and the molar ratio of lithium to magnesium was 1:9. All other operations and parameters were the same as in Example 1. The resulting material was labeled LiMgO (also known as Li 0.1 Mg 0.9 (oxides).

[0048] Example 2

[0049] Compared to Comparative Example 1, the only difference is that in step 1, cerium nitrate hexahydrate was added, and the molar ratio of Ce to magnesium was 1:9. All other operations and parameters were the same as in Example 1. The resulting material was labeled CeMgO (also known as Ce...). 0.1 Mg 0.9 (oxides).

[0050] Example 3

[0051] Compared to Example 1, the only difference is that the molar ratio of lithium to magnesium in step 1 is changed to 1:19; all other operations and parameters are the same as in Example 1. The resulting material is labeled LiMgO(0.05) (also known as Li 0.05 Mg 0.95 (oxides).

[0052] Example 4

[0053] Compared with Comparative Example 1, the only difference is the addition of lanthanum nitrate hexahydrate and the molar ratio of La to magnesium being 1:9. All other operations and parameters are the same as in Example 1. The resulting material is labeled as LaMgO (also known as La0.1Mg0.9 oxide).

[0054] Example 5

[0055] Compared with Example 1, the only difference is that the inlet air temperature for atomization is 240°C, the temperature of the first stage of calcination is 700°C for 5 hours, and the time of the second stage of calcination is 450°C for 1 hour. All other operations and parameters are the same as in Example 1. The obtained material is labeled LiMgO(700).

[0056] Example 6

[0057] Compared to Example 1, the only difference is that a second-stage calcination was not performed; all other operations and parameters are the same as in Example 1. The resulting material is labeled LiMgO (single-stage calcination).

[0058] Comparative Example 2

[0059] Compared to Example 1, the only difference is that the raw materials were not spray-treated; instead, they were directly evaporated and desolventized to obtain the precursor, which was then subjected to subsequent sintering. All other operations and parameters were the same as in Example 1. The resulting material was labeled LiMgO-2.

[0060] Comparative Example 3

[0061] Compared to Example 2, the only difference is that the raw materials were not spray-treated; instead, they were directly evaporated and desoluble to obtain the precursor, which was then subjected to subsequent sintering. All other operations and parameters were the same as in Example 1. The resulting material was labeled CeMgO-2.

[0062] Comparative Example 4

[0063] Compared to Example 1, the only difference is that the atmosphere for the first stage of calcination is air; all other operations and parameters are the same as in Example 1. The resulting material is labeled LiMgO (air).

[0064] Comparative Example 5

[0065] Compared to Comparative Example 1, the only difference is that in step 1, zinc nitrate nonahydrate was added, and the molar ratio of Zn to magnesium was 1:9. All other operations and parameters were the same as in Example 1. The resulting material was labeled ZnMgO (also known as Zn). 0.1 Mg 0.9 (oxides).

[0066] Test 1:

[0067] Scanning electron microscope (SEM) images of Comparative Example 1, Example 1, Example 2, and the powder precursor of the present invention are shown below. Figure 1 and Figure 2 As shown, Figure 1 This is a SEM image of the powder precursor. Figure 2 The images provided are the overall SEM images of Comparative Example 1, Example 1, and Example 2. Figure 3 The images shown are magnified SEM images and partial magnified images of the materials in Comparative Example 1, Example 1, and Example 2, where a is pure magnesium oxide prepared in Comparative Example 1, b is LiMgO prepared in Example 1, and c is CeMgO prepared in Example 2.

[0068] pass Figure 1 It can be seen that the prepared powder precursor is a spherical micron-sized particle material with wrinkled surface. (Comparison) Figure 2 , 3 The image shows that after two calcinations, the precursor powder particles began to shrink inward due to the high temperature during the calcination process, the particle diameter began to decrease and slight agglomeration occurred. The material after calcination is still spherical particles, but the surface is rougher than that of the precursor particles.

[0069] Test 2:

[0070] Comparative Example 1, Example 1, and Example 2 x X-ray diffraction results as follows Figure 4 As shown, a is pure magnesium oxide prepared in Comparative Example 1, b is LiMgO prepared in Example 1, and c is CeMgO prepared in Example 2.

