CN109234784A - A kind of preparation method of medical magnesium alloy composite material - Google Patents
A kind of preparation method of medical magnesium alloy composite material Download PDFInfo
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- CN109234784A CN109234784A CN201811323613.3A CN201811323613A CN109234784A CN 109234784 A CN109234784 A CN 109234784A CN 201811323613 A CN201811323613 A CN 201811323613A CN 109234784 A CN109234784 A CN 109234784A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
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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
- C25D11/30—Anodisation of magnesium or alloys based thereon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2202/00—Metallic substrate
- B05D2202/20—Metallic substrate based on light metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2508/00—Polyesters
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- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a kind of preparation methods of medical magnesium alloy composite material, comprising steps of successively being polished Mg alloy surface, being polished and micro-arc oxidation treatment, it is then immersed in the NaOH boiling solution that pH is 10~12, after 15~20h of isothermal reaction, is rinsed well with deionized water；The PLLA that molecular weight is 40~450,000 is weighed, is dissolved in chloroform, the solution that mass fraction is 3~5% is made into, it is dry complete to solvent volatilization coated on the Mg alloy surface after aforementioned processing.Invention increases the binding forces of coating and magnesium alloy, improve film corrosion resistance, and gained composite material of magnesium alloy will not discharge hydrogen in degradation process, not only overcome the defect of the prior art, but also simple process, are suitble to heavy industrialization application.
Description
Technical field
The present invention relates to medical alloy field of material technology, and in particular to a kind of preparation side of medical magnesium alloy composite material
Method.
Background technique
Magnesium alloy has good biocompatibility, density and Young's modulus and skeleton closest, and magnesium
It is minerals needed by human, plays an important role in metabolic processes, catabolite is nontoxic to the human body, can pass through body
Liquid excretes.Therefore, medical field generally acknowledges magnesium and its alloy before degradable biological medical Material Field has application well
Scape.But since degradation speed is too fast in body fluid for magnesium, it is difficult to reach scheduled service phase, lead to its answering in biomedicine
With being restricted.Therefore, the corrosion rate for reducing magnesium alloy has become a hot topic of research.
In the known method for reducing Corrosion Behaviors of Magnesium Alloys rate, simplest method is that carry out surface to it modified, such as
Electro-deposition, sol-gal process, thermal spraying, coating organic coating, powder coating, vapor deposition, ion implanting, high energy beam processing,
Nitriding and aluminising and differential arc oxidization technique etc., it is especially the widest in the application of biomedical materials field with organic coat method
It is general.In the technical solution reported at present, the coating material that can be used for Mg alloy surface coating has polylactic acid, polycaprolactone, gathers
The Biodegradable materials such as carbonic ester, can improve the corrosion resistance of magnesium alloy to a certain extent, but hydrolysate and magnesium
Alloy reaction can generate hydrogen, it is difficult to accomplish corrosion-resistant balanced with biological friendly.
Summary of the invention
In view of the above shortcomings of the prior art, the purpose of the present invention is be specifically related to a kind of medical magnesium alloy composite wood
The preparation method of material.By carrying out micro-arc oxidation treatment to the Mg alloy surface for removing removing oxide layer, then in Mg alloy surface original
Position generate magnesium hydroxide film, react it with the carboxyl in PLLA coating, improve coating compactness and its with matrix
Interface cohesion substantially increases corrosion resistance, and gained composite material of magnesium alloy exists on the basis of guaranteeing biocompatibility
Hydrogen will not be discharged in degradation process.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of medical magnesium alloy composite material, comprising steps of
S1, it successively polished Mg alloy surface, polished and micro-arc oxidation treatment；
S2, the NaOH solution that pH is 10~12 is prepared, is heated to boiling, then immerse step S1 treated magnesium alloy
Wherein, it after 15~20h of isothermal reaction, takes out, is rinsed well with deionized water, dry up moisture；
S3, the PLLA that molecular weight is 40~450,000 is weighed, is dissolved in chloroform, be made into the solution that mass fraction is 3~5%,
It is dry complete to solvent volatilization coated in step S2 treated Mg alloy surface.
Preferably, the technological parameter of the differential arc oxidation is as follows: electrolyte is 10~15g/L of potassium hydroxide, sodium metasilicate 10
~15g/L, 4~6g/L of potassium fluoride, pulse voltage are 300~350V, 30~35min of time.
