CN107460524B - Differential arc oxidation prepares the solution formula and technique of magnesium and the Mg alloy surface coating containing tantalum - Google Patents
Differential arc oxidation prepares the solution formula and technique of magnesium and the Mg alloy surface coating containing tantalum Download PDFInfo
- Publication number
- CN107460524B CN107460524B CN201710713489.0A CN201710713489A CN107460524B CN 107460524 B CN107460524 B CN 107460524B CN 201710713489 A CN201710713489 A CN 201710713489A CN 107460524 B CN107460524 B CN 107460524B
- Authority
- CN
- China
- Prior art keywords
- solution
- magnesium
- tantalum
- containing tantalum
- cathode
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000011248 coating agent Substances 0.000 title claims abstract description 52
- 238000000576 coating method Methods 0.000 title claims abstract description 52
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 39
- 239000011777 magnesium Substances 0.000 title claims abstract description 37
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 36
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 30
- 230000003647 oxidation Effects 0.000 title claims abstract description 20
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 claims abstract description 25
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 16
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 235000019795 sodium metasilicate Nutrition 0.000 claims abstract description 11
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 11
- JVOQKOIQWNPOMI-UHFFFAOYSA-N ethanol;tantalum Chemical compound [Ta].CCO JVOQKOIQWNPOMI-UHFFFAOYSA-N 0.000 claims abstract description 10
- OSYUGTCJVMTNTO-UHFFFAOYSA-D oxalate;tantalum(5+) Chemical group [Ta+5].[Ta+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O OSYUGTCJVMTNTO-UHFFFAOYSA-D 0.000 claims abstract description 7
- 239000010935 stainless steel Substances 0.000 claims abstract description 7
- 244000137852 Petrea volubilis Species 0.000 claims abstract description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 239000008213 purified water Substances 0.000 claims description 4
- 229910052909 inorganic silicate Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 claims 1
- 238000009434 installation Methods 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 10
- 230000007797 corrosion Effects 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000005498 polishing Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 239000007769 metal material Substances 0.000 abstract description 2
- 230000000087 stabilizing effect Effects 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 12
- 229960000935 dehydrated alcohol Drugs 0.000 description 7
- 239000000956 alloy Substances 0.000 description 6
- 210000000988 bone and bone Anatomy 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 230000000278 osteoconductive effect Effects 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000012620 biological material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 230000035876 healing Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 150000002739 metals Chemical group 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 230000000399 orthopedic effect Effects 0.000 description 2
- 230000002000 scavenging effect Effects 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- 229910001948 sodium oxide Inorganic materials 0.000 description 2
- 210000001519 tissue Anatomy 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 108010048734 sclerotin Proteins 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910001256 stainless steel alloy Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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
- C25D11/026—Anodisation with spark discharge
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
- Materials For Medical Uses (AREA)
Abstract
The invention belongs to metal material surface field of engineering technology, and in particular to differential arc oxidation prepares the solution formula and technique of magnesium and the Mg alloy surface coating containing tantalum.The invention discloses solution formulas, and including sodium metasilicate, tertiary sodium phosphate, sodium hydroxide, ethanol tantalum, water, the ethanol tantalum in formula can be replaced with tantalum oxalate, and water is solvent.The invention also discloses the preparation processes of coating: sample is cleaned with sand paper polishing, cold water wash, acetone oil removing, EtOH Sonicate, then solution is prepared, sample is connect with microarc oxidation equipment provided anode again, stainless steel substrates are cathode, cathode, anode are put into prepared solution, cooling and agitating solution, start it is microarc oxidation equipment provided, coating preparation complete close it is microarc oxidation equipment provided, unload sample, cleaning, drying.Gained coating binding force is good, even tissue, can improve the corrosion resistance of magnesium and magnesium alloy and improve its biocompatibility.Equipment needed for prepares coating of the present invention is simple, and process stabilizing is reliable, easy to realize.
Description
Technical field
The invention belongs to metal material surface field of engineering technology, and in particular to differential arc oxidation prepares magnesium and Mg alloy surface
The solution formula and technique of the coating containing tantalum.
