CN113512746A - Preparation method of medical titanium alloy bone plate surface nano coating - Google Patents
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- CN113512746A CN113512746A CN202110773159.7A CN202110773159A CN113512746A CN 113512746 A CN113512746 A CN 113512746A CN 202110773159 A CN202110773159 A CN 202110773159A CN 113512746 A CN113512746 A CN 113512746A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
- A61L27/306—Other specific inorganic materials not covered by A61L27/303 - A61L27/32
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
Abstract
A preparation method of a medical titanium alloy bone plate surface nano coating comprises the following steps: 1) pretreating a Ti6Al4V alloy plate to prepare a medical titanium alloy bone plate base plate; 2) a laser with the pulse width of 20ns, the wavelength of 1064nm and the working frequency of 5Hz is used; the power density is 5GW/cm2The laser beam with the lapping rate of 50 percent and the spot diameter of 2.4mm sequentially impacts the upper surface and the lower surface of the Ti6Al4V alloy plate; 3) the titanium alloy plate and the high-purity graphite plate are used as an anode and a cathode, are placed in parallel at a distance of 3cm and are immersed in electrolyte; the electrolyte is 0.3 wt% of NH4F and 2 vol% of water; the oxidation voltage is 60v, the time is 6h, and TiO is prepared2A nanotube coating; 4) deionized waterWashing, ultrasonically cleaning in absolute ethyl alcohol for 5min, and naturally drying; 5) placing the mixture in a vacuum atmosphere furnace for heat treatment; heating at a rate of 2 ℃/min, keeping the temperature at 450 ℃ for 2h, naturally cooling to room temperature, and taking out; the performances of wear resistance, binding force and the like are greatly improved.
Description
Technical Field
The invention relates to the technical field of medical titanium alloy, in particular to a preparation method of a nano coating on the surface of a medical titanium alloy bone plate.
Background
At present, the treatment of fracture diseases is mainly realized clinically by an internal fixation method. The internal fixation material mainly comprises titanium alloy (Ti6Al4V), and has the advantages of good tissue compatibility and accordance with biomechanics and clinical requirements. Although the titanium alloy bone fracture plate has excellent comprehensive performance, the following problems still exist:
(1) titanium is a biologically inert substance and rarely forms a direct chemical bond with bone tissue.
(2) Meanwhile, fine abrasive dust generated by friction and abrasion can be diffused to tissues around the bone fracture plate to easily cause adverse reactions.
(3) In open fracture and orthopedic implant surgery, titanium alloy bone plates often induce bacterial infection, despite the use of completely sterile and rigorous aseptic procedures. The main reason for this phenomenon is that the surface of the bone plate forms a layer of bacterial biofilm which can effectively resist the attack of the host immune system on bacteria, resulting in the failure of the surgery.
Therefore, it is highly desirable to modify the surface of titanium alloy properly, which can meet the requirement of internal fixation, and has bioactivity and improved clinical efficacy.
One promising approach is currently through anodic oxidationIn situ generation of TiO2And (4) coating the nanotube. The anodic oxidation method is a modification method of a nano structure and aims to form highly ordered TiO on the surface of titanium alloy2The nanotube coating has the advantages of simple process, low cost, controllable appearance of the prepared coating and the like. But at present TiO2The nanotube coating has poor properties such as wear resistance, binding force and the like, and is not favorable for clinical application.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a preparation method of a medical titanium alloy bone plate surface nano coating, which solves the existing problems and forms TiO2The performances of wear resistance, binding force and the like of the nanotube coating are improved, and the coating is more beneficial to clinical application.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a medical titanium alloy bone plate surface nano coating comprises the following steps:
step 1), selecting a Ti6Al4V alloy plate for pretreatment to prepare a medical titanium alloy bone plate foundation plate to be processed;
step 2), laser shock peening: a laser with the pulse width of 20ns, the wavelength of 1064nm and the working frequency of 5Hz is used; the power density is 5GW/cm2The laser beams with the lapping rate of 50 percent and the spot diameter of 2.4mm sequentially impact the upper surface and the lower surface of the Ti6Al4V alloy plate;
step 3), anodic oxidation treatment: fixing the titanium alloy plate subjected to laser shock strengthening on an end cover of an electrolytic cell through an electrode clamp to serve as an anode connected to a positive electrode of an oxidation power supply, selecting a high-purity graphite plate to serve as a cathode connected to a negative electrode of the power supply, keeping the two electrodes in parallel, enabling the distance between the anode and the cathode to be 3cm, and simultaneously immersing the anode and cathode samples into uniformly configured electrolyte;
wherein the electrolyte is 0.3 wt% NH4F and 2 vol% of water in ethylene glycol organic electrolyte;
opening an oxidation power switch, adjusting the anodic oxidation voltage to be 60v, and the oxidation time to be 6h to prepare TiO2A nanotube coating;
step 4), anodizing the junctionAnd after that, taking out the treated titanium alloy sample, quickly washing the titanium alloy sample by using a large amount of deionized water, then ultrasonically cleaning the titanium alloy sample in absolute ethyl alcohol for 5min to remove disordered filiform residues on the surface of the nanotube coating, and finally naturally airing to obtain TiO with clean and tidy surface2A nanotube coated titanium alloy bone plate;
step 5), TiO prepared by anodic oxidation method2The nanotube coating is amorphous and needs to be heat treated to obtain stable crystalline TiO2And (4) coating the nanotube. And (4) placing the sample obtained in the last step into a crucible, and placing the crucible into a vacuum atmosphere furnace for heat treatment. Setting the heating rate of the vacuum atmosphere furnace to be 2 ℃/min, preserving the heat for 2h at 450 ℃, naturally cooling to room temperature and taking out.
