Medical antibacterial dressing containing Zn / Ce electrode array and preparation method thereof
By preparing a Zn/Ce electrode array on the surface of cotton non-woven fabric and combining it with the microbattery effect, the problem of high cost of existing medical dressings is solved, and a medical antibacterial dressing with excellent antibacterial performance and low price is achieved, while ensuring biocompatibility.
Patent Information
- Application Number
- CN202311820324.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-27
- Publication Date
- 2025-09-19
- Estimated Expiration
- 2043-12-27
AI Technical Summary
Existing medical dressings use rare and precious metal silver as an antibacterial agent, which leads to high costs. There is an urgent need to develop an alternative material with excellent antibacterial properties and low price.
A Zn/Ce electrode array was prepared on the surface of cotton nonwoven fabric. The Ce and Zn electrode array was formed by sputtering technology. Combined with the microbattery effect, the antibacterial effect was improved, and the Zn content was controlled at 13%-36% to ensure biocompatibility.
A medical antibacterial dressing with excellent antibacterial performance and low price has been achieved. The microcurrent effect significantly improves the antibacterial effect while ensuring biocompatibility.
Abstract
Description
Technical Field
[0001] The present invention relates to the field of medical dressings, and in particular to a medical antibacterial dressing comprising a Zn / Ce electrode array and a preparation method thereof. Background Art
[0002] Inorganic antimicrobial agents have excellent antibacterial and antibacterial properties and are widely used in antimicrobial research and product development. Among various antimicrobial metal ions, silver ions have the best antimicrobial effect, boasting broad-spectrum, high efficacy, long-lasting efficacy, and resistance to drug resistance. Consequently, the inorganic antimicrobial agent currently used in medical dressings is mostly metallic silver. However, silver is a rare and precious metal, and its high price inevitably leads to rising medical costs. Therefore, there is an urgent need to design a medical antimicrobial dressing with excellent antimicrobial properties and low cost. Summary of the Invention
[0003] The object of the present invention is to provide a method for preparing a medical antibacterial dressing comprising a Zn / Ce electrode array. The medical antibacterial dressing prepared by the method has the advantages of excellent antibacterial performance and low price.
[0004] The technical solutions of the present invention are as follows:
[0005] A method for preparing a medical antibacterial dressing comprising a Zn / Ce electrode array comprises the following steps:
[0006] Substrate pretreatment: Cut the cotton nonwoven fabric into appropriate size, clean it with anhydrous ethanol and ultrasonic for 15 minutes to remove surface impurities, and dry it under inert gas for later use;
[0007] Preparation of Zn / Ce electrode array: Place the dried cotton nonwoven fabric into a magnetron sputtering coating machine, use Ce2O3 as the target material and argon as the working gas to form a Ce electrode array on the surface of the cotton nonwoven fabric. During the sputtering process, the background vacuum degree is 10 - 4 Pa, argon flow rate is 40-50sccm, working pressure is 1.0-1.2Pa, sputtering time is 15-18min; then Zn is used as target material and argon is used as working gas to form Zn electrode array on the surface of cotton nonwoven fabric. During the sputtering process, the background vacuum degree is 10 -4 Pa, argon flow rate is 40-50sccm, working pressure is 1.0-1.2Pa, and sputtering time is 15-18min; by adjusting the target power of the two sputterings, the mass content of Zn in the Zn / Ce electrode array is made to be 13%-50%.
[0008] Preferably, the size of the cotton nonwoven fabric is 10 cm*5 cm.
[0009] Preferably, the argon gas flow rate for both sputtering operations is 50 sccm.
[0010] Preferably, the working pressure of both sputtering processes is 1.0 Pa.
[0011] Preferably, the sputtering time of the Zn target is 15 minutes.
[0012] Preferably, the sputtering time of the Ce2O3 target is 15 minutes.
[0013] Preferably, the mass content of Zn in the Zn / Ce electrode array is 36%.
[0014] Furthermore, the present invention also provides a medical antibacterial dressing comprising a Zn / Ce electrode array prepared by the above preparation method.