Preferably, in the step S3, coating method is spraying.
Preferably, after step S3 processing, thickness of dry film is 15~20 μm.
Preferably, it is described polishing successively with 200 mesh, 360 mesh, 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1500 mesh sand
Paper carries out.
Preferably, polishing process is electrobrightening.
Preferably, polishing fluid is phosphoric acid/ethanol solution that volume ratio is 5:1, and polishing voltage is 3~5V, polishing temperature
Degree is -5~-20 DEG C.
Existing research shows that differential arc oxidization technique can prepare porous magnesia in the Mg alloy surface for removing removing oxide layer
Layer.Further the magnesium alloy containing the magnesium oxide layer is immersed in the NaOH solution of boiling, makes magnesia that hydro-thermal reaction occur,
Magnesium hydroxide is generated, and magnesium hydroxide can be reacted with the carboxyl in PLLA coating, generate magnesium salts and water, and material is avoided to degrade
Hydrogen is discharged in journey, the surface hole defect of simultaneous oxidation magnesium layer is conducive to increase the interface cohesion of follow-up coating and magnesium alloy, significantly
Improve the surface corrosion resistance energy of magnesium alloy.
Beneficial effects of the present invention:
By carrying out micro-arc oxidation treatment to the Mg alloy surface for removing removing oxide layer, porous magnesium oxide layer is obtained, then
It is immersed in the NaOH solution of boiling, in Mg alloy surface in-situ preparation magnesium hydroxide film, utilizes the porous knot of magnesium oxide layer
Structure and magnesium hydroxide are reacted with the carboxyl in PLLA coating, improve the compactness of coating and its interface cohesion with matrix,
On the basis of guaranteeing biocompatibility, corrosion resistance is substantially increased, and gained composite material of magnesium alloy is in degradation process
Hydrogen will not be discharged, the application requirement of biological medicine material can be met well.Present invention process is simple, is suitble to large-scale industry
Change application, is conducive to the application for pushing magnesium alloy in field of medical materials.
Specific embodiment
Below by specific embodiment, the present invention will be described in detail.
The present invention first carries out oxide layer and micro-arc oxidation treatment to magnesium alloy, is then immersed in the NaOH that pH is 10~12 and boils
It rises in solution, after 15~20h of isothermal reaction, is rinsed well with deionized water, the PLLA/ chlorine that re-coating mass fraction is 3~5%
Solution is imitated, the composite material of magnesium alloy of corrosion resistance excellent can be obtained after removal solvent chloroform.
Since the chemical property of magnesium is active, very thin magnesium oxide layer can be formed on surface, the oxide layer quality is loose, corrosion resistant
Corrosion is bad, and the surface that will affect the later period is modified, it is therefore desirable to remove before modification.Minimizing technology can be mechanical grinding
Or chemical method, to reduce the corrosion to magnesium alloy, currently preferred mode is sand paper grinding and buffing, preferred mode
It is successively to carry out electrolysis throwing with after the sand paper polishing of 200 mesh, 360 mesh, 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1500 mesh
Light, polishing fluid can be phosphoric acid/ethanol solution of volume ratio 5:1, and polishing voltage can be 3~5V, and polish temperature can be with
It is -5~-20 DEG C.
Differential arc oxidation is grown up on the basis of anodic oxidation, and electrochemical reaction and plasma chemical reaction are passed through
Form micro-arc oxidation films.Existing research shows that the consistency, surface quality and thickness of micro-arc oxidation films will affect the property of film layer
Energy, such as film layer are finer and close, and hardness and corrosion resistance are better.And differential arc oxidation of the invention is a kind of intermediate treatment technology, in addition to
Other than the property for considering micro-arc oxidation films, it is also contemplated that the applicability of follow-up hydrothermal reaction, such as when film layer is excessively fine and close, instead
And it is unfavorable for the progress of hydro-thermal reaction, it will have a direct impact on the adhesive force of PLLA coating, be unfavorable for the raising of corrosion resistance.It is based on
Above-mentioned design, inventors have found that optimal micro-arc oxidation process are as follows: electrolyte be 10~15g/L of potassium hydroxide, sodium metasilicate 10~
4~6g/L of 15g/L and potassium fluoride, pulse voltage are 300~350V, 30~35min of time.