As a further technical scheme of the invention: in the step 2), during laser shock peening, transparent water flow with the thickness of 1mm is adopted for the constraint layer.
Further: in the step 2), the ablation layer is provided with an opaque black band adhered to the surface of a Ti6Al4V alloy plate material.
In addition, further: and 3) keeping the components of the electrolyte uniform and quickly dissipating heat through a magnetic stirrer in the whole anodic oxidation process.
Preferably: the thickness of the Ti6Al4V alloy plate is 3.5 mm.
Further, the method comprises the following steps: cutting a bone plate material Ti6Al4V into bone plate processing sizes by using an electric spark wire cutting machine; then sequentially grinding the surfaces of the samples by using 600-2500 # metallographic abrasive paper without obvious scratches, and then mechanically polishing the samples for 5-10min by using polishing cloth, wherein each sample is ground into a mirror surface; and ultrasonically cleaning the mixture by using absolute ethyl alcohol, and drying the mixture in a drying box for later use.
The invention has the beneficial effects that: the TiO being2The nanotube coating increases the surface roughness of the bone plate, and the increased roughness may enhance friction between the internal fixation systems, thereby providing better initial stability during healing and reducing deleterious wear during healing.
At the same time, TiO2The improvement in nanotube roughness also creates a larger surface for cell growthIs favorable for promoting the proliferation of the human mesenchymal stem cells.
Furthermore, as can be seen from the Wenzel equation, when the intrinsic contact angle is less than 90 (based on the results of the contact angle test), the increase in surface roughness makes the coating surface more hydrophilic, and the TiO is more hydrophilic2The roughness of the nanotube coating is increased and its hydrophilicity is also better. The higher hydrophilicity of the plate surface will aid cell adhesion.
Meanwhile, the inherent tubular structure of the nanotube can be used as a channel for transporting nutrient substances and proteins, and is beneficial to the rapid growth of adherent cells.
The anodized bone plate after laser shock strengthening can provide the strength required by the titanium alloy (Ti6Al4V) as a bone plate material, improve the defect of overhigh surface hardness and reduce the damage of the bone plate to periosteum in bones. The TiO being2The nanotube coating further enhances adhesion to the substrate. Namely, the higher the bonding strength of the coating and the substrate, the stronger the resistance to external damage, thereby being beneficial to the long-term existence of the coating on the bone fracture plate.
