CN104562146A - Titanium alloy artificial articular head with wear resistant ceramic coating and preparation method of titanium alloy artificial articular head - Google Patents
Titanium alloy artificial articular head with wear resistant ceramic coating and preparation method of titanium alloy artificial articular head Download PDFInfo
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- CN104562146A CN104562146A CN201510010869.9A CN201510010869A CN104562146A CN 104562146 A CN104562146 A CN 104562146A CN 201510010869 A CN201510010869 A CN 201510010869A CN 104562146 A CN104562146 A CN 104562146A
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- abrasion
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Abstract
The invention discloses a titanium alloy artificial articular head with wear-resistant ceramic coating and a preparation method of the titanium alloy artificial articular head. The titanium alloy artificial articular head comprises a titanium alloy articular head body, wherein a micropore array texture is formed on the surface of the titanium alloy articular head body, an antifriction and wear-resistant ceramic coating is arranged on the surface of the titanium alloy artificial articular head, and the surface layer of the antifriction and wear-resistant ceramic coating is a compact ceramic coating subjected to pore filling and sealing with hard nanoparticles; the microproe array texture is a regular micropore array which is formed in the surface where the titanium alloy articular head is in contact with a joint cup; and an oxidation ceramic coating is a hard oxidation layer prepared by adopting a two-step plasma electrolytic oxidation process and is compounded on a textured surface. The artificial articular head with the wear-resistant ceramic coating capable of improving lubricating property has the advantages that wear resistance is enhanced, and the wear of paired friction parts, namely cotyle, can be obviously reduced; meanwhile, toughness of the titanium alloy body is maintained, and cost is obviously lower than that of a full ceramic articular head.
Description
Technical field
The present invention relates to a kind of implant device and preparation method thereof, be specifically related to a kind of band titanium alloy artificial joint head being improved the abrasion-proof ceramic coat of lubricity and preparation method thereof.
Background technology
Wearing and tearing are the aseptic loosening principal elements lost efficacy with late period of joint prosthesis, current artificial joint head is primarily of cobalt-base alloy and alumina-ceramic preparation, pottery bulb has high, good with the wettability of the knuckle synovia advantage of wear resistance, but the essential fragility of ceramic bulb and high cost, affect its widespread use.Although cobalt-base alloy ball and socket joint has higher wear resistance, due to insufficient lubrication in body, the wettability of metal and body fluid is poor, is difficult to form hydrldynamic pressure lubrication in the lower situation of sliding velocity, and be often in mixed lubricating state in vivo, frictional coefficient is higher.Therefore, still can produce a large amount of metal filings in its use procedure, metal filings can infiltrate blood, and dissolves the harmful metal ions such as a large amount of Cr-, causes soft tissue infection that entire patient even can be made poisoning, has a strong impact on its reliability and work-ing life.
Titanium alloy has the features such as good biocompatibility, rotproofness, high strength, low-gravity, is widely used in medicine equipment and Aeronautics and Astronautics device field.But, because titanium alloy surface hardness is low, wear no resistance, thus limit the application of titanium alloy on friction load bearing component.The patent of invention " titanium alloy artificial joint head surface titanium oxide is to the method for making of titanium nitride gradient wear resistant layer " of publication number CN1715439A is authorized to adopt All directions ion implantation machine to titanium alloy ball and socket joint first with the target temperature of 600 ~ 700 DEG C, High dose implantation Nitrogen ion, produces deep nitrizaton thing dispersion-strengthened substrate on titanium alloy ball and socket joint surface; High dose implantation oxonium ion again, forms Ti-O-Ti-N Gradient Film on titanium alloy ball and socket joint surface.Authorize the patent of invention " Ti-TiN-CNx gradient multilayer film and preparation method thereof " of publication number CN101804708A to adopt the amorphous CNx rete of the standby TiN/CNx gradient multilayer transition layer that is mutually alternately made up of TiN and amorphous CNx of non-balance magnetically controlled sputter legal system and graphite-like structure, have lower frictional coefficient and wear rate.But these two