To guarantee there is a certain amount of carboxyl in PLLA molecule, and guaranteeing corrosion resistance, the molecular weight of PLLA is preferably 40~
450000.The coating method of PLLA solution preferably sprays, and preferred thickness of dry film is 15~20 μm, therefore more using that can use
The method of secondary spraying guarantees the uniformity of film.
Embodiment 1
1, the sand paper of 200 mesh, 360 mesh, 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1500 mesh magnesium alloy is successively used to beat
After mill, electrobrightening is carried out, polishing fluid is phosphoric acid/ethanol solution that volume ratio is 5:1, and polishing voltage is 5V, polishing temperature
Degree is -10 DEG C, after polishing, cleans surface with alcohol；
2, micro-arc oxidation treatment is carried out, electrolyte is potassium hydroxide 10g/L, sodium metasilicate 10g/L, potassium fluoride 4g/L, pulse
Voltage is 300V, time 35min；
3, the NaOH solution that pH is 10 is prepared, is heated to boiling, then by step 1, treated that magnesium alloy is immersed,
It after isothermal reaction 20h, takes out, is rinsed well with deionized water, dry up moisture；
4, the PLLA that molecular weight is 450,000 is weighed, is dissolved in chloroform, the solution that mass fraction is 3% is made into, at step 3
The magnesium alloy surface spraying solution after reason is volatilized completely with heated-air drying to solvent, and spraying-drying behaviour is then repeated
Make, until coating thickness is 15 μm, obtains composite material of magnesium alloy.
Embodiment 2
1, the sand paper of 200 mesh, 360 mesh, 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1500 mesh magnesium alloy is successively used to beat
After mill, electrobrightening is carried out, polishing fluid is phosphoric acid/ethanol solution that volume ratio is 5:1, and polishing voltage is 4V, polishing temperature
Degree is -5 DEG C, after polishing, cleans surface with alcohol；
2, micro-arc oxidation treatment is carried out, electrolyte is potassium hydroxide 13g/L, sodium metasilicate 12g/L, potassium fluoride 5g/L, pulse
Voltage is 320V, time 35min；
3, the NaOH solution that pH is 12 is prepared, is heated to boiling, then by step 1, treated that magnesium alloy is immersed,
It after isothermal reaction 15h, takes out, is rinsed well with deionized water, dry up moisture；
4, the PLLA that molecular weight is 450,000 is weighed, is dissolved in chloroform, the solution that mass fraction is 3% is made into, at step 3
The magnesium alloy surface spraying solution after reason is volatilized completely with heated-air drying to solvent, and spraying-drying behaviour is then repeated
Make, until coating thickness is 15 μm, obtains composite material of magnesium alloy.
Embodiment 3
1, the sand paper of 200 mesh, 360 mesh, 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1500 mesh magnesium alloy is successively used to beat
After mill, electrobrightening is carried out, polishing fluid is phosphoric acid/ethanol solution that volume ratio is 5:1, and polishing voltage is 5V, polishing temperature
Degree is -15 DEG C, after polishing, cleans surface with alcohol；
2, micro-arc oxidation treatment is carried out, electrolyte is potassium hydroxide 13g/L, sodium metasilicate 15g/L, potassium fluoride 5g/L, pulse
Voltage is 350V, time 30min；
3, the NaOH solution that pH is 10 is prepared, is heated to boiling, then by step 1, treated that magnesium alloy is immersed,
It after isothermal reaction 20h, takes out, is rinsed well with deionized water, dry up moisture；
4, the PLLA that molecular weight is 400,000 is weighed, is dissolved in chloroform, the solution that mass fraction is 4% is made into, at step 3
The magnesium alloy surface spraying solution after reason is volatilized completely with heated-air drying to solvent, and spraying-drying behaviour is then repeated
Make, until coating thickness is 15 μm, obtains composite material of magnesium alloy.
Comparative example 1
Compared with Example 1, the PLLA molecular weight is 600,000.
Comparative example 2
Compared with Example 1, the PLLA molecular weight is 300,000.
Comparative example 3
Compared with Example 1, using the electrolyte of aluminates system.
Test case
Surface corrosion resistance for magnesium alloy after testing example and comparative example processing.
Test method are as follows: the sample of embodiment 1-3 and comparative example 1-3 are separately immersed in simulated body fluid, after impregnating 5 days
Coating surface state is observed, test result is as shown in table 1.