Background technique
Traditional biological material based on stainless steel and titanium alloy plays the development of implantation material fixed in modern orthopaedics
Great effect.But traditional orthopedic implanting material generates stress shielding after implanting and hinders union；After union
Second operation is needed to take out；The problems such as after taking out refracture easily occurs for material promotes people to find possible substitute.Using magnesium as base
The biomaterial of matter is due to good metallic character, mechanical property and degradability (absorption of human body is not necessarily to second operation)
As the hot spot studied now, and very likely become new orthopedic implanting material.But magnesium-based material corrosion resistance is low, in bone
Matter loses mechanical property because of corrosion before not healing, therefore, how while improving with the corrosion resistance of magnesium-based material again
It can guarantee the biomechanics characteristic and biocompatibility of magnesium-based material, this is the hot spot studied at this stage.In it is mainly studied
Have: (1) magnesium and other one or more metals form alloy.Common metallic element has manganese, zinc, aluminium, calcium and rare earth element
Deng.The purer magnesium material of magnesium alloy materials corrosion resistance after synthesis is greatly improved, but as biological implantable material,
Its bio-compatible sex expression is unsatisfactory.(2) another common method is to carry out surface modification, increase on magnesium alloy materials surface
Surface covering or surface protection film.Existing result of study shows that tantalum element has more good biofacies compared with magnesium, titanium elements
Capacitive, while coating containing tantalum has good osteoconductive and bone-inducing activity.
Currently, still belonging to blank in the technology of preparing of magnesium alloy surface micro-arc preparation coating containing tantalum and its application.Therefore it studies
Has the technology of preparing of the coating containing tantalum of biocompatibility, osteoconductive and bone-inducing activity to magnesium and magnesium with realization Mg alloy surface
The application of alloy is of great significance.
In conclusion main problem of the existing technology has: 1. magnesium-based material corrosion resistances are poor, in sclerotin
Mechanical property is lost because of corrosion before not healing；2. magnesium and other metals form the magnesium alloy materials corrosion resistance after alloy
Purer magnesium material is greatly improved, but as biological implantable material, bio-compatible sex expression is unsatisfactory.
Summary of the invention
The purpose of the present invention is aiming at the problems existing in the prior art, provide the anti-corruption that magnesium and magnesium alloy both can be improved
Corrosion energy, but the differential arc oxidation that can improve its biocompatibility prepares the solution formula and work of magnesium and the Mg alloy surface coating containing tantalum
Skill.The technique also has many advantages, such as to be simple and convenient to operate, is easily achieved, is high-efficient, is suitable for production and application.Pass through the technique
The coating binding force of acquisition is good, even tissue.
To achieve the above object, first technical solution that the present invention uses is: differential arc oxidation prepares magnesium and magnesium alloy table
The solution formula of face coating containing tantalum, which is characterized in that include: sodium metasilicate, tertiary sodium phosphate, sodium hydroxide, ethyl alcohol in solution formula
Tantalum, water.
Further, sodium metasilicate, tertiary sodium phosphate, sodium hydroxide, the concentration of ethanol tantalum are respectively silicic acid in the solution formula
Sodium: 8-10g/L, tertiary sodium phosphate: 6-8g/L, sodium hydroxide: 1-2g/L, ethanol tantalum: 5-10ml/L.
Further, sodium metasilicate, tertiary sodium phosphate, sodium hydroxide, ethanol tantalum are that analysis is pure in the solution formula, and water is to steam
Distilled water or purified water.
Second technical solution that the present invention uses is: differential arc oxidation prepares the solution of magnesium and the Mg alloy surface coating containing tantalum
Formula, which is characterized in that include: sodium metasilicate, tertiary sodium phosphate, sodium hydroxide, tantalum oxalate, water in solution formula.
Further, sodium metasilicate, tertiary sodium phosphate, sodium hydroxide, the concentration of tantalum oxalate are respectively silicic acid in the solution formula
Sodium: 8-10g/L, tertiary sodium phosphate: 6-8g/L, sodium hydroxide: 1-2g/L, tantalum oxalate: 5-10ml/L.
Further, sodium metasilicate, tertiary sodium phosphate, sodium hydroxide, tantalum oxalate are that analysis is pure in the solution formula, and water is to steam
Distilled water or purified water.