kinds method complex process preparing wear-resistant coating, cost are high.Authorize the patent of invention " medical titanium alloy hip joint bulb surface carburization process " of publication number CN 100510156C that medical titanium alloy hip joint bulb is put into vacuum cementation furnace, acetylene is adopted to do carburizing gas, carburizing under 1300 DEG C of high temperature, because carburizing temperature is too high, inevitably cause joint ball head to be out of shape, affect its actual use.Authorize the patent of invention of publication number CN 101347358 B " titanium alloy artificial hip joint of band abrasion-proof ceramic coat and manufacture method thereof " on the capital sphere of titanium alloy, carry out spark with the surface of titanium alloy hip cup and strengthen electrochemical oxidation generation abrasion-proof ceramic coat, obtain that film thickness is thick, film and substrate combinating strength is high, mechanics supporting capacity is good wear-resistant coating, but the coated porous that the method obtains, its compactness need to improve.The patent of invention " a kind of preparation method of microarc oxidation/hydrothermtreatment treatment composite film on surface of magnesium alloy " of application number 201210049884.0 adopts follow-up hydrothermal treatment consists, while calcium phosphoric is introduced on oxidation ceramic layer surface, shutoff can also be carried out to the hole of ceramic surface, effectively reduce the intrusion of corrosive medium.But obtaining this composite film needs multi step strategy, and technique is loaded down with trivial details, and the rete of subsequent deposition in use easily peels off, and loses plugging effect.
Summary of the invention
After joint replacement, joint capsule is cut, and knuckle synovia deficiency can cause that replacement joint lubricating status is not good and unstable wear and titanium alloy wear no resistance, and can not do joint first order issue.The object of this invention is to provide a kind of abrasion-proof ceramic coat titanium alloy artificial joint head and preparation method thereof, this artificial joint head imitates native articular cartilage porous water-bearing structure and lubricating function, lubrication is improved by surface micropore array texture, micropore can also catch abrasive dust, reduce abrasive wear, improve the wear resistance of ball and socket joint and mortar simultaneously.Two step plasma electrolysis oxidation process are adopted to make top coat finer and close.A wear resistance of ceramic articulation head is not only had on surface of the present invention with the titanium alloy artificial joint head of texture and ceramic composite coating, also have to improve lubrication, reduce fricting couple piece---the function of cotyla wearing and tearing, and also its cost is significantly lower than ceramic articulation head.
Object of the present invention is achieved through the following technical solutions:
A kind of abrasion-proof ceramic coat titanium alloy artificial joint head, it is characterized in that: this artificial joint head comprises the titanium alloy ball and socket joint body that surface forms microwell array texture, be provided with anti-friction wear-resistant ceramic coating at titanium alloy ball and socket joint body surface, the top layer of described anti-friction wear-resistant ceramic coating is the dense ceramic layers through the filling perforation of hard nanometer particle and sealing of hole.
In the present invention, described anti-friction wear-resistant ceramic coating adopts two step plasma electrolysis oxidation process preparations, and anti-friction wear-resistant ceramic coating total thickness is 25-55 μm, and the thickness of surface compact ceramic layer is 10-15 μm.
Described microwell array texture is circular micropore and is evenly distributed on titanium alloy ball and socket joint body sphere, micro-pore diameter D=50 ~ 1000 μm, micropore degree of depth h=10 ~ 55 μm, micropore area occupation rate S=5% ~ 35%.
A preparation method for abrasion-proof ceramic coat titanium alloy artificial joint head, is characterized in that the method concrete steps are as follows:
1) titanium alloy ball and socket joint body outer round surface is polished to minute surface;
2) surface-texturing process is carried out to the titanium alloy ball and socket joint body of polishing, formation rule microwell array texture; Described microwell array texture is prepared by laser ablation, photoetching electrochemical micromachining and mechanical pressing in method, described microwell array texture is made up of in the distribution of titanium alloy ball and socket joint body spherical uniform circular micropore, micro-pore diameter D=50 ~ 1000 μm, micropore degree of depth h=10 ~ 55 μm, micropore area occupation rate S=5% ~ 35%.