[0015] In order to obtain a medical antibacterial dressing with excellent antibacterial performance and low price, the present invention prepares a Zn / Ce electrode array on the surface of a cotton nonwoven fabric and forms a microbattery on the surface. 2+ or Ce 3+ In addition to its antibacterial properties, the Zn / Ce electrodes also exert a microcurrent effect, which significantly enhances the antibacterial effect. Furthermore, as the Zn content in the Zn / Ce electrode array increases, the material's hemolysis rate exhibits irregular changes. When the Zn content reaches 50%, the dressing's hemolysis rate becomes unacceptable. Therefore, for the biocompatibility of medical dressings, the Zn content in the Zn / Ce electrode array should be controlled between 13% and 36%. DETAILED DESCRIPTION
[0016] The technical effects of the present invention are verified below through specific examples, but the embodiments of the present invention are not limited thereto.
[0017] Example 1
[0018] Substrate pretreatment: Cut the cotton nonwoven fabric into a size of 10 cm*5 cm, clean it with anhydrous ethanol and ultrasonic for 15 minutes to remove surface impurities, and dry it under inert gas for later use;
[0019] Preparation of Zn / Ce electrode array: Place the dried cotton nonwoven fabric into a magnetron sputtering coating machine, use Ce2O3 as the target material and argon as the working gas to form a Ce electrode array on the surface of the cotton nonwoven fabric. During the sputtering process, the background vacuum degree is 10 - 4 Pa, argon flow rate is 40sccm, working pressure is 1.0Pa, sputtering time is 15min; then Zn is used as target material and argon is used as working gas to form Zn electrode array on the surface of cotton nonwoven fabric. During the sputtering process, the background vacuum degree is 10 -4Pa, argon flow rate of 50 sccm, working pressure of 1.2 Pa, sputtering time of 15 min. By adjusting the target power of the two sputterings, the mass content of Zn in the Zn / Ce electrode array was made to be 13%.
[0020] Example 2
[0021] Substrate pretreatment: Cut the cotton nonwoven fabric into a size of 10 cm*5 cm, clean it with anhydrous ethanol and ultrasonic for 15 minutes to remove surface impurities, and dry it under inert gas for later use;
[0022] Preparation of Zn / Ce electrode array: Place the dried cotton nonwoven fabric into a magnetron sputtering coating machine, use Ce2O3 as the target material and argon as the working gas to form a Ce electrode array on the surface of the cotton nonwoven fabric. During the sputtering process, the background vacuum degree is 10 - 4 Pa, argon flow rate is 40sccm, working pressure is 1.0Pa, sputtering time is 15min; then Zn is used as target material and argon is used as working gas to form Zn electrode array on the surface of cotton nonwoven fabric. During the sputtering process, the background vacuum degree is 10 -4 Pa, argon flow rate of 50 sccm, working pressure of 1.2 Pa, sputtering time of 15 min. By adjusting the target power of the two sputterings, the mass content of Zn in the Zn / Ce electrode array was made to be 20%.
[0023] Example 3
[0024] Substrate pretreatment: Cut the cotton nonwoven fabric into a size of 10 cm*5 cm, clean it with anhydrous ethanol and ultrasonic for 15 minutes to remove surface impurities, and dry it under inert gas for later use;
[0025] Preparation of Zn / Ce electrode array: Place the dried cotton nonwoven fabric into a magnetron sputtering coating machine, use Ce2O3 as the target material and argon as the working gas to form a Ce electrode array on the surface of the cotton nonwoven fabric. During the sputtering process, the background vacuum degree is 10 - 4 Pa, argon flow rate is 40sccm, working pressure is 1.0Pa, sputtering time is 15min; then Zn is used as target material and argon is used as working gas to form Zn electrode array on the surface of cotton nonwoven fabric. During the sputtering process, the background vacuum degree is 10 -4 Pa, argon flow rate of 50 sccm, working pressure of 1.2 Pa, sputtering time of 15 min. By adjusting the target power of the two sputterings, the mass content of Zn in the Zn / Ce electrode array was made to be 28%.
