CN103882497A - Method for preparing composite ceramic membrane on surface of magnesium alloy intravascular stent by micro-arc oxidation - Google Patents
Method for preparing composite ceramic membrane on surface of magnesium alloy intravascular stent by micro-arc oxidation Download PDFInfo
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Abstract
The invention discloses a method for preparing a composite ceramic membrane on the surface of a magnesium alloy intravascular stent by micro-arc oxidation. The method comprises the following steps: 1) preparing an electrolyte; 2) performing micro-arc oxidation treatment by taking the magnesium alloy intravascular stent as an anode, taking a stainless steel plate as a cathode and taking a stainless steel wire with the surface coated with an insulating plastic membrane as an auxiliary cathode so as to in-situ grow a layer of uniform composite ceramic membrane on the surface of the magnesium alloy intravascular stent. Micron-grade holes which are uniformly distributed in the prepared composite ceramic membrane can be used as carriers for directly transporting a medicament to a lesion part in a tubular cavity. When the composite ceramic membrane is not subjected to hole sealing post-treatment, the resistance to corrosion of neutral NaCl salt mist can be up to 500h, the resistance to corrosion of a simulated body fluid environment can be up to 2400h, and the fracture toughness is obviously improved. The preparation process disclosed by the invention has the advantages of high efficiency and energy conservation.
Description
Technical field
The invention belongs to metal material surface processing technology field, especially relate to a kind of method that magnesium alloy blood vessel rack surface by micro-arc oxidation is prepared composite ceramic film.
Background technology
Endoluminal stent is a kind of fabulous medical device of the narrow symptom curative effect of various pipelines that is used for the treatment of, and along with growth in the living standard, people also more and more pay attention to the health of self health, in modern medical service, the demand of endoluminal stent are also being increased rapidly.But the support of clinical application at present also exists some problems, except structure design aspect needs further to optimize, main is erosion resistance and the biocompatibility problem to be improved of endoluminal stent material.Therefore, research is carried out surface modification treatment further to improve its biocompatibility to endoluminal stent material, reduces thrombosis to bottom line, thoroughly eliminates the rear human body rejection of support implantation and angiostenosis and is necessary.
MAGNESIUM METAL and alloy thereof appear in the newspapers repeatly as the correlative study of biodegradable stent material, because MAGNESIUM METAL has extremely low current potential, very easily be corroded at wet environment and contain chlorion in the situation that, therefore also for it provides prerequisite as degradable material, application magnesium alloy is made biodegradable endoluminal stent becomes the focus of current research.No matter from mechanical property or biocompatibility, magnesium alloy is all fabulous body implanting material, but because the magnesium alloy utmost point is not anti-corrosion, in human body fluid and blood, the corrosion speed of magnesium alloy is too fast, after degraded, will lose support function, causes the state of an illness to worsen once again.After degradable magnesium support is implanted, endothelialization is complete and rapid, a small amount of neointimal hyperplasia, inflammatory reaction is low, in follow-up period, be not in the mood for stalk, subacute or advanced thrombus and cardiac death event, therefore improve magnesium alloy materials corrosion resisting property and degraded after support performance be solve its critical problem as endoluminal stent material.
