CN102787339A - Method for preparing magnesium alloy - calcium phosphorus coating composite material by electrochemical deposition - Google Patents
Method for preparing magnesium alloy - calcium phosphorus coating composite material by electrochemical deposition Download PDFInfo
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- CN102787339A CN102787339A CN2012102666501A CN201210266650A CN102787339A CN 102787339 A CN102787339 A CN 102787339A CN 2012102666501 A CN2012102666501 A CN 2012102666501A CN 201210266650 A CN201210266650 A CN 201210266650A CN 102787339 A CN102787339 A CN 102787339A
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- electrochemical deposition
- magnesiumalloy
- matrix material
- phosphor coating
- magnesium alloy
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Abstract
The invention relates to a method for preparing a magnesium alloy - calcium phosphorus coating composite material by electrochemical deposition. The method comprises the steps of preprocessing a magnesium alloy matrix, preparing an electrolyte solution, electrochemically depositing and the like, and then the magnesium alloy - calcium phosphorus coating composite material is obtained. The test on the electrochemical corrosion performance of the magnesium alloy - calcium phosphorus coating composite material prepared in the electrochemical deposition method proves that the corrosion potential of the composite material is higher than that of a magnesium matrix and the corrosion current of the composite material smaller than that of the magnesium matrix, so that the corrosion resistance of the composite material is better. Compared with the prior art, the magnesium alloy - calcium phosphorus coating composite material obtained by preparing a calcium phosphorus coating on the surface of a magnesium alloy matrix in the electrochemical deposition method is improved in coating uniformity and corrosion resistance, no residual stress exists in the coating, and the calcium phosphorus coating can be deposited on the surface of an inhomogeneous matrix.
Description
Technical field
The present invention relates to the method that a kind of electrochemical deposition prepares magnesiumalloy-calcium phosphor coating matrix material.
Background technology
The researchdevelopment of biomaterial and Materials science development in modern age are closely related.Based on the importance of biomaterial, bio-medical material becomes one of important research field of materialogy.At present, traditional single type bio-medical material all has application like metallic substance, stupalith, macromolecular material etc., but as bone alternate material, its limitation is arranged all in organism.
Calcium phosphate is paid close attention to by people with its superior biocompatibility and biological activity.Inorganic components in it and human body bone, the tooth is approaching, can induce new bone to grow after the implantation, makes material obtain good biological activity, thereby makes implant combine well with biological tissue.The research of multiple biological ceramics and bio-vitric coating all has report, and wherein the research of Win 40350 (HA) coating is maximum.From then on, the composite medical material has got into people's the visual field.
The research of metal-base composites mainly concentrates in the research to metal surface modification, after coatings such as metal material surface coating calcium phosphate, obtains good anti-corrosion and biocompatibility.At present, in the biomaterial Application Areas, the surface treatment method that improves the Mg alloy surface performance is mainly contained: plasma spraying method, differential arc oxidation, organic coating, calcium phosphate coating etc.Plasma spraying method exists residual interfacial stress, and coating is inhomogeneous, and cost is crossed problems such as height; Micro-arc oxidation process also exists the homogeneity of rete, compactness undesirable; Arc oxidation ceramic layer fragility is big, and energy consumption is bigger in the production process, the electrolytic solution cooling difficulty; Subsequent disposal is cumbersome, also sintering energy undue concentration might take place and produces burning or matrix ablation phenomen etc.The bonding force of polymer organic coating and metallic matrix is relatively poor, when organic coating inadequately evenly or with matrix bond when relatively poor, matrix metal is easy to take place filiform corrosion.
Electrochemical deposition method has incomparable meliority as a kind of coating production: the coating through this method obtains is comparatively fine and close, and high with high base strength; The preparation process is carried out under mild conditions, and is simple to operation; Electrochemical process is a non-linear process, can on the magnesium matrix of complex-shaped and porous surface, prepare uniform calcium phosphor coating.