The third technical solution that the present invention uses is: differential arc oxidation prepares the work of magnesium and the Mg alloy surface coating containing tantalum
Skill, which comprises the following steps:
S1. cold water wash after magnesium and magnesium alloy sample being polished with 200#-1500# sand paper, acetone oil removing, EtOH Sonicate
Cleaning, then drying is stand-by；
S2. microarc oxidation solution is prepared, prepared solution is stirred evenly with glass bar；
S3. sample is connect with microarc oxidation equipment provided anode, uses stainless steel substrates as cathode, using the small sun of big cathode
Pole structure；
S4. the cathode connected, anode are put into prepared solution, cathode is placed in parallel with anode, spacing 2-
3cm；
S5. the cooling solution of cooling device is opened, agitating device agitating solution is opened；
S6. start it is microarc oxidation equipment provided, be arranged its operating voltage be 380-420V, duty ratio 20, power frequency 300-
500HZ, working time 30-40min；
S7. microarc oxidation equipment provided, cooling device and agitating device are closed after the completion of coating preparation；
S8. the sample after differential arc oxidation is unloaded, EtOH Sonicate cleaning, drying to get.
Further, acetone oil removing described in step S1 is that sample is put into acetone to impregnate, soaking time >=5min；It is described
EtOH Sonicate scavenging period >=5min.
Further, ethyl alcohol described in step S1 and S8 is dehydrated alcohol, wherein containing CH3CH2OH≥99.7%。
Further, the area ratio of big cathode and primary anode described in step S3 are as follows: cathode plane Ji ︰ annode area >=2 ︰ 1.
Further, solution is cooled to 20-30 DEG C in step S5.
Further, cooling device described in step S5 and S7 is circulating water device, and the agitating device is air pump.
Further, the scavenging period of EtOH Sonicate described in step S8 >=2min.
Further, drying described in step S8 is that hair dryer or natural wind dry up.
The 4th technical solution that the present invention uses is: magnesium and the Mg alloy surface coating containing tantalum of differential arc oxidation preparation,
It is characterized in that, includes the Mg containing tantalum in the composition of the coating containing tantalum2SiO4And MgO.
Beneficial effects of the present invention:
1, the present invention solves the technical problem that magnesium and corrosion resistance of magnesium alloy can be poor；
2, the coating containing tantalum prepared by the present invention has more excellent biocompatibility, good osteoconductive and lures bone
Activity；
3, equipment needed for prepares coating of the present invention is simple, and process stabilizing is reliable, easy to realize, gained coating binding force is good,
Even tissue.
Detailed description of the invention
Fig. 1 a is the microstructure figure by the coating surface obtained containing tantalum of the embodiment of the present invention 1；
Fig. 1 b is the microstructure figure by the coating cross sections obtained containing tantalum of the embodiment of the present invention 1；
Fig. 2 a is the microstructure figure by the coating surface obtained containing tantalum of the embodiment of the present invention 2；
Fig. 2 b is the microstructure figure by the coating cross sections obtained containing tantalum of the embodiment of the present invention 2；
Fig. 3 a is the microstructure figure by the coating surface obtained containing tantalum of the embodiment of the present invention 3；
Fig. 3 b is the microstructure figure by the coating cross sections obtained containing tantalum of the embodiment of the present invention 3；
Fig. 4 is the structural schematic diagram by the coating cross sections obtained containing tantalum of the embodiment of the present invention 1；
In figure, 1 is coating, and 2 be matrix；
Fig. 5 is the process flow chart that differential arc oxidation of the present invention prepares magnesium and the Mg alloy surface coating containing tantalum.
Specific embodiment
Technical solution of the present invention is described in detail with reference to the accompanying drawing, but the contents of the present invention are not limited to
This.
Embodiment 1
Magnesium and Mg alloy surface coating containing tantalum are prepared using micro-arc oxidation.
As shown in the process flow chart of Fig. 5, the present embodiment is followed the steps below: 1. by magnesium alloy sample successively
The cold water wash after the polishing of 200#, 600#, 1200# and 1500# sand paper, acetone soak 5min oil removing, dehydrated alcohol ultrasonic cleaning
5min, then drying is stand-by；2. preparing microarc oxidation solution: wherein containing the sodium metasilicate of 8g/L, the tertiary sodium phosphate of 6g/L, 1g/L
Sodium hydroxide, the ethanol tantalum of 5ml/L, solvent is distilled water, and prepared solution is stirred evenly with glass bar；3. by sample
It is connect with microarc oxidation equipment provided anode, uses stainless steel substrates as cathode, using big cathode primary anode structure (cathode plane Ji ︰ sun
Pole-face accumulates >=2 ︰ 1)；4. the cathode connected, anode are put into prepared solution, cathode is placed in parallel with anode, and spacing is
2cm；5. circulating water is used, to guarantee the temperature of solution in experimentation for 20 DEG C；Solution is stirred using air pump
It mixes；6. starting is microarc oxidation equipment provided, it is 380V, duty ratio 20, power frequency 300HZ, working time that its operating voltage, which is arranged,
30min；7. closing microarc oxidation equipment provided, circulating water cooling device and air pump agitating device after the completion of coating preparation；8. will
Sample after differential arc oxidation unloads, dehydrated alcohol be cleaned by ultrasonic 2min, hair dryer drying to get.