3) HF-HNO is adopted
3solution cleaning is with the titanium alloy ball and socket joint body surface of microwell array texture;
4) with the titanium alloy ball and socket joint body with microwell array texture for anode, be immersed in silicate/phosphate solution, adopt high-pressure pulse direct current source carry out the process of the first step plasma electrolysis oxidation; Wherein water glass (Na
2siO
3) concentration 6-10g/L, ten phosphate dihydrate sodium (Na
3pO
412H
2o) concentration 6-10g/L.Described the first step plasma electrolysis oxidation process, voltage of supply is 500-600V, pulse-repetition 400-800Hz, dutycycle 10%-20%, treatment time 30-60min, and obtaining ceramic oxide layer thickness is 10-35 μm.
5) will the titanium alloy ball and socket joint body of the first step plasma electrolysis oxidation process be completed, and be immersed in the silicate/phosphate suspension liquid containing nanometer hard particles, carry out the process of second step plasma electrolysis oxidation; The described silicate/phosphate suspension liquid containing nanometer hard particles, OP emulsifying dispersant wherein containing 0.1-0.5g/L, its nanometer hard particles is silicon-dioxide, aluminum oxide or silicon nitride nano ceramic particle, and particle diameter is 1 ~ 100 nm, and content is 10-20g/L.Described second step plasma electrolysis oxidation process, voltage of supply 550-650V, pulse-repetition 400-800Hz, dutycycle 10%-20%, treatment time 30-60min, obtaining oxidation ceramic layer total thickness is 15-55 μm, and wherein containing nano particle filling perforation density ceramic oxide layer thickness is 5-15 μm.
6) carry out surface grinding to the titanium alloy ball and socket joint body completing the process of second step plasma electrolysis oxidation, remove the rough layer of outside surface, then polished finish, obtains abrasion-proof ceramic coat titanium alloy artificial joint head.
In the present invention, microwell array texture is the regular microwell array be processed to form on the surface that titanium alloy ball and socket joint contacts with mortar cup; Ceramic oxide coating is hardening oxidation layer prepared by employing two step plasma electrolysis oxidation process, and is compounded in textured surfaces; Two step method plasma electrolysis oxidation process for first carrying out the process of the first step plasma electrolysis oxidation using silicate/phosphate mixing solutions as electrolytic solution, then carries out second step oxide treatment using the silicate/phosphate suspension liquid containing nano particle as electrolytic solution.
Compared with prior art, advantage of the present invention:
Surface texturing techniques and two step plasma electrolysis oxidation technology combine by the present invention, prepare texturing/ceramic compound coating at titanium alloy ball and socket joint outer round surface.Surface Texture as the storage pond of knuckle synovia, can provide lubricant to friction surface in sliding friction process, increases the thickness of lubricant film, realizes hydrldynamic pressure lubrication.Plasma electrolysis oxidation ceramic layer can as wearing layer, reduces the problems such as the inflammation that causes because of the wearing and tearing on titanium alloy ball and socket joint surface and ball and socket joint loosen.Adopt two step plasma electrolysis oxidation treatment process, not only further increase thickness of ceramic coating, and the nano particle in electrolytic solution carries out filling perforation density to loose porous ceramic oxide skin.Compared with the secondary hole sealing treatment technologies such as the hydrothermal treatment consists that tradition is follow-up, the present invention adopts two step ion electrolysis oxidation technologies electrolytic oxidation and nano particle filling perforation, sealing of hole to be carried out simultaneously, further increase the thickness of ceramic oxide coating, because the filling perforation of hard nanometer ceramic particle, sealing of hole carry out in ion electrolytic oxidation, the bonding properties of nano particle and porous oxidation pottery is better, surface filling perforation, sealing of hole layer compactness are higher, can improve hardness and the wear resistance of ceramic layer further.