Summary of the invention
Shortcoming in view of above-mentioned prior art the purpose of this invention is to provide the method that a kind of electrochemical deposition prepares magnesiumalloy calcium phosphor coating matrix material, and magnesiumalloy-calcium phosphor coating matrix material that this method obtains has better erosion resistance and biocompatibility.
For realizing above-mentioned purpose and other relevant purposes, the present invention adopts following technical scheme:
A kind of electrochemical deposition prepares the method for magnesiumalloy-calcium phosphor coating matrix material, comprises the steps:
1) pre-treatment: the magnesium alloy substrate of getting suitable size is polished to the non-oxidation layer; Adopt the polishing of aluminum oxide water-proof abrasive paper then successively, adopt the SiC liquid honing; With the magnesium alloy substrate that obtains ultrasonic cleaning in acetone successively, ultrasonic cleaning and in zero(ppm) water, cleaning in alcohol; Dry, subsequent use then; In electrochemical deposition process, the state of matrix surface is bigger to the coating performance influence that makes, so the pre-treatment of matrix is essential.
Preferable, in the step 1), adopt No. 220 sand paper when polishing magnesium alloy substrate to the non-oxidation layer; Employed aluminum oxide water-proof abrasive paper is 800 order aluminum oxide water-proof abrasive papers; The SiC waterproof abrasive paper that is adopted is No. 2000 SiC waterproof abrasive paper.
Preferable, in the step 1), the time of ultrasonic cleaning is 20-40 minute in acetone; The time of ultrasonic cleaning is 20-40 minute in alcohol.
2) configuration electrolyte solution: the configuration aqueous electrolyte liquid, and the pH value of regulator solution is 3.8 ~ 4.3, temperature is 20 ~ 60 ℃; Ca (the NO that contains 0.09-0.11M in the electrolyte solution that is wherein disposed
3)
24H
2The NH of O, 0.058-0.062M
4H
2PO
3, 15-20mL/L 30%H
2O
2Above-mentioned steps 2) 30%H in
2O
2Be meant H
2O
2Volumn concentration.
3) electrochemical deposition: as anode, pretreated magnesium alloy substrate adopts outside D.C. regulated power supply to supply power as negative electrode with graphite, behind electrochemical deposition, obtains said magnesiumalloy-calcium phosphor coating matrix material; Wherein, the voltage of electrochemical deposition is 3.8-4.2V, and electric current is 1 ~ 2mA, and the electrochemical deposition time is 1-2h;
Adopt electrochemical deposition method of the present invention can make magnesiumalloy-calcium phosphor coating matrix material; And this magnesiumalloy-calcium phosphor coating matrix material carried out the test of electrochemical corrosion performance; Can know that this matrix material compares with magnesium matrix; Its corrosion potential is higher than the corrosion potential of magnesium matrix, and corrosion current is littler than the corrosion current of magnesium matrix, explains that the corrosion resistance nature of this matrix material is better.
Compared with prior art; The present invention utilizes electrochemical deposition method to prepare the calcium phosphor coating at magnesium alloy matrix surface; The magnesiumalloy that is obtained-calcium phosphor coating matrix material; The homogeneity of its coating and corrosion resistance nature all have lifting, and do not have unrelieved stress in the coating, can be at non-homogeneous matrix surface deposition calcium phosphor coating.
Embodiment
Below through specific specific examples embodiment of the present invention is described, those skilled in the art can understand other advantages of the present invention and effect easily by the content that this specification sheets disclosed.The present invention can also implement or use through other different embodiment, and each item details in this specification sheets also can be based on different viewpoints and application, carries out various modifications or change under the spirit of the present invention not deviating from.
The method of following steps is adopted in the pre-treatment of the alloy substrate among following examples 1-5: the magnesium alloy substrate of getting moderate size is at first polished to the non-oxidation layer on No. 220 sand paper; On 800 order aluminum oxide water-proof abrasive papers, polish then, on No. 2000 SiC waterproof abrasive paper, polish again; With the magnesium alloy substrate that obtains in acetone ultrasonic cleaning 20-40 minute, in the alcohol ultrasonic cleaning 20-40 minute, zero(ppm) water cleaned, and drying is subsequent use; In electrochemical deposition process, the state of matrix surface is bigger to the coating performance influence that makes, so the pre-treatment of matrix is essential.