Fig. 1 a and Fig. 1 b are shown in by the microstructure figure that embodiment 1 obtains coating surface containing tantalum and section respectively.
As shown in figure 4, by the obtained coating containing tantalum on magnesium alloy matrix of embodiment 1, wherein the master of coating containing tantalum
It will be by the Mg containing tantalum2SiO4It is formed with MgO, electronic probe component analysis is shown, the chemical component of the coating are as follows: 52.07O-
29.26Mg-2.42Al-6.68Si-9.57Ta at.% realizes the preparation of Mg alloy surface coating containing tantalum, and entire coating matter
Amount is good.
Embodiment 2
Magnesium and Mg alloy surface coating containing tantalum are prepared using micro-arc oxidation.
As shown in the process flow chart of Fig. 5, the present embodiment is followed the steps below: 1. successively pass through magnesium alloy sample
Cold water wash after the polishing of 200#, 600#, 1200# and 1500# sand paper, acetone soak 5min oil removing, dehydrated alcohol ultrasonic cleaning
10min, then drying is stand-by；2. preparing microarc oxidation solution: the sodium metasilicate of 9g/L, the tertiary sodium phosphate of 7g/L, the hydrogen of 1.5g/L
Sodium oxide molybdena, the ethanol tantalum of 7.5ml/L, solvent are distilled water, and prepared solution is stirred evenly with glass bar；3. by sample with
Microarc oxidation equipment provided anode connection, uses stainless steel substrates as cathode, using big cathode primary anode structure (cathode plane Ji ︰ anode
Area >=2 ︰ 1)；4. the cathode connected, anode are put into prepared solution, cathode is placed in parallel with anode, and spacing is
2.5cm；5. circulating water is used, to guarantee the temperature of solution in experimentation for 25 DEG C；Air pump is used in experimentation
Solution is stirred；6. starting is microarc oxidation equipment provided, it is 400V, duty ratio 20, power frequency that its operating voltage, which is arranged,
400HZ, working time 35min；7. closing microarc oxidation equipment provided, circulating water cooling device and air pump after the completion of coating preparation
Agitating device；8. the sample after differential arc oxidation is unloaded, dehydrated alcohol is cleaned by ultrasonic 2.5min, natural wind drying to get.
Fig. 2 a and Fig. 2 b are shown in by the microstructure figure that embodiment 2 obtains coating surface containing tantalum and section respectively.
Embodiment 3
Magnesium and Mg alloy surface coating containing tantalum are prepared using micro-arc oxidation.
As shown in the process flow chart of Fig. 5, the present embodiment is followed the steps below: 1. successively pass through magnesium alloy sample
Cold water wash after the polishing of 200#, 600#, 1200# and 1500# sand paper, acetone soak 5min oil removing, dehydrated alcohol ultrasonic cleaning
10min, then drying is stand-by；2. preparing microarc oxidation solution: the sodium metasilicate of 10g/L, the tertiary sodium phosphate of 8g/L, the hydrogen of 2g/L
Sodium oxide molybdena, the ethanol tantalum of 10ml/L, solvent are distilled water, and prepared solution is stirred evenly with glass bar；3. by sample with it is micro-
The anode of arc oxidation furnaces connects, and uses stainless steel substrates as cathode, using big cathode primary anode structure (cathode plane Ji ︰ anode surface
>=2 ︰ 1 of product)；4. the cathode connected, anode are put into prepared solution, cathode is placed in parallel with anode, spacing 3cm；
5. circulating water is used, to guarantee the temperature of solution in experimentation for 25 DEG C；Using air pump to solution in experimentation
It is stirred；6. starting is microarc oxidation equipment provided, it is 420V, duty ratio 20, power frequency 500HZ, work that its operating voltage, which is arranged,
Make time 40min；7. closing microarc oxidation equipment provided, circulating water cooling device and air pump agitating device after the completion of coating preparation；
8. the sample after differential arc oxidation is unloaded, dehydrated alcohol is cleaned by ultrasonic 3min, natural wind drying to get.