Table 1
It can be seen from the above result that composite material of magnesium alloy surface corrosion resistance performance of the invention is preferable, especially PLLA molecule
Amount and electrolyte type selecting have a significant impact.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
Claims (7)
1. a kind of preparation method of medical magnesium alloy composite material, which is characterized in that comprising steps of
S1, it successively polished Mg alloy surface, polished and micro-arc oxidation treatment；
S2, the NaOH solution that pH is 10~12 is prepared, is heated to boiling, then treated that magnesium alloy immerses it by step S1
In, it after 15~20h of isothermal reaction, takes out, is rinsed well with deionized water, dry up moisture；
S3, the PLLA that molecular weight is 40~450,000 is weighed, be dissolved in chloroform, be made into the solution that mass fraction is 3~5%, coating
It is dry complete to solvent volatilization in step S2 treated Mg alloy surface.
2. the preparation method of medical magnesium alloy composite material according to claim 1, which is characterized in that the work of differential arc oxidation
Skill parameter is as follows: electrolyte is 10~15g/L of potassium hydroxide, 10~15g/L of sodium metasilicate, 4~6g/L of potassium fluoride, and pulse voltage is
300~350V, 30~35min of time.
3. the preparation method of medical magnesium alloy composite material according to claim 1 or 2, which is characterized in that the step
In S3, coating method is spraying.
4. the preparation method of medical magnesium alloy composite material according to claim 3, which is characterized in that handled through step S3
Afterwards, thickness of dry film is 15~20 μm.
5. the preparation method of medical magnesium alloy composite material according to claim 1 or 2, which is characterized in that polishing is successively
It is carried out with the sand paper of 200 mesh, 360 mesh, 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1500 mesh.
6. the preparation method of medical magnesium alloy composite material according to claim 1 or 2, which is characterized in that polishing process
For electrobrightening.
7. the preparation method of medical magnesium alloy composite material according to claim 6, which is characterized in that polishing fluid is volume
Than phosphoric acid/ethanol solution for 5:1, polishing voltage is 3~5V, and polish temperature is -5~-20 DEG C.
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| CN201811323613.3A CN109234784A (en) | 2018-11-08 | 2018-11-08 | A kind of preparation method of medical magnesium alloy composite material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109881238A (en) * | 2019-03-21 | 2019-06-14 | 西安交通大学 | Magnesium-based surface has the active coating and preparation method thereof of self-healing function |
| CN114892238A (en) * | 2022-04-02 | 2022-08-12 | 西安交通大学 | Method for improving corrosion resistance of magnesium alloy micro-arc oxidation film layer by pretreatment process |
| CN114990667A (en) * | 2022-07-14 | 2022-09-02 | 哈尔滨工程大学 | Method for preparing super-hydrophobic composite film on surface of magnesium-lithium alloy and magnesium-lithium alloy with super-hydrophobic composite film |
| CN115708896A (en) * | 2022-11-16 | 2023-02-24 | 南京友德邦医疗科技有限公司 | Degradable magnesium alloy composite material and preparation method thereof |
-
2018
- 2018-11-08 CN CN201811323613.3A patent/CN109234784A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109881238A (en) * | 2019-03-21 | 2019-06-14 | 西安交通大学 | Magnesium-based surface has the active coating and preparation method thereof of self-healing function |
| CN114892238A (en) * | 2022-04-02 | 2022-08-12 | 西安交通大学 | Method for improving corrosion resistance of magnesium alloy micro-arc oxidation film layer by pretreatment process |
| CN114990667A (en) * | 2022-07-14 | 2022-09-02 | 哈尔滨工程大学 | Method for preparing super-hydrophobic composite film on surface of magnesium-lithium alloy and magnesium-lithium alloy with super-hydrophobic composite film |
| CN114990667B (en) * | 2022-07-14 | 2023-10-31 | 哈尔滨工程大学 | Method for preparing super-hydrophobic composite film on surface of magnesium-lithium alloy and magnesium-lithium alloy with super-hydrophobic composite film |
| CN115708896A (en) * | 2022-11-16 | 2023-02-24 | 南京友德邦医疗科技有限公司 | Degradable magnesium alloy composite material and preparation method thereof |
| CN115708896B (en) * | 2022-11-16 | 2024-03-19 | 南京友德邦医疗科技有限公司 | Degradable magnesium alloy composite material and preparation method thereof |
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