CN106757251A - A kind of preparation method of Mg alloy surface composite coating - Google Patents
A kind of preparation method of Mg alloy surface composite coating Download PDFInfo
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- CN106757251A CN106757251A CN201710036099.4A CN201710036099A CN106757251A CN 106757251 A CN106757251 A CN 106757251A CN 201710036099 A CN201710036099 A CN 201710036099A CN 106757251 A CN106757251 A CN 106757251A
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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
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
- C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
- C25D9/12—Electrolytic coating other than with metals with inorganic materials by cathodic processes 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
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
- B05D3/0466—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases the gas being a non-reacting gas
- B05D3/048—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases the gas being a non-reacting gas for cooling
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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
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/10—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by other chemical means
- B05D3/102—Pretreatment of metallic substrates
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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
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/12—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by mechanical means
-
- 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
- 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
Abstract
The invention discloses a kind of magnesium alloy materials surface modifying method, and in particular to a kind of preparation method of Mg alloy surface composite coating, it is comprised the following steps：1) pre-treatment：Magnesium alloy sample is polished, polishing, alkali cleaning, dried process；2) magnesium hydroxide coating is deposited on surface using cathodic electrodeposition method；3) organic coating is coated：PLA coating is formed in the specimen surface by electrodeposition process.In the inventive method, magnesium hydroxide coating reacts with PLA, does not produce hydrogen, and the very ingenious polylactic acid PLA that solves is applied directly to the problems such as the hydrogen release produced by Mg alloy surface；Easily there is micropore in the pore self-sealing structural improvement electro-deposition magnesium hydroxide coating that the two is formed, and porosity is high, not fine and close enough the defect of structure.Degraded in acidity in human body for PLA, change body fluid pH value, be unfavorable for the problem of the healing of wound, magnesium hydroxide plays neutralization.
Description
Technical field
The present invention provides a kind of preparation method of Mg alloy surface composite coating, is related to the technology of Magnesiumalloy surface modifying to lead
Domain.
Background technology
Magnesium and its alloy have good biocompatibility, and its density and Young's modulus are closest with skeleton, its
Catabolite is nontoxic to human body, and can be excreted by body fluid.Due to magnesium and its advantage of alloy, medical field generally acknowledge magnesium and its
Alloy is revolutionary biomedical metallic material.But its degradation speed in body fluid is too fast, with cambium around and more
Mismatched between sum velocity, cause its application in biomedicine to be restricted.Therefore, the corrosion of magnesium and its alloy is reduced
The key that speed is studied as this year, is also the hot issue of current domestic and foreign scholars research.
The method for reducing magnesium and its alloy corrosion speed is mainly divided to two major classes:One class is to magnesium by way of ion implanting
Alloy material carries out bulk modified:Another kind of is that the surface of magnesium alloy is modified by surface treatment or coating technology.
The mode of ion implanting may influence other performances of magnesium, practical application also to there is certain difficulty.Surface is modified not to be interfered with
The performance of magnesium, and process, it is simple to operate, it is easy to accomplish.
Preparation method about magnesium and coating of magnesium alloy surface is a lot, and the modified method in surface is usually used at present chemistry
Plating, chemical oxygen (turning) change, sol-gal process, surface electrodeposited coating, thermal spraying, organic coating and powder coating, vapour deposition,
Diffusion alloying, ion implanting, high energy beam treatment, nitriding and aluminising, consonance coating technology and differential arc oxidization technique etc..But
Used as biological and medicinal implant material, its coating must assure that non-toxic, good biocompatibility, and degradability to magnesium, this
Existing surface treatment method is limited in magnesium alloy as the application on implantation material.Electro-deposition techniques and organic coating method
Because process is simple, operation are easy, Environmental security, equipment investment is few, and the mode of production flexibly, obtains relatively broad application.And
In the technical scheme of current report, polylactic acid PLA organic coating directly such as is coated in Mg alloy surface, and utilize electro-deposition
Method is obtained magnesium hydroxide coating in Mg alloy surface, and the decay resistance of magnesium alloy is improve to a certain extent, but generally
There are problems that it is many, for example：Easily there is micropore and cracking phenomena, porosity is high, it is impossible to which pore self-sealing, structure is not fine and close enough, hydrolyze
The problems such as product produces hydrogen gas with magnesium alloy substrate reaction.