The ball and socket joint surface ceramic deposition that the present invention adopts two step plasma electrolysis oxidation process to make with microwell array texture, not only obtain thickness and reach the ceramic layer of 55 μm, and its top layer there is hard nanometer ceramic particle filling perforation sealing of hole, thickness reaches the dense ceramic layers of 15 μm.The present invention not only has the wear resistance of ceramic articulation head, also has and increases lubrication film thickness and rigidity, improve the function of lubricating status after displacement, and surface micropore can also catch abrasive dust simultaneously, reduces abrasive wear.Therefore, the abrasion-proof ceramic coat artificial joint head that band of the present invention is improved lubricity not only increases the wear resistance of self, and significantly can reduce fricting couple piece---the wearing and tearing of cotyla, and also its cost is significantly lower than full ceramic articulation head.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Fig. 2 is A portion partial enlarged drawing in Fig. 1.
Embodiment
In conjunction with the accompanying drawings and embodiments, technical solution of the present invention is described in detail, but protection scope of the present invention is not limited to described embodiment.
Embodiment 1:
A kind of abrasion-proof ceramic coat titanium alloy artificial joint head, this artificial joint head comprises the titanium alloy ball and socket joint body 1 that surface forms microwell array texture 2, be provided with anti-friction wear-resistant ceramic coating 3 on titanium alloy ball and socket joint body 1 surface, the top layer of anti-friction wear-resistant ceramic coating 3 is the dense ceramic layers 4 through hard nanometer particle 5 filling perforation and sealing of hole.Hard nanometer particle is SiO
2particle.
A kind of Nano-meter SiO_2
2the titanium alloy artificial joint head surface texture of particle filling perforation and sealing of hole and the preparation method of ceramic wear-resistant coating, concrete preparation process is as follows:
1) polished finish is carried out to titanium alloy ball and socket joint body periphery;
2) laser etching techniques is adopted to carry out texturing process to titanium alloy ball and socket joint body surface, formation rule microwell array, wherein micro-pore diameter D=400 μm, micropore degree of depth h=30 μm, micropore area occupation rate S=35%.
3) HF-HNO is adopted
3solution cleaning, through the ball and socket joint of texturing process, removes the oxide compound on surface;
4) in silicate/phosphate mixed electrolytic solution, carry out the process of the first step plasma electrolysis oxidation, electrolytic solution is containing water glass 6g/L, sodium phosphate 10g/L, and voltage of supply is 500V, pulse-repetition 400Hz, dutycycle 10%, treatment time 60min;
5) be 10 μm of Nano-meter SiO_2 containing granularity
2carry out the process of second step plasma electrolysis oxidation in the silicate/phosphate suspension liquid of particle, water glass and sodium phosphate content constant, OP emulsifying agent 0.1g/L, Nano-meter SiO_2
2particle 10g/L, voltage 550V, pulse-repetition 400Hz, dutycycle 10%, treatment time 60min;
(6) surface grinding and polished finish are carried out to the titanium alloy ball and socket joint with Surface Texture and ceramic layer, obtain lubricious ceramic layer, obtain abrasion-proof ceramic coat titanium alloy artificial joint head.
Embodiment 2:
A kind of abrasion-proof ceramic coat titanium alloy artificial joint head, structure is with embodiment 1, and hard nanometer particle is Al
2o
3particle.
A kind of nanometer Al
2o
3the titanium alloy artificial joint head surface texture of particle filling perforation and sealing of hole and the preparation method of ceramic wear-resistant coating, concrete preparation process is as follows:
1) polished finish is carried out to titanium alloy ball and socket joint periphery;
2) photoetching electrochemical micromachining technology is adopted to carry out texturing process to titanium alloy ball and socket joint, formation rule microwell array, micro-pore diameter D=100 μm, micropore degree of depth h=10 μm, micropore area occupation rate S=20%.