Embodiment 1
Configuration 150mL contains 0.1M Ca (NO
3)
24H2O, 0.06M NH
4H
2PO
3, 30%H
2O
215mL/L, the pH value is 4 electrolyte solution, the magnesium alloy substrate of 10mm * 10mm that pre-treatment is good is as negative electrode; Graphite is as anode, at the electric current of 1 ~ 2mA, under the voltage of 4V; Deposit 2h in 20 ℃ of environment of water-bath, can obtain magnesiumalloy-calcium phosphor coating matrix material.
Magnesiumalloy-calcium phosphor coating composite sample that present embodiment is obtained carries out the galvanic corrosion test, and the corrosion potential of this sample is-1.329V that corrosion current is 3.391e
-7(corrosion potential of magnesium matrix is-1.531V that corrosion current is 1.768e to A
-4A).
The magnesiumalloy of present embodiment-calcium phosphor coating matrix material is compared with the magnesium matrix material, and its corrosion potential is higher than the corrosion potential of magnesium matrix, and corrosion current is littler than the corrosion current of magnesium matrix, explains that the corrosion resistance nature of this magnesiumalloy-calcium phosphor coating matrix material is better.Because corrosion potential is high more, corrosion current is more little, and its erosion resistance is good more.
The standard of the galvanic corrosion test of adopting adopts three-electrode method, and SCE is a reference electrode, and the Pt electrode is a supporting electrode, and specimen is a working electrode, in 37 ℃ bionical body fluid, tests electrochemical data.
Embodiment 2
Configuration 150mL contains 0.1M Ca (NO
3)
24H2O, 0.06M NH
4H
2PO
3, 30%H
2O
215mL/L, the pH value is 4 electrolyte solution, the magnesium alloy substrate of 10mm * 10mm that pre-treatment is good is as negative electrode; Graphite is as anode, at the electric current of 1 ~ 2mA, under the voltage of 4V; Deposit 2h in 30 ℃ of environment of water-bath, can obtain magnesiumalloy calcium phosphor coating matrix material.
Magnesiumalloy-calcium phosphor coating composite sample that present embodiment is obtained carries out the galvanic corrosion test, and the corrosion potential of this sample is-1.420V that corrosion current is 6.258e
-7(corrosion potential of magnesium matrix is-1.531V that corrosion current is 1.768e to A
-4A).
The magnesiumalloy of present embodiment-calcium phosphor coating matrix material is compared with the magnesium matrix material, and its corrosion potential is higher than the corrosion potential of magnesium matrix, and corrosion current is littler than the corrosion current of magnesium matrix, explains that the corrosion resistance nature of this magnesiumalloy-calcium phosphor coating matrix material is better.Because corrosion potential is high more, corrosion current is more little, and its erosion resistance is good more.
Embodiment 3
Configuration 150mL contains 0.1M Ca (NO
3)
24H2O, 0.06M NH
4H
2PO
3, 30%H
2O
215mL/L, the pH value is 4 electrolyte solution, the magnesium alloy substrate of 10mm * 10mm that pre-treatment is good is as negative electrode; Graphite is as anode, at the electric current of 1 ~ 2mA, under the voltage of 4V; Deposit 2h in 40 ℃ of environment of water-bath, can obtain magnesiumalloy-calcium phosphor coating matrix material.
Magnesiumalloy-calcium phosphor coating composite sample that present embodiment is obtained carries out the galvanic corrosion test, and the corrosion potential of this sample is-1.393V that corrosion current is 3.466e
-7(corrosion potential of magnesium matrix is-1.531V that corrosion current is 1.768e to A
-4A).
The magnesiumalloy of present embodiment-calcium phosphor coating matrix material is compared with the magnesium matrix material, and its corrosion potential is higher than the corrosion potential of magnesium matrix, and corrosion current is littler than the corrosion current of magnesium matrix, explains that the corrosion resistance nature of this magnesiumalloy-calcium phosphor coating matrix material is better.Because corrosion potential is high more, corrosion current is more little, and its erosion resistance is good more.