The content of the invention
Technical problem：It is an object of the invention to provide a kind of preparation method of Mg alloy surface composite coating, for control
Magnesium alloy is degraded too fast problem in human body, reduces the corrosion rate of magnesium and its alloy, and then improve the biofacies of magnesium alloy
Capacitive.
Technical scheme：In order to achieve the above object, the main technical schemes that the present invention is used include:
1) pre-treatment：Magnesium alloy sample is polished with the sand paper of 240,400,600,800,1500 mesh, polishing gets well it
After be processed by shot blasting, be polished to Mg alloy surface and minute surface and no marking be presented, then alkali cleaning is carried out to Mg alloy surface, dry at
Reason, removes grease and polishing compound；
2) magnesium hydroxide coating is deposited on surface using cathodic electrodeposition method：Weigh magnesium nitrate hexahydrate, be dissolved in from
In sub- water, 0.1-0.2mol/L MgNO are prepared3Solution；Using magnesium alloy as negative electrode, platinum electrode enters as anode to magnesium alloy
Row constant potential electrodeposition process, as shown in Figure 1；Voltage is 4-6V, electro-deposition duration 1.5-2.5h；Take out, clean, dry
Preserve；
3) organic coating is coated：PLA is weighed, dichloromethane is dissolved in, lasting stirring, compound concentration is the solution of 4-6wt%
500ml；To repeatedly be immersed in PLA solution by the sample of electrodeposition process and lifted, dried, the immersion time is 20-
40s；It is cool to room temperature after drying 7-15min at 70-90 DEG C；Sample is taken out and hung to the sealing of the precooling equipped with dry ice and is held
In device, vacuumize, and container is placed in 10-15h in 50~60 DEG C of hothouses, make solvent evaporating completely.
Beneficial effect：
(1) to use polylactic acid PLA to be applied directly to Mg alloy surface corrosion-resistant to improve magnesium alloy for conventional technique scheme
Performance, slows down the corrosion rate of magnesium alloy, but hydrolyzes easily generation acidity-COOH in the solution due to PLA, is produced with magnesium matrix
Following reaction：
Mg+-COOH→-(COO)2Mg+H2,
Produced H2Bubble, stomata is formed in PLA coat insides, can reduce coating and magnesium matrix binding ability.The present invention
Magnesium hydroxide intermediate layer, magnesium hydroxide coating and PLA are introduced between magnesium alloy substrate and PLA coatings using negative electrode deposition process
Reaction, does not produce hydrogen, very ingenious to solve the problem that foregoing hydrogen release band is come.
Secondly, there is following reaction between magnesium hydroxide coating and PLA organic coatings：
Mg(OH)2+-COOH→-(COO)2Mg+H2O
Wherein ,-(COO)2Mg is glue, is attached on Mg (OH)2Porous surface, makes Mg (OH)2Coating is tight with PLA coatings
With reference to, composite coating is formed, the two forms self-styled pore structure, reduces its surface micropore porosity, and micropore diminishes, is effectively improved
Mg(OH)2The loose porous shortcoming of coating.PLA degrades in acidity in human body, changes body fluid pH value, is unfavorable for healing for wound
Close, magnesium hydroxide plays neutralization.
(2) magnesium hydroxide is mutually the intermediate product that magnesium metal is degraded in human body, nontoxic to human body, used as magnesium alloy coating
Composition is present, and is applied to have with inherent advantage in human body as medical material for magnesium alloy.
Brief description of the drawings
Fig. 1 is the preparation method and technology flow chart of Mg alloy surface composite coating of the present invention.
Specific embodiment
In order to preferably explain the present invention, in order to understand, below by specific embodiment, present invention work is retouched in detail
State.