Drawings
The invention will be further explained and explained with reference to the drawings and examples:
FIG. 1(a) is a prior art nanotube coating (Ti6Al 4V-TiO)2) Surface and cross-sectional topography of the medium nanotube;
FIG. 1(b) is a nanotube coating (LSP-TiO) prepared using the method of the present invention2) Surface and cross-sectional topography of the medium nanotube;
FIG. 2(a) is a three-dimensional morphology of a titanium alloy plate (Ti6Al4V) before anodic oxidation in the prior art;
FIG. 2(b) is a three-dimensional morphology of a titanium alloy sheet material (Ti6Al4V-LSP) after laser shock peening using the method of the present invention;
FIG. 2(c) is the titanium alloy plate in FIG. 2(a) after being anodized to prepare a nanotube coating (Ti6Al 4V-TiO)2) A three-dimensional topography map of (a);
FIG. 2(d) is a schematic view of the titanium alloy sheet shown in FIG. 2(b) after being anodized to prepare a nanotube coating (LSP-TiO)2) A three-dimensional topography map of (a);
FIG. 3(a) is a digital photograph of the titanium alloy sheet material (Ti6Al4V) of FIG. 2(a) having water droplets on the surface;
FIG. 3(b) is a digital photograph of Ti6Al4V-LSP from FIG. 2(b) with water droplets on the surface;
FIG. 3(c) is the Ti6Al4V-TiO shown in FIG. 2(c)2A digital photograph of a water droplet on the surface;
FIG. 3(d) is the LSP-TiO of FIG. 2(d)2A digital photograph of a water droplet on the surface;
FIG. 4 shows Ti6Al4V-TiO2And LSP-TiO2A typical measurement curve of adhesion of the coating to a titanium alloy substrate of (a);
FIG. 5(a) shows Ti6Al4V, Ti6Al4V-LSP, Ti6Al4V-TiO2、LSP-TiO2The change curve of the friction coefficients of the four materials along with time;
FIG. 5(b) shows Ti6Al4V, Ti6Al4V-LSP, Ti6Al4V-TiO2、LSP-TiO2Average friction coefficient of four materials;
FIG. 6 shows Ti6Al4V, Ti6Al4V-LSP, Ti6Al4V-TiO2、LSP-TiO2Average wear quality of four materials.
Detailed Description
The preparation method of the nano coating on the surface of the medical titanium alloy bone plate comprises the following steps:
step 1), selecting a Ti6Al4V alloy plate for pretreatment to prepare a medical titanium alloy bone plate foundation plate to be processed;
the thickness of the Ti6Al4V alloy plate in the embodiment is 3.5 mm.
The pretreatment comprises the following steps: cutting a bone plate material Ti6Al4V into bone plate processing sizes by using an electric spark wire cutting machine; then sequentially grinding the surfaces of the samples by using 600-2500 # metallographic abrasive paper without obvious scratches, and then mechanically polishing the samples for 5-10min by using polishing cloth, wherein each sample is ground into a mirror surface; and ultrasonically cleaning the mixture by using absolute ethyl alcohol, and drying the mixture in a drying box for later use.
Step 2), laser shock peening: a laser with the pulse width of 20ns, the wavelength of 1064nm and the working frequency of 5Hz is used; the power density is 5GW/cm2The laser beams with the lap joint rate of 50 percent and the spot diameter of 2.4mm sequentially impact onThe upper surface and the lower surface of the Ti6Al4V alloy plate;
in this embodiment, the restriction layer is a transparent water flow with a thickness of 1mm during laser shock peening.
The surface of the ablation layer is provided with an opaque black band which is adhered to the surface of a Ti6Al4V alloy plate material, and the opaque black band can effectively inhibit the heat effect of laser on the base material.
Step 3), anodic oxidation treatment: fixing the titanium alloy plate subjected to laser shock strengthening on an end cover of an electrolytic cell through an electrode clamp to serve as an anode connected to a positive electrode of an oxidation power supply, selecting a high-purity graphite plate to serve as a cathode connected to a negative electrode of the power supply, keeping the two electrodes in parallel, enabling the distance between the anode and the cathode to be 3cm, and simultaneously immersing the anode and cathode samples into uniformly configured electrolyte;
wherein the electrolyte is 0.3 wt% NH4F and 2 vol% of water in ethylene glycol organic electrolyte;
opening an oxidation power switch, adjusting the anodic oxidation voltage to be 60v, and the oxidation time to be 6h to prepare TiO2A nanotube coating;
in the embodiment, the components of the electrolyte are kept uniform and the heat is rapidly dissipated by a magnetic stirrer in the whole anodic oxidation process in the step 3).
Step 4), after the anodic oxidation treatment is finished, taking out the treated titanium alloy sample, rapidly washing the titanium alloy sample by using a large amount of deionized water, then ultrasonically cleaning the titanium alloy sample in absolute ethyl alcohol for 5min to remove disordered filiform residues on the surface of the nanotube coating, and finally naturally airing the titanium alloy sample to obtain TiO with clean and tidy surface2A nanotube coated titanium alloy bone plate;
step 5), TiO prepared by anodic oxidation method2The nanotube coating is amorphous and needs to be heat treated to obtain stable crystalline TiO2And (4) coating the nanotube. And (4) placing the sample obtained in the last step into a crucible, and placing the crucible into a vacuum atmosphere furnace for heat treatment. Setting the heating rate of the vacuum atmosphere furnace to be 2 ℃/min, preserving the heat for 2h at 450 ℃, naturally cooling to room temperature and taking out.