Fig. 3 a and Fig. 3 b are shown in by the microstructure figure that embodiment 3 obtains coating surface containing tantalum and section respectively.
The above is only presently preferred embodiments of the present invention, the interest field being not intended to limit the invention.It is any with this
The technical solution or anyone skilled in the art that the interest field that claim is covered is implemented utilize
The method content of the disclosure above makes the scheme of many possible changes and modifications, all belongs to the scope of protection of the present invention.
Claims (4)
1. the solution that differential arc oxidation prepares magnesium and the Mg alloy surface coating containing tantalum, which is characterized in that include: silicic acid in solution formula
Sodium: 8-10g/L, tertiary sodium phosphate: 6-8g/L, sodium hydroxide: 1-2g/L, ethanol tantalum: 5-10ml/L；The sodium metasilicate, tricresyl phosphate
Sodium, sodium hydroxide, ethanol tantalum are that analysis is pure, and water is distilled water or purified water.
2. the solution that differential arc oxidation prepares magnesium and the Mg alloy surface coating containing tantalum, which is characterized in that include: silicic acid in solution formula
Sodium: 8-10g/L, tertiary sodium phosphate: 6-8g/L, sodium hydroxide: 1-2g/L, tantalum oxalate: 5-10ml/L；Silicic acid in the solution formula
Sodium, tertiary sodium phosphate, sodium hydroxide, tantalum oxalate are that analysis is pure, and water is distilled water or purified water.
3. the technique that differential arc oxidation prepares magnesium and the Mg alloy surface coating containing tantalum, which comprises the following steps:
S1. cold water wash after magnesium and magnesium alloy sample being polished with 200#-1500# sand paper, acetone oil removing, EtOH Sonicate cleaning,
Then drying is stand-by；
S2. microarc oxidation solution is prepared with solution formula as claimed in claim 1 or 2, configured solution is stirred equal with glass bar
It is even；
S3. sample is connect with microarc oxidation equipment provided anode, uses stainless steel substrates as cathode, using big cathode primary anode knot
Structure；The area ratio of the big cathode and primary anode are as follows: cathode plane Ji ︰ annode area >=2 ︰ 1；
S4. the cathode connected, anode are put into configured solution, cathode is placed in parallel with anode, spacing 2-3cm；
S5. the cooling solution of cooling device is opened, agitating device agitating solution is opened；
S6. start it is microarc oxidation equipment provided, be arranged its operating voltage be 380-420V, duty ratio 20%, power frequency 300-
500HZ, working time 30-40min；
S7. microarc oxidation equipment provided, cooling device and agitating device are closed after the completion of coating preparation；The cooling device is circulation
Water installations, the agitating device are air pump, and the solution is cooled to 20-30 DEG C；
S8. the sample after differential arc oxidation is unloaded, EtOH Sonicate cleaning, drying to get.