Embodiment 1
This example Mg alloy surface preparation method of composite coating includes following process:
(1) pre-treatment, step is as follows：
The material for test on this example institute side is AZ31 magnesium alloys, and the content of wherein magnesium is up to more than 95%.Test specimen is main
Element constituent is as shown in table 1.
| Al | Zn | Mn | Si | Cu | Ni | Fe | Mg |
| 3.1 | 0.8 | 0.15 | 0.06 | 0.03 | 0.02 | 0.01 | Surplus |
Table 1 AZ31 magnesium alloy essential element nominal composition (mass fraction) %
The present embodiment from 60mm × 14mm × 2mm AZ31 magnesium alloys, respectively successively with 240,400,600,800,
The sand paper of 1500 mesh is polished, and is carried out at the polishing of Mg alloy surface with PG2A types metallographic-sample polisher after polishing is good
Reason, is polished to Mg alloy surface and minute surface and no marking is presented.Alkali cleaning is carried out to Mg alloy surface again, dried process removes grease
And polishing compound.
(2) magnesium hydroxide coating is deposited on surface using cathodic electrodeposition method：
Electro-deposition method prepares hydroxide film layer, is to carry out negative electrode electro-deposition in solution of the pH value less than 7, solution
Reducing agent (such as H2O, NO3Deng) reduced in electrode surface first, form OH-；Then, the metal ion or complex compound in solution with
Adsorb the OH in electrode surface-React, generate metal hydroxides.
Experimental power supply selects WYK-300 types dc source (production of Yangzhou Jin Tong electric corporation) in the present embodiment.
Prepare comprising the following steps that for magnesium hydroxide coating：
1. 6.410g magnesium nitrate hexahydrates are weighed with electronic balance to be dissolved in deionized water, is stirred, until completely molten
Solution, configuration 0.1mol/L MgNO3Solution 250ml；
2. two section leads are intercepted, magnesium plate is connected as anode as negative electrode, platinum electrode with power supply, two electrode runs parallels are relative,
In the setting-out at the 5cm of magnesium plate border, it is ensured that the area of magnesium plate immersion solution is 50mm × 14mm；
3. voltage source is opened：
4. supply voltage is adjusted to 5V；
5. by power-off after electro-deposition duration 2h, the magnesium alloy that taking-up is prepared is taken out, and cleaning, drying is preserved.
(3) organic coating is coated, step is as follows:
1. PLA 25g are weighed with electronic balance, is dissolved in dichloromethane, lasting stirring, compound concentration is the solution of 5wt%
500ml；
2. by by the sample of electrodeposition process immersion PLA solution 30s；Lifting, it is cool to room after drying 10min at 75 DEG C
Temperature；
3. 2. step is repeated several times by different needs, Mg alloy surface is formed the PLA organic coatings of half solidification；
4. sample is taken out and is placed in air；
5. sample is hung into the sealing container of the precooling equipped with dry ice, is vacuumized；
6. container is placed in 10h in 55 DEG C of hothouses, makes solvent evaporating completely.
Embodiment 2
This example Mg alloy surface preparation method of composite coating includes following process：
(1) pre-treatment, step is as follows：
The material for test on this example institute side is AZ31 magnesium alloys, with embodiment 1；
The present embodiment from 60mm × 14mm × 2mm AZ31 magnesium alloys, respectively successively with 240,400,600,800,
The sand paper of 1500 mesh is polished, and is carried out at the polishing of Mg alloy surface with PG2A types metallographic-sample polisher after polishing is good
Reason, is polished to Mg alloy surface and minute surface and no marking is presented.Alkali cleaning is carried out to Mg alloy surface again, dried process removes grease
And polishing compound.
(2) magnesium hydroxide coating is deposited on surface using cathodic electrodeposition method：
Experimental power supply selects WYK-300 types dc source (production of Yangzhou Jin Tong electric corporation) in the present embodiment.