In FIG. 1, (a) and (b) are respectively in Ti6Al4V bone plate and excitedLight Shock Peening (LSP) TiO 6Al4V bone plate surface2Surface and cross-sectional topography of the nanotube coating. It was found that TiO was uniformly aligned on both surfaces2And (4) coating the nanotube. Although the pipe orifice of the nanotube in each sample is circular or oval, the pipe wall is clear and complete, the length of the nanotube and the size of the inner diameter and the outer diameter of the nanotube are obviously different, so that the nanotube prepared by the method has thicker pipe wall and increased pipe length, and the thicker pipe wall can enhance the bearing capacity of the nanotube.
In this example, the substrate, the anodized substrate, the laser shock-strengthened substrate, and the anodized substrate after laser shock strengthening were named Ti6Al4V and Ti6Al4V-TiO, respectively2Ti6Al4V-LSP and LSP-TiO2。
The three-dimensional shapes of the four materials are respectively shown in fig. 2(a), (b), (c) and (d), and each contour graph is marked with a depth value. It can be readily seen from FIGS. 2(a-b) that the surface morphology of the Ti6Al4V-LSP sample exhibits a significant change compared to the Ti6Al4V sample. It can be seen in fig. 2(c-d) that the surface roughness of the sample after anodization increased significantly, with roughness ranging from 0.5 μm to 4.5 μm, which means that the overall smoothness of the sample decreased.
The digital photographs of the four materials with water drops on the surface are shown in fig. 3(a), (b), (c), and (d), wherein the contact angles of the surfaces are marked; both fig. 3(a-b) clearly show that the water droplets on the surface of the Ti6Al4V and Ti6Al4V-LSP samples were spherical with contact angles of 65.4 ° and 59.3 °, respectively. In FIG. 3(c-d) Ti6Al4V-TiO can be seen2And LSP-TiO2The sample surface droplet was arced with contact angles falling to 19.6 and 13.6, respectively, indicating improved hydrophilicity of the bone plate.
Typical measurement curves of adhesion as shown in fig. 4, when the applied load exceeds the adhesion of the coating to the substrate, the coating is scratched, and the acoustic signal (red line) and the friction force (blue line) fluctuate dramatically at the same time, which is the critical load of the adhesion of the coating to the substrate. Ti6Al4V-TiO2And LSP-TiO2The adhesion force of the coating and the matrix of the sample is respectively 10.7 +/-20.6N and 12.6 + -0.5N. LSP-TiO2The strongest adhesion was obtained because of LSP-TiO2The coating of the sample showed a ratio to Ti6Al4V-TiO2The coated samples of the test specimens had denser surface and greater thickness.
Fig. 5(a) is a friction coefficient curve of four samples in a simulated body fluid environment, and the average friction coefficients thereof are summarized in fig. 5 (b). Fig. 5 shows the average wear quality of the four samples. The results show that LSP-TiO2The average coefficient of friction and wear quality of the test specimens were the lowest.
The TiO prepared by the method of the invention can be known by detecting and analyzing the sample2The nanotube coating increases the surface roughness of the bone plate, and the increased roughness may enhance friction between the internal fixation systems, thereby providing better initial stability during healing and reducing deleterious wear during healing. At the same time, TiO2The improvement of the roughness of the nanotube also creates a larger surface for the growth of cells, which is beneficial to promoting the proliferation of the mesenchymal stem cells of the human bone marrow. Further, as can be seen from the Wenzel equation, when the intrinsic contact angle is less than 90 (based on the results of the contact angle test), the increase in surface roughness makes the coating surface more hydrophilic2The roughness of the nanotube coating is increased and its hydrophilicity is also better. The higher hydrophilicity of the plate surface will aid cell adhesion. Meanwhile, the inherent tubular structure of the nanotube can be used as a channel for transporting nutrient substances and proteins, and is beneficial to the rapid growth of adherent cells. The anodized bone plate after laser shock strengthening can provide the strength required by the titanium alloy (Ti6Al4V) as a bone plate material, improve the defect of overhigh surface hardness and reduce the damage of the bone plate to periosteum in bones. The TiO being2The nanotube coating further enhances adhesion to the substrate. In other words, the greater the bond strength of the coating to the substrate, the greater the resistance to external damage, thereby facilitating the long-term presence of the coating on the bone plate.