While at present magnesium alloy being carried out to differential arc oxidation processing, adopt silicate, phosphoric acid salt and meta-aluminate solution system as electrolytic solution, the ceramic membrane of preparation is all improved significantly at aspects such as solidity to corrosion, hardness, wear resistancies more.But, along with the continuous popularization of magnesium alloy range of application, the requirement of being prepared by magnesium alloy differential arc oxidation to ceramic membrane also improves constantly, especially when magnesium alloy is applied as endoluminal stent material, on endoluminal stent material, the solidity to corrosion of ceramic membrane that differential arc oxidation forms and toughness all need to meet further requirement, and ceramic membrane prepared by prior art cannot meet the requirement to endoluminal stent material in medical field.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned deficiency of the prior art, provides a kind of magnesium alloy blood vessel rack surface by micro-arc oxidation to prepare the method for composite ceramic film.Adopt electrolytic solution of the present invention and preparation technology parameter, can obtain even, the fine and close composite ceramic film of one deck for intraluminal magnesium alloy blood vessel rack surface fast, this composite ceramic film is mainly by MgF
2, Mg
2zr
5o
12, t-ZrO
2with MgO phase composite, its speed of growth is up to 1.5 μ m/min～3.0 μ m/min, the present invention has efficiently, energy-conservation advantage, in this composite ceramic film, the micrometer grade hole of equally distributed 1 μ m～2 μ m can directly be transported to medicine intraluminal lesions position as carrier simultaneously, utilize surface coverage to have the magnesium alloy blood vessel rack of composite ceramic film to have simply as endoluminal stent material, fast, feature reliably, the composite ceramic film of preparation is not in the time carrying out sealing of hole aftertreatment, resistance to neutral NaCl salt air corrosion reaches 500h, the environmental corrosion of resistance to simulated body fluid reaches 2400h, fracture toughness property obviously improves.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of magnesium alloy blood vessel rack surface by micro-arc oxidation is prepared the method for composite ceramic film, it is characterized in that, the method comprises the following steps:
Above-mentioned magnesium alloy blood vessel rack surface by micro-arc oxidation is prepared the method for composite ceramic film, it is characterized in that, zirconium-containing compound described in step 1 is ammonium fluozirconate, zirconium hydroxide, zirconium carbonate, zirconium carbonate ammonium, acetic acid zirconium or zirconium silicate.
Above-mentioned magnesium alloy blood vessel rack surface by micro-arc oxidation is prepared the method for composite ceramic film, it is characterized in that, pulse-repetition described in step 2 is 500Hz～800Hz.
Above-mentioned magnesium alloy blood vessel rack surface by micro-arc oxidation is prepared the method for composite ceramic film, it is characterized in that, described pulse-repetition is 650Hz.
Above-mentioned magnesium alloy blood vessel rack surface by micro-arc oxidation is prepared the method for composite ceramic film, it is characterized in that, dutycycle described in step 2 is 20%～30%.
Above-mentioned magnesium alloy blood vessel rack surface by micro-arc oxidation is prepared the method for composite ceramic film, it is characterized in that, described dutycycle is 25%.
Above-mentioned magnesium alloy blood vessel rack surface by micro-arc oxidation is prepared the method for composite ceramic film, it is characterized in that, voltage described in step 2 is 350V.
Above-mentioned magnesium alloy blood vessel rack surface by micro-arc oxidation is prepared the method for composite ceramic film, it is characterized in that, the time of the processing of differential arc oxidation described in step 2 is 8min.
Above-mentioned magnesium alloy blood vessel rack surface by micro-arc oxidation is prepared the method for composite ceramic film, it is characterized in that, the distance between magnesium alloy blood vessel rack described in step 2 and stainless steel plate is 10cm.
The present invention compared with prior art has the following advantages:
1, adopt electrolytic solution of the present invention and preparation technology parameter, can obtain even, the fine and close composite ceramic film of one deck for intraluminal magnesium alloy blood vessel rack surface fast, this composite ceramic film is mainly by MgF
2mg
2zr
5o
12, t-ZrO
2with MgO phase composite, its speed of growth is up to 1.5 μ m/min～3.0 μ m/min, the present invention has efficiently, energy-conservation advantage, in this composite ceramic film, the micrometer grade hole of equally distributed 1 μ m～2 μ m can directly be transported to medicine intraluminal lesions position as carrier simultaneously, utilize surface coverage to have the magnesium alloy blood vessel rack of composite ceramic film to have simply as endoluminal stent material, fast, feature reliably, the composite ceramic film of preparation is not in the time carrying out sealing of hole aftertreatment, resistance to neutral NaCl salt air corrosion reaches 500h, the environmental corrosion of resistance to simulated body fluid reaches 2400h, fracture toughness property obviously improves.