Embodiment 4
Configuration 150mL contains 0.1M Ca (NO
3)
24H2O, 0.06M NH
4H
2PO
3, 30%H
2O
215mL/L, the pH value is 4 electrolyte solution, the magnesium alloy substrate of 10mm * 10mm that pre-treatment is good is as negative electrode; Graphite is as anode, at the electric current of 1 ~ 2mA, under the voltage of 4V; Deposit 2h in 50 ℃ of environment of water-bath, can obtain magnesiumalloy calcium phosphor coating matrix material.
Magnesiumalloy-calcium phosphor coating composite sample that present embodiment is obtained carries out the galvanic corrosion test, and the corrosion potential of this sample is-1.410V that corrosion current is 5.346e
-7(corrosion potential of magnesium matrix is-1.531V that corrosion current is 1.768e to A
-4A).
The magnesiumalloy of present embodiment-calcium phosphor coating matrix material is compared with the magnesium matrix material, and its corrosion potential is higher than the corrosion potential of magnesium matrix, and corrosion current is littler than the corrosion current of magnesium matrix, explains that the corrosion resistance nature of this magnesiumalloy-calcium phosphor coating matrix material is better.Because corrosion potential is high more, corrosion current is more little, and its erosion resistance is good more.
Embodiment 5
Configuration 150mL contains 0.1M Ca (NO
3)
24H2O, 0.06MNH
4H
2PO
3, 30%H
2O
215mL/L, the pH value is 4 electrolyte solution, the magnesium alloy substrate of 10mm * 10mm that pre-treatment is good is as negative electrode; Graphite is as anode, at the electric current of 1 ~ 2mA, under the voltage of 4V; Deposit 2h in 60 ℃ of environment of water-bath, can obtain magnesiumalloy calcium phosphor coating matrix material.
Magnesiumalloy-calcium phosphor coating composite sample that present embodiment is obtained carries out the galvanic corrosion test, and the corrosion potential of this sample is-1.376V that corrosion current is 1.664e
-6(corrosion potential of magnesium matrix is-1.531V that corrosion current is 1.768e to A
-4A).
The magnesiumalloy of present embodiment-calcium phosphor coating matrix material is compared with the magnesium matrix material, and its corrosion potential is higher than the corrosion potential of magnesium matrix, and corrosion current is littler than the corrosion current of magnesium matrix, explains that the corrosion resistance nature of this magnesiumalloy-calcium phosphor coating matrix material is better.Because corrosion potential is high more, corrosion current is more little, and its erosion resistance is good more.
Embodiment 6
Configuration 150mL contains 0.09M Ca (NO
3)
24H2O, 0.062MNH
4H
2PO
3, 30%H
2O
218mL/L, the pH value is 4.3 electrolyte solution, the magnesium alloy substrate of 10mm * 10mm that pre-treatment is good is as negative electrode; Graphite is as anode, at the electric current of 1 ~ 2mA, under the voltage of 4.2V; Deposit 1.5h in 20 ℃ of environment of water-bath, can obtain magnesiumalloy-calcium phosphor coating matrix material.
After testing; The magnesium alloy of present embodiment-calcium phosphor coating composite is compared with the magnesium matrix material; Its corrosion potential is higher than the corrosion potential of magnesium matrix, and corrosion current is littler than the corrosion current of magnesium matrix, illustrates that the decay resistance of this magnesium alloy-calcium phosphor coating composite is better.Because corrosion potential is high more, corrosion current is more little, and its erosion resistance is good more.
Embodiment 7
Configuration 150mL contains 0.11M Ca (NO
3)
24H2O, 0.058M NH
4H
2PO
3, 30%H
2O
220mL/L, the pH value is 3.8 electrolyte solution, the magnesium alloy substrate of 10mm * 10mm that pre-treatment is good is as negative electrode; Graphite is as anode, at the electric current of 1 ~ 2mA, under the voltage of 3.8V; Deposit 2h in 20 ℃ of environment of water-bath, can obtain magnesiumalloy-calcium phosphor coating matrix material.