In conclusion, the coating has larger surface roughness, higher hydrophilicity, stronger bonding force and better wear resistance. The coating improves the bioactivity of the surface of the bone plate and the wear resistance of the bone plate, and is beneficial to clinical application.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention and do not limit the scope of the present invention, and various modifications and improvements of the present invention may be made by those skilled in the art without departing from the spirit of the present invention as defined by the appended claims.
Claims (6)
1. A preparation method of a medical titanium alloy bone plate surface nano coating is characterized by comprising the following steps:
step 1), selecting a Ti6Al4V alloy plate for pretreatment to prepare a medical titanium alloy bone plate foundation plate to be processed;
step 2), laser shock peening: a laser with the pulse width of 20ns, the wavelength of 1064nm and the working frequency of 5Hz is used; the power density is 5GW/cm2The laser beams with the lapping rate of 50 percent and the spot diameter of 2.4mm sequentially impact the upper surface and the lower surface of the Ti6Al4V alloy plate;
step 3), anodic oxidation treatment: fixing the titanium alloy plate subjected to laser shock strengthening on an end cover of an electrolytic cell through an electrode clamp to serve as an anode connected to a positive electrode of an oxidation power supply, selecting a high-purity graphite plate to serve as a cathode connected to a negative electrode of the power supply, keeping the two electrodes in parallel, enabling the distance between the anode and the cathode to be 3cm, and simultaneously immersing the anode and cathode samples into uniformly configured electrolyte;
wherein the electrolyte is 0.3 wt% NH4F and 2 vol% of water in ethylene glycol organic electrolyte;
opening an oxidation power switch, adjusting the anodic oxidation voltage to be 60v, and the oxidation time to be 6h to prepare TiO2A nanotube coating;
step 4), after the anodic oxidation treatment is finished, taking out the treated titanium alloy sample, rapidly washing the titanium alloy sample by using a large amount of deionized water, then ultrasonically cleaning the titanium alloy sample in absolute ethyl alcohol for 5min to remove disordered filiform residues on the surface of the nanotube coating, and finally naturally airing the titanium alloy sample to obtain TiO with clean and tidy surface2A nanotube coated titanium alloy bone plate;
step 5), TiO prepared by anodic oxidation method2The nanotube coating is amorphous and needs to be heat treated to obtain stable crystalline TiO2And (4) coating the nanotube. And (4) placing the sample obtained in the last step into a crucible, and placing the crucible into a vacuum atmosphere furnace for heat treatment. Setting the heating rate of the vacuum atmosphere furnace to be 2 ℃/min, preserving the heat for 2h at 450 ℃, naturally cooling to room temperature and taking out.
2. The method for preparing the nano coating on the surface of the medical titanium alloy bone plate according to claim 1, which is characterized in that: in the step 2), during laser shock peening, transparent water flow with the thickness of 1mm is adopted for the constraint layer.
3. The method for preparing the nano coating on the surface of the medical titanium alloy bone plate according to claim 1 or 2, which is characterized in that: in the step 2), the ablation layer is provided with an opaque black strip which is adhered to the surface of the Ti6Al4V alloy plate.
4. The method for preparing the nano coating on the surface of the medical titanium alloy bone plate according to claim 1, which is characterized in that: and 3) keeping the components of the electrolyte uniform and quickly dissipating heat through a magnetic stirrer in the whole anodic oxidation process.
5. The method for preparing the nano coating on the surface of the medical titanium alloy bone plate according to claim 1, which is characterized in that: the thickness of the Ti6Al4V alloy plate is 3.5 mm.
6. The method for preparing the nano coating on the surface of the medical titanium alloy bone plate according to claim 5, wherein the method comprises the following steps: cutting a bone plate material Ti6Al4V into bone plate processing sizes by using an electric spark wire cutting machine; then sequentially grinding the surfaces of the samples by using 600-2500 # metallographic abrasive paper without obvious scratches, and then mechanically polishing the samples for 5-10min by using polishing cloth, wherein each sample is ground into a mirror surface; and ultrasonically cleaning the mixture by using absolute ethyl alcohol, and drying the mixture in a drying box for later use.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115970057A (en) * | 2022-09-09 | 2023-04-18 | 浙江科惠医疗器械股份有限公司 | Petal-shaped TiO 2 Preparation method of nano-pore antibacterial coating |
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