2, the present invention is 8～12 Zr that zirconium-containing compound is ionized out in electrolytic solution by regulating electrolytic solution pH
4+and generate Zr (OH) with the OH-combination in electrolytic solution
4colloidal solid, introducing Nanosized Zirconia Powders increases the zirconium content in electrolytic solution, adds ammonium citrate and regulates Nanosized Zirconia Powders and Zr (OH)
4the charged state of colloidal solid and dispersion situation, make zirconium dioxide powder and Zr (OH)
4colloidal solid is uniformly distributed in electrolytic solution in differential arc oxidation treating processes, and can react by the mobile differential arc oxidation that participates in anode magnesium alloy blood vessel rack surface under electric field action, Nanosized Zirconia Powders participates in differential arc oxidation reaction has increased the content of zirconium dioxide in composite ceramic film, reduce the micropore size in composite ceramic film, improve the solidity to corrosion of composite ceramic film, in addition, in electrolytic solution, add ceric ammonium nitrate to introduce cerium ion, cerium ion participates in differential arc oxidation reaction can generate cerium oxide, cerium oxide can stabilize to zirconium dioxide tetragonal structure zirconium dioxide (t-ZrO
2), and the normal temperature fracture toughness property of tetragonal structure zirconia ceramic film is better than Cubic zirconium dioxide (m-ZrO
2) ceramic membrane and other ceramic membranes, can improve the fracture toughness property of composite ceramic film, the composite ceramic film that therefore prepared by the present invention has good toughness, for by implanting after magnesium alloy blood vessel rack compressive set, provide in tube chamber may.
3, in the present invention, reach more than 4 months the work-ing life of electrolytic solution, owing to not containing high valence chrome etc. in electrolytic solution environment is produced the metal ion of severe contamination, in addition electrolytic solution long service life, therefore electrolytic solution of the present invention has advantages of long-acting, environmental protection, and composite ceramics rete is not containing toxic substance, harmless.
4, the material of microarc oxidation treatment process of the present invention to magnesium alloy blood vessel rack, size are all without particular requirement, every magnesium alloy blood vessel rack being immersed in electrolytic solution, after processing by differential arc oxidation, all can obtain even, fine and close composite ceramic film on its surface, therefore microarc oxidation treatment process of the present invention has good versatility.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the schematic appearance of magnesium alloy blood vessel rack after differential arc oxidation of the present invention is processed.
Fig. 2 is the schematic appearance of magnesium alloy blood vessel rack shown in Fig. 1 after by compression.
Fig. 3 is the surface picture through the embodiment of the present invention 1 differential arc oxidation magnesium alloy blood vessel rack after treatment.
Fig. 4 corrodes the surface picture after 500h without the magnesium alloy blood vessel rack of differential arc oxidation processing in neutral NaCl salt fog.
Fig. 5 corrodes the surface picture after 500h through the embodiment of the present invention 1 differential arc oxidation magnesium alloy blood vessel rack after treatment in neutral NaCl salt fog.
Fig. 6 corrodes the surface picture after 2400h without the magnesium alloy blood vessel rack of differential arc oxidation processing in simulated body fluid environment.
Fig. 7 corrodes the surface picture after 2400h through the embodiment of the present invention 1 differential arc oxidation magnesium alloy blood vessel rack after treatment in simulated body fluid environment.
Fig. 8 is the SEM photo through the embodiment of the present invention 1 differential arc oxidation magnesium alloy blood vessel rack surface recombination after treatment ceramic membrane.
Fig. 9 is the XRD figure spectrum through the embodiment of the present invention 1 differential arc oxidation magnesium alloy blood vessel rack surface recombination after treatment ceramic membrane.