[0026] Example 4
[0027] Substrate pretreatment: Cut the cotton nonwoven fabric into a size of 10 cm*5 cm, clean it with anhydrous ethanol and ultrasonic for 15 minutes to remove surface impurities, and dry it under inert gas for later use;
[0028] Preparation of Zn / Ce electrode array: Place the dried cotton nonwoven fabric into a magnetron sputtering coating machine, use Ce2O3 as the target material and argon as the working gas to form a Ce electrode array on the surface of the cotton nonwoven fabric. During the sputtering process, the background vacuum degree is 10 - 4 Pa, argon flow rate is 40sccm, working pressure is 1.0Pa, sputtering time is 15min; then Zn is used as target material and argon is used as working gas to form Zn electrode array on the surface of cotton nonwoven fabric. During the sputtering process, the background vacuum degree is 10 -4 Pa, argon flow rate of 50 sccm, working pressure of 1.2 Pa, sputtering time of 15 min. By adjusting the target power of the two sputterings, the mass content of Zn in the Zn / Ce electrode array was made to be 36%.
[0029] Example 5
[0030] Substrate pretreatment: Cut the cotton nonwoven fabric into a size of 10 cm*5 cm, clean it with anhydrous ethanol and ultrasonic for 15 minutes to remove surface impurities, and dry it under inert gas for later use;
[0031] Preparation of Zn / Ce electrode array: Place the dried cotton nonwoven fabric into a magnetron sputtering coating machine, use Ce2O3 as the target material and argon as the working gas to form a Ce electrode array on the surface of the cotton nonwoven fabric. During the sputtering process, the background vacuum degree is 10 - 4 Pa, argon flow rate is 40sccm, working pressure is 1.0Pa, sputtering time is 15min; then Zn is used as target material and argon is used as working gas to form Zn electrode array on the surface of cotton nonwoven fabric. During the sputtering process, the background vacuum degree is 10 -4 Pa, argon flow rate of 50 sccm, working pressure of 1.2 Pa, sputtering time of 15 min. By adjusting the target power of the two sputterings, the mass content of Zn in the Zn / Ce electrode array was made to be 50%.
[0032] Comparative Example 1
[0033] Substrate pretreatment: Cut the cotton nonwoven fabric into a size of 10 cm*5 cm, clean it with anhydrous ethanol and ultrasonic for 15 minutes to remove surface impurities, and dry it under inert gas for later use;
[0034] Preparation of Ce electrode array: The only difference between this step and Example 4 is that only Ce array is prepared in both sputtering steps, and the other process conditions are exactly the same.
[0035] Comparative Example 2
[0036] Substrate pretreatment: Cut the cotton nonwoven fabric into a size of 10 cm*5 cm, clean it with anhydrous ethanol and ultrasonic for 15 minutes to remove surface impurities, and dry it under inert gas for later use;
[0037] Preparation of Zn electrode array: The only difference between this step and Example 4 is that only Zn electrode array is prepared in both sputtering steps, and the other process conditions are exactly the same.
[0038] Next, we evaluated the antibacterial properties and biocompatibility of the samples in Examples 1-5 and Comparative Examples 1-2. The specific methods are as follows:
[0039] Antibacterial performance: The concentration of bacterial solution was selected to be 4×10 6 cfu / ml of Staphylococcus aureus was used as the test bacterial solution. 0.2 ml of the test bacterial solution was dripped onto the sample surface and incubated at 37°C and relative humidity RH>90% for 48 hours. The samples were then taken out for viable bacterial counts, and the antibacterial rate was obtained by counting. Five parallel tests were performed on each sample, with a blank cotton nonwoven fabric as the control group. The antibacterial rate calculation formula is:
[0040] R(%)=(AB) / A×100
[0041] Where: R represents the antibacterial rate;
[0042] A represents the average number of recovered bacteria in the control group;
[0043] B represents the average number of recovered bacteria in the examples or comparative examples.
[0044] Biocompatibility: The biocompatibility of each sample was evaluated through a hemolysis test. The principle is to directly contact the sample with blood and measure the amount of hemoglobin released after the red blood cell membrane ruptures to determine the degree of hemolysis of each sample in vitro. Hemoglobin absorbs at a wavelength of 545nm, and its concentration can be measured using a spectrophotometer. The specific steps are as follows:
[0045] (1) After anesthetizing and fixing a healthy rabbit, slowly draw 4 mL of venous blood from the rabbit's ear vein, add 0.2 mL of 2% potassium oxalate to prepare fresh anticoagulated blood, and dilute with 5 mL of 0.9% sodium chloride injection.