After testing; The magnesium alloy of present embodiment-calcium phosphor coating composite is compared with the magnesium matrix material; Its corrosion potential is higher than the corrosion potential of magnesium matrix, and corrosion current is littler than the corrosion current of magnesium matrix, illustrates that the decay resistance of this magnesium alloy-calcium phosphor coating composite is better.Because corrosion potential is high more, corrosion current is more little, and its erosion resistance is good more.
The above; Being merely preferred embodiment of the present invention, is not to any formal and substantial restriction of the present invention, should be understood that; For those skilled in the art; Under the prerequisite that does not break away from the inventive method, also can make some improvement and replenish, these improvement and replenish and also should be regarded as protection scope of the present invention.Allly be familiar with the professional and technical personnel, under the situation that does not break away from the spirit and scope of the present invention, the technology contents that is disclosed more than capable of using and a little change of making, modify the equivalent variations with differentiation, be equivalent embodiment of the present invention; Simultaneously, the change of any equivalent variations that all foundations essence technology of the present invention is done the foregoing description, modify and differentiation, all still belong in the scope of technical scheme of the present invention.
Claims (7)
1. an electrochemical deposition prepares the method for magnesiumalloy-calcium phosphor coating matrix material, comprises the steps:
1), pre-treatment: the magnesium alloy substrate of getting suitable size is polished to the non-oxidation layer; Adopt the polishing of aluminum oxide water-proof abrasive paper then successively, adopt the SiC liquid honing; With the magnesium alloy substrate that obtains ultrasonic cleaning in acetone successively, ultrasonic cleaning and in zero(ppm) water, cleaning in alcohol; Dry, subsequent use then;
2), the configuration electrolyte solution: configuration aqueous electrolyte liquid, and the pH value of regulator solution is 3.8 ~ 4.3, temperature is 20 ~ 60 ℃; Ca (the NO that contains 0.09-0.11M in the electrolyte solution that is wherein disposed
3)
24H
2The NH of O, 0.058-0.062M
4H
2PO
3, 15-20mL/L 30%H
2O
2
3), electrochemical deposition: as anode, pretreated magnesium alloy substrate adopts outside D.C. regulated power supply to supply power as negative electrode with graphite, behind electrochemical deposition, obtains said magnesiumalloy-calcium phosphor coating matrix material.
2. electrochemical deposition as claimed in claim 1 prepares the method for magnesiumalloy-calcium phosphor coating matrix material, it is characterized in that, in the step 3), the voltage of electrochemical deposition is 3.8-4.2V, and electric current is 1 ~ 2mA, and the electrochemical deposition time is 1-2h.
3. electrochemical deposition as claimed in claim 1 prepares the method for magnesiumalloy-calcium phosphor coating matrix material, it is characterized in that, in the step 1), adopts No. 220 sand paper when polishing magnesium alloy substrate to the non-oxidation layer.
4. electrochemical deposition as claimed in claim 1 prepares the method for magnesiumalloy-calcium phosphor coating matrix material, it is characterized in that, in the step 1), employed aluminum oxide water-proof abrasive paper is 800 order aluminum oxide water-proof abrasive papers.
5. electrochemical deposition as claimed in claim 1 prepares the method for magnesiumalloy-calcium phosphor coating matrix material, it is characterized in that, in the step 1), the SiC waterproof abrasive paper that is adopted is No. 2000 SiC waterproof abrasive paper.
6. electrochemical deposition as claimed in claim 1 prepares the method for magnesiumalloy-calcium phosphor coating matrix material, it is characterized in that, in the step 1), the time of ultrasonic cleaning is 20-40 minute in acetone; The time of ultrasonic cleaning is 20-40 minute in alcohol.
7. magnesiumalloy-calcium phosphor coating matrix material is for the method that adopts the arbitrary described electrochemical deposition of claim 1-6 to prepare magnesiumalloy-calcium phosphor coating matrix material makes.
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Cited By (1)
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Application publication date: 20121121 |