Description of reference numerals:
1-internal layer composite ceramic film; 2-outer composite ceramic film; 3-magnesium alloy blood vessel rack;
Embodiment
The present embodiment comprises the following steps:
Fig. 1 is the schematic appearance of magnesium alloy blood vessel rack 3 after differential arc oxidation of the present invention is processed.After differential arc oxidation is processed as seen from Figure 1, the internal surface of magnesium alloy blood vessel rack 3 and outside surface grown respectively one deck internal layer composite ceramic film 1 and outer composite ceramic film 2; Fig. 2 is the schematic appearance of magnesium alloy blood vessel rack shown in Fig. 1 after by compression; Fig. 3 is the surface picture through the embodiment of the present invention 1 differential arc oxidation magnesium alloy blood vessel rack after treatment, disappears as can be seen from Figure 3 through the metalluster on the present embodiment differential arc oxidation magnesium alloy blood vessel rack after treatment surface, and ceramic membrane color and luster is even; Fig. 4 corrodes the surface picture after 500h without the magnesium alloy blood vessel rack of differential arc oxidation processing in neutral NaCl salt fog, without the magnesium alloy blood vessel rack of differential arc oxidation processing, serious corrosion occurring as seen from Figure 4, there is a large amount of corrosion dells and linen corrosion product in surface; Fig. 5 corrodes the surface picture after 500h through the embodiment of the present invention 1 differential arc oxidation magnesium alloy blood vessel rack after treatment in neutral NaCl salt fog, the ceramic coating formed by micro-arc oxidation that the present embodiment differential arc oxidation is processed rear magnesium alloy blood vessel rack surface is as seen from Figure 5 compared with (Fig. 3) before corrosion, without considerable change, do not find obvious signs of corrosion; Fig. 6 corrodes the surface picture after 2400h without the magnesium alloy blood vessel rack of differential arc oxidation processing in simulated body fluid environment, as can be seen from Figure 6 without the magnesium alloy blood vessel rack generation heavy corrosion of differential arc oxidation processing, surface produces a large amount of grey black corrosion pits, and is attended by the generation of macro-corrosion product; Fig. 7 corrodes the surface picture after 2400h through the embodiment of the present invention 1 differential arc oxidation magnesium alloy blood vessel rack after treatment in simulated body fluid environment, as seen from Figure 7 through the ceramic coating formed by micro-arc oxidation on the present embodiment differential arc oxidation magnesium alloy blood vessel rack after treatment surface compared with (Fig. 3) before corrosion, there is a small amount of small pit in surface, but do not find heavy corrosion sign, this shows that the erosion resistance of herbal classic embodiment differential arc oxidation magnesium alloy blood vessel rack after treatment in simulated body fluid environment increases substantially.
Fig. 8 is the SEM photo through the embodiment of the present invention 1 differential arc oxidation magnesium alloy blood vessel rack surface recombination after treatment ceramic membrane, in the composite ceramics rete on the present embodiment differential arc oxidation magnesium alloy blood vessel rack after treatment surface, be uniform-distribution with as seen from Figure 8 the micrometer grade hole of 1 a large amount of μ m～2 μ m, these micropores can directly be transported to medicine intraluminal lesions position as carrier.
Fig. 9 is the XRD figure spectrum through the embodiment of the present invention 1 differential arc oxidation magnesium alloy blood vessel rack surface recombination after treatment ceramic membrane, and Analysis of X RD collection of illustrative plates shows that this composite ceramic film is mainly by MgF
2, Mg
2zr
5o
12, t-ZrO
2and MgO phase composite, its speed of growth is up to 2 μ m/min.The present embodiment by introducing Zr (OH) in electrolytic solution
4colloid, nanometer ZrO
2powder and Ce
4+, in the magnesium alloy angiocarpy bracket ceramic coating formed by micro-arc oxidation that makes to prepare, contain t-ZrO
2, MgO phase, to improve solidity to corrosion and the fracture toughness property of ceramic membrane, when the magnesium alloy differential arc oxidation ceramic membrane of preparing by the present embodiment does not carry out sealing of hole aftertreatment, resistance to neutral NaCl salt air corrosion reaches 500h, the environmental corrosion of resistance to simulated body fluid reaches 2400h, and fracture toughness property obviously improves.