[0046] (2) Take three siliconized test tubes, add the test sample and 10 mL of sodium chloride injection into one test tube, add 10 mL of sodium chloride saline into one blank test tube as a negative control group, and add 10 mL of distilled water into the other blank test tube as a positive control group.
[0047] (3) All test tubes were kept in a 37°C water bath for 30 min, 0.2 mL of anticoagulated rabbit blood was added to each tube, and the tubes were kept at 37°C for 60 min. The tubes were then centrifuged at 1000 rpm for 5 min.
[0048] (4) Take the supernatant from the test tube and measure the absorbance at a wavelength of 545 nm. Perform three parallel tests for each sample and take the average value.
[0049] The formula for calculating the hemolysis rate is as follows:
[0050] Hemolysis rate (%) = (average absorbance of sample - absorbance of negative group) / (absorbance of positive group - absorbance of negative group) × 100
[0051] The test results are shown in Table 1.
[0052] Table 1 Antibacterial rate and hemolysis rate of each sample
[0053] serial number Antibacterial rate / % Hemolysis rate / % Example 1 85.1 5.3 Example 2 87.3 2.7 Example 3 92.5 4.3 Example 4 98.1 6.2 Example 5 89.3 11.6 Comparative Example 1 62.1 3.1 Comparative Example 2 75.6 14.2
[0054] After the Zn / Ce electrode array was prepared on the surface of cotton nonwoven fabric, a microbattery was formed on its surface, and the antibacterial method was to remove the original Zn 2+ or Ce 3+ In addition to its antibacterial properties, the Zn / Ce electrodes also exert a microcurrent effect, which significantly enhances the antibacterial effect, as shown in Table 1. Furthermore, as the Zn content in the Zn / Ce electrode array increases, the material's hemolysis rate exhibits irregular changes. When the Zn content reaches 50%, the dressing's hemolysis rate becomes unacceptable. Therefore, for the biocompatibility of medical dressings, the Zn content in the Zn / Ce electrode array should be controlled between 13% and 36%.
[0055] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the technical principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.
Claims
1. A method for preparing a medical antibacterial dressing comprising a Zn / Ce2O3 electrode array, characterized in that: The preparation method consists of the following steps: Substrate pretreatment: Cut the cotton nonwoven fabric into appropriate size, clean it with anhydrous ethanol and ultrasonic for 15 minutes to remove surface impurities, and dry it under inert gas for later use; Preparation of Zn / Ce2O3 electrode array: Place the dried cotton nonwoven fabric into a magnetron sputtering coating machine, use Ce2O3 as the target material and argon as the working gas to form a Ce2O3 electrode array on the surface of the cotton nonwoven fabric. During the sputtering process, the background vacuum degree is 10 - 4 Pa, argon flow rate is 40-50sccm, working pressure is 1.0-1.2Pa, sputtering time is 15-18min; then Zn is used as target material and argon is used as working gas to form Zn electrode array on the surface of cotton nonwoven fabric. During the sputtering process, the background vacuum degree is 10 -4 Pa, argon flow rate is 40-50sccm, working pressure is 1.0-1.2Pa, and sputtering time is 15-18min; by adjusting the target power of the two sputterings, the mass content of Zn in the Zn / Ce2O3 electrode array is made to be 20%-28%.
2. A preparation method according to claim 1, characterized in that: The size of the cotton nonwoven fabric is 10 cm*5 cm.
3. A preparation method according to claim 1, characterized in that: The argon gas flow rate for both sputtering processes was 50 sccm.
4. A preparation method according to claim 1, characterized in that: The working pressure of both sputtering processes was 1.0 Pa.
5. A preparation method according to claim 1, characterized in that: The sputtering time of the Zn target was 15 min.
6. A preparation method according to claim 1, characterized in that: The sputtering time of Ce2O3 target is 15min.
7. A medical antibacterial dressing comprising a Zn / Ce2O3 electrode array prepared by the preparation method according to any one of claims 1 to 6.
Citation Information
Patent Citations
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CN101637679A
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CN103640282A
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WO2008028355A1