4. magnesium and the Mg alloy surface coating containing tantalum of differential arc oxidation preparation, include the Mg containing tantalum in the composition of the coating containing tantalum2SiO4With
MgO, which is characterized in that the chemical component of the coating containing tantalum are as follows: 52.07O-29.26Mg-2.42Al-6.68Si-9.57Ta
at.%。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710713489.0A CN107460524B (en) | 2017-08-16 | 2017-08-16 | Differential arc oxidation prepares the solution formula and technique of magnesium and the Mg alloy surface coating containing tantalum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710713489.0A CN107460524B (en) | 2017-08-16 | 2017-08-16 | Differential arc oxidation prepares the solution formula and technique of magnesium and the Mg alloy surface coating containing tantalum |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107460524A CN107460524A (en) | 2017-12-12 |
| CN107460524B true CN107460524B (en) | 2019-08-16 |
Family
ID=60550050
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710713489.0A Active CN107460524B (en) | 2017-08-16 | 2017-08-16 | Differential arc oxidation prepares the solution formula and technique of magnesium and the Mg alloy surface coating containing tantalum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107460524B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115198331A (en) * | 2021-04-14 | 2022-10-18 | 株式会社日立制作所 | Electrolyte and micro-arc oxidation method of high-thermal-conductivity magnesium alloy |
| CN114381778B (en) * | 2021-12-20 | 2023-12-01 | 中国兵器科学研究院宁波分院 | Method for preparing tantalum biological coating on surface of magnesium and magnesium alloy |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8808522B2 (en) * | 2011-09-07 | 2014-08-19 | National Chung Hsing University | Method for forming oxide film by plasma electrolytic oxidation |
| CN103526262A (en) * | 2013-10-17 | 2014-01-22 | 赵全明 | Method for performing surface modification on tantalum and tantalum alloy and electrolyte used in method |
| CN106637352A (en) * | 2015-08-19 | 2017-05-10 | 宁波瑞隆表面技术有限公司 | Electrolytic solution and method for preparing biological activity Ca-P ceramic film on magnesium alloy surface |
-
2017
- 2017-08-16 CN CN201710713489.0A patent/CN107460524B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN107460524A (en) | 2017-12-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Chang et al. | Formation of dicalcium phosphate dihydrate on magnesium alloy by micro-arc oxidation coupled with hydrothermal treatment | |
| CN107460524B (en) | Differential arc oxidation prepares the solution formula and technique of magnesium and the Mg alloy surface coating containing tantalum | |
| CN106958014B (en) | In the method for pure magnesium surface building hybrid inorganic-organic function and service coating | |
| CN101709496B (en) | Micro-arc oxidation-electrodeposition preparation method of magnesium-based bioactive coating | |
| CN104784750B (en) | Improve the corrosion proof surface modifying method of morphotropism Biological magnesium alloy implant devices | |
| CN103643274B (en) | A kind of method and application thereof preparing graphene oxide layer by being electrodeposited in titanium surface | |
| CN101560685B (en) | Method for preparing bioactive coating on titanium alloy surface | |
| CN107142444A (en) | A kind of preparation method of the medical zircaloy of β types of surface oxidation | |
| Tao et al. | Synthesis of a porous oxide layer on a multifunctional biomedical titanium by micro-arc oxidation | |
| CN101994143A (en) | Preparation method of titanium alloy/biological ceramic layer composite material | |
| CN105696054A (en) | Preparation method for forming calcium-containing nanosheet film layer on surface of sandblasted and acid-etched titanium | |
| CN104562145A (en) | Method for preparing bioceramic membrane by composite oxidation | |
| CN103526262A (en) | Method for performing surface modification on tantalum and tantalum alloy and electrolyte used in method | |
| CN110408975A (en) | Low pressure micro-arc oxidation electrolyte, method and products thereof | |
| CN103194781A (en) | Bioactivity surface modification method used in degradable magnesium alloy | |
| CN102304746A (en) | Polypyrrole calcium phosphate/magnesium oxide bioceramic coating and preparation method thereof | |
| CN104988558A (en) | Method for preparing biological ceramic membrane layer on titanium alloy surface through graded combined oxidation in stages | |
| CN103301512B (en) | Absorbable biological material and preparation method thereof | |
| CN102389588B (en) | Magnesium or magnesium alloy material used for biological implantation and preparation method thereof | |
| CN103451640A (en) | Method for preparing degradable biomedical magnesium alloy/calcium-phosphorus coating composite material | |
| CN106075600A (en) | A kind of preparation method of medical degradable calcium phosphate coating magnesium alloy | |
| CN103272284A (en) | Biological medical controllable all-degradable material and preparation method thereof | |
| CN108930023A (en) | A kind of method that Mg alloy surface magnetron sputtering prepares tantalum biological coating | |
| CN103498184A (en) | Micro arc electrophoresis modification method of biomedical magnesium alloy | |
| CN106282975A (en) | The hydroxyapatite super-hydrophobic film layer prepared at Mg alloy surface and method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240513 Address after: No. 6 Qihang Road, West District, Guangde Economic Development Zone, Xuancheng City, Anhui Province, 242000 Patentee after: Anhui Muyi Technology Co.,Ltd. Country or region after: China Address before: 750021 No. 204, Wenchang North Street, Xixia District, the Ningxia Hui Autonomous Region, Yinchuan Patentee before: BEIFANG MINZU University Country or region before: China |
|
| TR01 | Transfer of patent right |