The present embodiment comprises the following steps:
Adopt electrolytic solution and the preparation technology parameter of the present embodiment, can obtain even, the fine and close composite ceramic film of one deck for intraluminal magnesium alloy blood vessel rack surface fast, this composite ceramic film is mainly by MgF
2, Mg
2zr
5o
12, t-ZrO
2with MgO phase composite, its speed of growth is up to 2 μ m/min, in this composite ceramic film, the micrometer grade hole of equally distributed 1 μ m～2 μ m can be as the carrier that directly medicine is transported to lesions position simultaneously, utilize magnesium alloy blood vessel rack that surface coverage has a composite ceramic film as endoluminal stent material have simply, fast, feature reliably, the composite ceramic film of preparation is not in the time carrying out sealing of hole aftertreatment, resistance to neutral NaCl salt air corrosion reaches 500h, the environmental corrosion of resistance to simulated body fluid reaches 2400h, and fracture toughness property obviously improves.
The present embodiment comprises the following steps:
Adopt electrolytic solution and the preparation technology parameter of the present embodiment, can obtain even, the fine and close composite ceramic film of one deck for intraluminal magnesium alloy blood vessel rack surface fast, this composite ceramic film is mainly by MgF
2, Mg
2zr
5o
12, t-ZrO
2with MgO phase composite, its speed of growth is up to 3 μ m/min, in this composite ceramic film, the micrometer grade hole of equally distributed 1 μ m～2 μ m can be as the carrier that directly medicine is transported to lesions position simultaneously, utilize magnesium alloy blood vessel rack that surface coverage has a composite ceramic film as endoluminal stent material have simply, fast, feature reliably, the composite ceramic film of preparation is not in the time carrying out sealing of hole aftertreatment, resistance to neutral NaCl salt air corrosion reaches 500h, the environmental corrosion of resistance to simulated body fluid reaches 2400h, and fracture toughness property obviously improves.
Embodiment 4
The present embodiment comprises the following steps:
Adopt electrolytic solution and the preparation technology parameter of the present embodiment, can obtain even, the fine and close composite ceramic film of one deck for intraluminal magnesium alloy blood vessel rack surface fast, this composite ceramic film is mainly by MgF
2, Mg
2zr
5o
12, t-ZrO
2with MgO phase composite, its speed of growth is up to 1.5 μ m/min, in this composite ceramic film, the micrometer grade hole of equally distributed 1 μ m～2 μ m can be as the carrier that directly medicine is transported to lesions position simultaneously, utilize magnesium alloy blood vessel rack that surface coverage has a composite ceramic film as endoluminal stent material have simply, fast, feature reliably, the composite ceramic film of preparation is not in the time carrying out sealing of hole aftertreatment, resistance to neutral NaCl salt air corrosion reaches 500h, the environmental corrosion of resistance to simulated body fluid reaches 2400h, and fracture toughness property obviously improves.
Embodiment 5
The present embodiment comprises the following steps:
Adopt electrolytic solution and the preparation technology parameter of the present embodiment, can obtain even, the fine and close composite ceramic film of one deck for intraluminal magnesium alloy blood vessel rack surface fast, this composite ceramic film is mainly by MgF
2, Mg
2zr
5o
12, t-ZrO
2with MgO phase composite, its speed of growth is up to 2.5 μ m/min, in this composite ceramic film, the micrometer grade hole of equally distributed 1 μ m～2 μ m can be as the carrier that directly medicine is transported to lesions position simultaneously, utilize magnesium alloy blood vessel rack that surface coverage has a composite ceramic film as endoluminal stent material have simply, fast, feature reliably, the composite ceramic film of preparation is not in the time carrying out sealing of hole aftertreatment, resistance to neutral NaCl salt air corrosion reaches 500h, the environmental corrosion of resistance to simulated body fluid reaches 2400h, and fracture toughness property obviously improves.