[0071] To compare and analyze the crystal phases of the antibacterial material before and after metal doping, the material was subjected to... x X-ray diffraction. From Figure 4 As can be seen, after comparison with the standard card, pure magnesium oxide perfectly matches the standard card, indicating that the magnesium oxide prepared according to the method of the claims has a stable crystal structure and high purity. It was also found that the lithium-loaded magnesium oxide material also perfectly matches the standard card, indicating that metal loading did not significantly alter the overall crystal phase of the material. However, a slight shift in the peak shape was observed after magnifying a single peak, indicating that the metal has been incorporated into the magnesium oxide and replaced the magnesium element. This achieves the purpose of preparing metal-doped magnesium oxide antibacterial materials.

[0072] Test 3:

[0073] The XPS test results for Comparative Example 1, Example 1, and Example 2 are as follows: Figure 5 As shown, a is pure magnesium oxide prepared in Comparative Example 1, b is LiMgO prepared in Example 1, and c is CeMgO prepared in Example 2.

[0074] It is denoted as CeMgO. The purpose of the XPS test is to verify whether the number of surface oxygen vacancies / defects has been improved.

[0075] The number of surface oxygen vacancies / defects is mainly determined by narrow-scanning of oxygen and the proportion of different peaks after peak splitting. Literature review indicates that lattice oxygen has a binding energy of 529.3–529.8 eV, while absorbing oxygen has a binding energy of 531.2–531.6 eV. Furthermore, as the number of surface oxygen vacancies increases, the number of external oxygen atoms...

[0076] As oxygen is absorbed onto the material surface, the oxygen content increases accordingly. Therefore, a higher oxygen content indicates a higher surface oxygen vacancy rate.

[0077] The more bits, the better. Figure 5 It can be seen that the oxygen absorption content increases after metal doping, indicating that metal doping effectively increases the number of oxygen vacancies on the surface of magnesium oxide.

[0078] Test 4:

[0079] Antibacterial performance test:

[0080] Metal doping can effectively improve the antibacterial properties of magnesium oxide. Gram-negative bacteria (E. coli, ATCC8739) were selected as the test subjects. The minimum inhibitory concentration (MIC) and inhibition rate were tested for Comparative Example 1, Example 1, and Example 2 to determine the performance difference in antibacterial properties of the magnesium oxide material before and after metal doping, demonstrating the effectiveness of this invention. The specific experimental steps are as follows:

[0081] Step 1. Bacterial Culture: The *E. coli* strain was cultured in LB medium at 37°C for 4–5 hours until the absorbance of the bacterial suspension at 600 nm reached 1.3–1.4. Under these conditions, the bacteria reached the logarithmic growth phase and exhibited the highest cell viability. It should be noted that all glassware and culture media used in the test were sterilized under high temperature and autoclave conditions at 121°C.

[0082] Step 2. Minimum Inhibitory Concentration (MIC) Test: Different concentrations of antimicrobial material were added to LB liquid (10 ml) medium, followed by the addition of 0.2 ml of logarithmic phase with a concentration of 10... 6 Bacterial cultures were collected. The mixture was incubated at 37°C for 24 hours. The minimum inhibitory concentration (MIC) was determined by the concentration of the sample in the clear bottle after incubation. Specific experimental sample images are shown below. Figure 6 As shown.

[0083] Step 3. Antibacterial rate test:

[0084] Blank control group setup: 1 mL of the original bacterial solution (bacterial concentration approximately 10) was added. 8 (cfu / mL) was added to 10 mL of physiological saline to obtain a blank control group.

[0085] Antibacterial test group: 1 mL of the original bacterial solution (bacterial concentration approximately 10) was added. 8 Add (cfu / mL) to 9 mL of physiological saline. Then, add 4 mg of different test samples, with a sample concentration of 400 μg / mL. -1 After incubating at 37°C for 15 minutes, 100 μL was evenly spread onto an agar plate. The plate was then incubated at 37°C for 24 hours, and the inhibition rate was calculated. The formula for calculating the inhibition rate is as follows:

[0086]

[0087] It should be noted that Ar represents the inhibition rate, A represents the count of live bacteria in the control group, and B represents the count of live bacteria in the experimental group.

[0088] according to Figure 6 The experimental results show that metal doping reduces the minimum inhibitory concentration (MIC) of the antibacterial material, indicating that metal doping significantly improves the antibacterial performance of magnesium oxide. Table 2 shows that, at the same material concentration, metal-doped magnesium oxide exhibits a higher antibacterial rate than pure magnesium oxide, indicating better antibacterial performance. Specifically, lithium-doped magnesium oxide demonstrates an antibacterial rate exceeding 99.99% after 15 minutes of antibacterial contact, while pure magnesium oxide only achieves a rate of 67.86%, showcasing the superior antibacterial performance of metal-doped magnesium oxide.