Prepare comprising the following steps that for magnesium hydroxide coating：
1. 9.615g magnesium nitrate hexahydrates are weighed with electronic balance to be dissolved in deionized water, is stirred, until completely molten
Solution, configuration 0.15mol/L MgNO3Solution 250ml；
2. two section leads are intercepted, magnesium plate is connected as anode as negative electrode, platinum electrode with power supply, two electrode runs parallels are relative,
In the setting-out at the 5cm of magnesium plate border, it is ensured that the area of magnesium plate immersion solution is 50mm × 14mm；
3. voltage source is opened：
4. supply voltage is adjusted to 5.5V；
5. by power-off after electro-deposition duration 1.5h, the magnesium alloy that taking-up is prepared is taken out, and cleaning, drying is protected
Deposit.
(3) organic coating is coated, step is as follows:
1. PLA 30g are weighed with electronic balance, is dissolved in dichloromethane, lasting stirring, compound concentration is the solution of 5wt%
500ml；
2. by by the sample of electrodeposition process immersion PLA solution 40s；Lifting, it is cool to room after drying 12min at 85 DEG C
Temperature；
3. 2. step is repeated several times by different needs, Mg alloy surface is formed the PLA organic coatings of half solidification；
4. sample is taken out and is placed in air；
5. sample is hung into the sealing container of the precooling equipped with dry ice, is vacuumized；
6. container is placed in 12h in 60 DEG C of hothouses, makes solvent evaporating completely.
Above-described embodiment is technology design and feature to illustrate the invention, its object is to allow people to will appreciate that this
The content of invention is simultaneously implemented according to this, and it is not intended to limit the scope of the present invention.It is all according to main technical schemes of the present invention
The equivalent transformation that is done of Spirit Essence or modification, should all be included within the scope of the present invention.
Claims (1)
1. a kind of preparation method of Mg alloy surface composite coating, it is characterised in that：The composite coating with magnesium alloy as matrix,
Respectively through being prepared after pre-treatment, negative electrode electro-deposition treatment, to have thickness be 5-50 μm of magnesium hydroxide coating on its surface, then with carrying
Daraf(reciprocal of farad) coats PLA organic coating in magnesium hydroxide coating surface, and its preparation comprises the following steps：
1）Pre-treatment：Magnesium alloy sample is polished with the sand paper of 240,400,600,800,1500 mesh, after polishing is good
It is processed by shot blasting, is polished to Mg alloy surface and minute surface and no marking is presented, then alkali cleaning is carried out to Mg alloy surface, at drying
Reason, removes grease and polishing compound；
2）Magnesium hydroxide coating is deposited in Mg alloy surface using cathodic electrodeposition method：Magnesium nitrate hexahydrate is weighed, is dissolved in
In ionized water, 0.1-0.2mol/L MgNO are prepared3Solution；Using magnesium alloy as negative electrode, platinum electrode as anode, to magnesium alloy
Carry out constant potential electrodeposition process；Voltage is 4-6V, electro-deposition duration 1.5-2.5h；Take out, clean, drying is preserved；
3）Coating organic coating：PLA is weighed, dichloromethane is dissolved in, lasting stirring, compound concentration is the PLA solution of 4-6wt%
500ml；To repeatedly be immersed in PLA solution by the sample of electrodeposition process and lifted, dried, the immersion time is 20-
40s；It is cool to room temperature after drying 7-15min at 70-90 DEG C；Sample is taken out and hung to the sealing of the precooling equipped with dry ice and is held
In device, vacuumize, and container is placed in 10-15h in 50 ~ 60 DEG C of hothouses, make solvent evaporating completely.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108660494A (en) * | 2018-03-23 | 2018-10-16 | 郑州大学 | The polymer compound film layer and preparation process of a kind of magnesium and Mg alloy surface Covalent bonding together |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108660494A (en) * | 2018-03-23 | 2018-10-16 | 郑州大学 | The polymer compound film layer and preparation process of a kind of magnesium and Mg alloy surface Covalent bonding together |
| CN108660494B (en) * | 2018-03-23 | 2020-04-24 | 郑州大学 | Macromolecular composite film layer with covalent bond combination on surface of magnesium and magnesium alloy and preparation process thereof |
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Application publication date: 20170531 |