Embodiment 6
The present embodiment comprises the following steps:
Adopt electrolytic solution and the preparation technology parameter of the present embodiment, can obtain even, the fine and close composite ceramic film of one deck for intraluminal magnesium alloy blood vessel rack surface fast, this composite ceramic film is mainly by MgF
2, Mg
2zr
5o
12, t-ZrO
2with MgO phase composite, its speed of growth is up to 2 μ m/min, in this composite ceramic film, the micrometer grade hole of equally distributed 1 μ m～2 μ m can be as the carrier that directly medicine is transported to lesions position simultaneously, utilize magnesium alloy blood vessel rack that surface coverage has a composite ceramic film as endoluminal stent material have simply, fast, feature reliably, the composite ceramic film of preparation is not in the time carrying out sealing of hole aftertreatment, resistance to neutral NaCl salt air corrosion reaches 500h, the environmental corrosion of resistance to simulated body fluid reaches 2400h, and fracture toughness property obviously improves.
Embodiment 7
The present embodiment comprises the following steps:
Adopt electrolytic solution and the preparation technology parameter of the present embodiment, can obtain even, the fine and close composite ceramic film of one deck for intraluminal magnesium alloy blood vessel rack surface fast, this composite ceramic film is mainly by MgF
2, Mg
2zr
5o
12, t-ZrO
2with MgO phase composite, its speed of growth is up to 2.5 μ m/min, in this composite ceramic film, the micrometer grade hole of equally distributed 1 μ m～2 μ m can be as the carrier that directly medicine is transported to lesions position simultaneously, utilize magnesium alloy blood vessel rack that surface coverage has a composite ceramic film as endoluminal stent material have simply, fast, feature reliably, the composite ceramic film of preparation is not in the time carrying out sealing of hole aftertreatment, resistance to neutral NaCl salt air corrosion reaches 500h, the environmental corrosion of resistance to simulated body fluid reaches 2400h, and fracture toughness property obviously improves.
The above; it is only preferred embodiment of the present invention; not the present invention is imposed any restrictions, every any simple modification of above embodiment being done according to the technology of the present invention essence, change and equivalent structure change, and all still belong in the protection domain of technical solution of the present invention.
Claims (9)
1. magnesium alloy blood vessel rack surface by micro-arc oxidation is prepared a method for composite ceramic film, it is characterized in that, the method comprises the following steps:
Step 1, take deionized water as solvent preparation electrolytic solution, regulating the pH of electrolytic solution is 8～12, then by electrolytic solution supersound process 2h～5h; Every liter of electrolytic solution comprises zirconium-containing compound 10g～20g, trisodium phosphate 10g～15g, tertiary sodium phosphate 8g～15g, ammonium citrate 2g～5g, Nanosized Zirconia Powders 5g～10g, ceric ammonium nitrate 2g～5g;
Step 2, electrolytic solution after pending magnesium alloy blood vessel rack is placed in step 1 supersound process are as anode, using stainless steel plate as negative electrode, surface is coated with to the Stainless Steel Wire of insulating plastics film as auxiliary cathode, the temperature of controlling electrolytic solution is 20 ℃～50 ℃, regulating the pulse-repetition of mao power source is 300Hz～1000Hz, dutycycle is 10%～40%, voltage is 300V～400V, magnesium alloy blood vessel rack constant voltage differential arc oxidation is processed to 5min～10min, at the uniform composite ceramic film of magnesium alloy blood vessel rack surface in situ growth one deck; Distance between described magnesium alloy blood vessel rack and stainless steel plate is 9cm～12cm, and described mao power source is direct current pulse power source.
2. the method for preparing composite ceramic film according to magnesium alloy blood vessel rack surface by micro-arc oxidation claimed in claim 1, is characterized in that, zirconium-containing compound described in step 1 is ammonium fluozirconate, zirconium hydroxide, zirconium carbonate, zirconium carbonate ammonium, acetic acid zirconium or zirconium silicate.