[0089] Table 1 Results of Minimum Inhibitory Concentration (MIC) Tests

[0090]

[0091] It should be noted that O represents turbidity, indicating bacterial growth, while x represents clarity, indicating the absence of bacterial growth.

[0092] Table 2 Bacterial counts after antibacterial tests on different samples

[0093]

[0094]

[0095] In summary, this invention directly atomizes a metal solution without the addition of a conventional carbon source, and then subjectes it to a first-stage calcination process in an oxygen-free atmosphere, particularly a second-stage calcination in an oxygen-containing atmosphere. This unexpectedly creates a gradient oxygen defect on the surface and also enables particle shrinkage to form a suitable wrinkled surface. Research in this invention shows that the material prepared using this method unexpectedly exhibits significantly improved antibacterial properties, particularly demonstrating excellent antibacterial activity against Gram-negative bacteria within a short timeframe.

[0096] The above are merely preferred embodiments of the present invention, and only describe the implementation of the present invention. They are not intended to limit the patent scope of the present invention. All equivalent structural transformations made using the contents of the present invention's specification and drawings under the technical concept of the present invention, or direct / indirect applications in other related technical fields, are included within the patent protection scope of the present invention.

Claims

1. An oxygen-deficient folding M for inhibiting Gram-negative bacteria x Mg 1-x The method for preparing oxide antibacterial materials is characterized by, A metal solution containing dissolved Mg and M sources is obtained, and then atomized to obtain metal raw material particles. These particles are then subjected to a first-stage calcination at 500-1000°C in an oxygen-free atmosphere, followed by a second-stage calcination at 350-450°C in an oxygen-containing atmosphere to produce the oxygen-defect wrinkled M source. x Mg 1-x Oxide antibacterial material; the particle size of the metal raw material is 1~5μm; the holding time at the first calcination temperature is 2~6h; the holding time at the second calcination temperature is 1~4h; The M mentioned x Mg 1-x In the oxide, M is at least one of Li or Ce; x is 0.1 to 0.15; Mg source and M source are water-soluble salts of various metal elements.

2. The oxygen-deficient fold M as described in claim 1 x Mg 1-x The method for preparing oxide antibacterial materials is characterized by, The Mg source and M source are at least one of the inorganic acid salts and acetates of each metal element.

3. The oxygen-deficient fold M as described in claim 1 x Mg 1-x The method for preparing oxide antibacterial materials is characterized by, The inlet air temperature for atomization is 180~240℃, and the outlet air temperature is 100~160℃.

4. The oxygen-deficient fold M as described in claim 1 x Mg 1-x The method for preparing oxide antibacterial materials is characterized by, The inlet air temperature for atomization is 200~240℃, and the outlet air temperature is 100~120℃.

5. The oxygen-deficient fold M as described in claim 1 x Mg 1-x The method for preparing oxide antibacterial materials is characterized by, The oxygen-free atmosphere is at least one of nitrogen or an inert gas.

6. The oxygen-deficient fold M as described in claim 1 x Mg 1-x The method for preparing oxide antibacterial materials is characterized by, The temperature for the first stage of calcination is 550~800℃.

7. The oxygen-deficient fold M as described in claim 1 x Mg 1-x The method for preparing oxide antibacterial materials is characterized by, The temperature of the first stage of calcination is 600~700℃; the holding time at the first stage of calcination temperature is 4~6h.

8. The oxygen-deficient fold M as described in claim 1 x Mg 1-x The method for preparing oxide antibacterial materials is characterized by, The holding time at the second calcination temperature is 1-2 hours.

9. An oxygen-deficient fold M prepared by the preparation method according to any one of claims 1 to 8 x Mg 1-x Oxide antibacterial materials.

10. An oxygen-deficient wrinkle M prepared by the preparation method according to any one of claims 1 to 8 x Mg 1-x The application of oxide antibacterial materials is characterized by, It is used as an antibacterial active ingredient in the preparation of antibacterial products that inhibit microorganisms; The microorganisms mentioned are Gram-negative bacteria.

11. An antibacterial product, characterized in that, Add oxygen-deficient folds M prepared by the preparation method according to any one of claims 1 to 8 x Mg 1-x Oxide antibacterial materials, and / or through the oxygen-deficient folds M x Mg 1-x Oxide antibacterial materials were prepared.

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