3. the method for preparing composite ceramic film according to magnesium alloy blood vessel rack surface by micro-arc oxidation claimed in claim 1, is characterized in that, pulse-repetition described in step 2 is 500Hz～800Hz.
4. the method for preparing composite ceramic film according to magnesium alloy blood vessel rack surface by micro-arc oxidation claimed in claim 3, is characterized in that, described pulse-repetition is 650Hz.
5. the method for preparing composite ceramic film according to magnesium alloy blood vessel rack surface by micro-arc oxidation claimed in claim 1, is characterized in that, dutycycle described in step 2 is 20%～30%.
6. the method for preparing composite ceramic film according to magnesium alloy blood vessel rack surface by micro-arc oxidation claimed in claim 5, is characterized in that, described dutycycle is 25%.
7. the method for preparing composite ceramic film according to magnesium alloy blood vessel rack surface by micro-arc oxidation claimed in claim 1, is characterized in that, voltage described in step 2 is 350V.
8. the method for preparing composite ceramic film according to magnesium alloy blood vessel rack surface by micro-arc oxidation claimed in claim 1, is characterized in that, the time of the processing of differential arc oxidation described in step 2 is 8min.
9. the method for preparing composite ceramic film according to magnesium alloy blood vessel rack surface by micro-arc oxidation claimed in claim 1, is characterized in that, the distance between magnesium alloy blood vessel rack described in step 2 and stainless steel plate is 10cm.
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| CN106702458A (en) * | 2015-08-19 | 2017-05-24 | 宁波瑞隆表面技术有限公司 | Electrolyte for preparing titanium alloy micro-arc oxidation ceramic film layer with high emissivity, and method |
| CN105923751A (en) * | 2016-05-13 | 2016-09-07 | 长安大学 | Ceramic membrane and membrane aeration biologic reactor provided with same |
| CN106521601A (en) * | 2016-11-22 | 2017-03-22 | 佳木斯大学 | Preparation method for micro-arc oxidation-dopamine coupling carried traditional Chinese medicine coating of pure titanium oral implant |
| CN106521603A (en) * | 2016-11-22 | 2017-03-22 | 佳木斯大学 | Preparation method of medical pure magnesium surface coupling load inducing bone growth traditional Chinese medicine coating |
| CN106676608A (en) * | 2016-11-22 | 2017-05-17 | 佳木斯大学 | Preparation method of medical pure magnesium surface electrophoretic deposition carried bone growth inducing traditional Chinese medicine coating |
| CN106521603B (en) * | 2016-11-22 | 2018-06-26 | 佳木斯大学 | A kind of medical pure magnesium surface coupling carries the preparation method of medicine coating in induction of bone growth |
| CN109082691A (en) * | 2018-08-16 | 2018-12-25 | 张家港市汇鼎新材料科技有限公司 | A kind of preparation method of wear-resistant nanometer zirconium oxide ceramic coating |
| CN110241453A (en) * | 2019-04-25 | 2019-09-17 | 西南大学 | A kind of release fluoride and the degradable kirsite bone nail of cerium and preparation method thereof |
| CN110552043A (en) * | 2019-09-26 | 2019-12-10 | 长安大学 | high-corrosion-resistance magnesium alloy hub surface treatment method |
| CN110552043B (en) * | 2019-09-26 | 2022-02-22 | 长安大学 | High-corrosion-resistance magnesium alloy hub surface treatment method |
| CN112899754A (en) * | 2021-01-27 | 2021-06-04 | 太原科技大学 | Electrolyte for preparing self-sealing hole micro-arc oxidation coating on surface of magnesium alloy and preparation method of coating |
| CN113668043A (en) * | 2021-08-19 | 2021-11-19 | 重庆大学 | Hard alloy loudspeaker box mesh enclosure and processing method thereof |
| CN113668043B (en) * | 2021-08-19 | 2024-02-27 | 重庆大学 | Hard alloy loudspeaker screen and processing method thereof |
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