3) HF-HNO is adopted
3solution cleaning, through the ball and socket joint of texturing process, removes the oxide compound on surface;
4) in silicate/phosphate mixed electrolytic solution, carry out the process of the first step plasma electrolysis oxidation, electrolytic solution is containing water glass 8g/L, sodium phosphate 8g/L, and voltage of supply is 550V, pulse-repetition 600Hz, dutycycle 15%, treatment time 45min;
5) be 40 μm of nanometer Al containing granularity
2o
3carry out the process of second step plasma electrolysis oxidation in the silicate/phosphate suspension liquid of particle, water glass and sodium phosphate content constant, OP emulsifying agent 0.3g/L, nanometer Al
2o
3particle 15g/L, voltage 600V, pulse-repetition 600Hz, dutycycle 15%, treatment time 45min;
6) surface grinding and polished finish are carried out to the titanium alloy ball and socket joint with Surface Texture and ceramic layer, obtain lubricious ceramic layer.
Embodiment 3:
A kind of nano Si
3n
4the titanium alloy artificial joint head surface texture of particle filling perforation and sealing of hole and the preparation method of ceramic wear-resistant coating, concrete preparation process is as follows:
1) polished finish is carried out to titanium alloy ball and socket joint periphery;
2) mechanical pressing in method titanium alloy ball and socket joint is adopted to carry out texturing process, formation rule microwell array, micro-pore diameter D=1000 μm, micropore degree of depth h=55 μm, micropore area occupation rate S=5%.
3) HF-HNO is adopted
3solution cleaning, through the ball and socket joint of texturing process, removes the oxide compound on surface;
4) in silicate/phosphate mixed electrolytic solution, carry out the process of the first step plasma electrolysis oxidation, electrolytic solution is containing water glass 10g/L, sodium phosphate 6g/L, and voltage of supply is 600V, pulse-repetition 800Hz, dutycycle 20%, treatment time 30min;
5) be 80 μm of nano Si containing granularity
3n
4carry out the process of second step plasma electrolysis oxidation in the silicate/phosphate suspension liquid of particle, water glass and sodium phosphate content constant, OP emulsifying agent 0.5g/L, nano Si
3n
4particle 20g/L, voltage 650V, pulse-repetition 800Hz, dutycycle 20%, treatment time 30min;
6) surface grinding and polished finish are carried out to the titanium alloy ball and socket joint with Surface Texture and ceramic layer, obtain lubricious ceramic layer.
Claims (8)
1. an abrasion-proof ceramic coat titanium alloy artificial joint head, it is characterized in that: this artificial joint head comprises the titanium alloy ball and socket joint body (1) that surface forms microwell array texture (2), be provided with anti-friction wear-resistant ceramic coating (3) on titanium alloy ball and socket joint body (1) surface, the top layer of described anti-friction wear-resistant ceramic coating (3) is the dense ceramic layers (4) through (5) filling perforation of hard nanometer particle and sealing of hole.
2. abrasion-proof ceramic coat titanium alloy artificial joint head according to claim 1, it is characterized in that: described anti-friction wear-resistant ceramic coating (3) adopts two step plasma electrolysis oxidation process preparations, anti-friction wear-resistant ceramic coating (3) total thickness is 25-55 μm, and the thickness of surface compact ceramic layer (4) is 10-15 μm.
3. abrasion-proof ceramic coat titanium alloy artificial joint head according to claim 1, it is characterized in that: described microwell array texture (2) is for circular micropore and be evenly distributed on titanium alloy ball and socket joint body (1) sphere, micro-pore diameter D=50 ~ 1000 μm, micropore degree of depth h=10 ~ 55 μm, micropore area occupation rate S=5% ~ 35%.
4. abrasion-proof ceramic coat titanium alloy artificial joint head according to claim 1, is characterized in that: described hard nanometer particle (5) is silicon-dioxide, aluminum oxide or silicon nitride nano ceramic particle, and particle diameter is 1 ~ 100 nm.
5. the preparation method of abrasion-proof ceramic coat titanium alloy artificial joint head according to claim 1, is characterized in that the method concrete steps are as follows:
1) titanium alloy ball and socket joint body outer round surface is polished to minute surface;
2) surface-texturing process is carried out to the titanium alloy ball and socket joint body of polishing, formation rule microwell array texture;
3) HF-HNO is adopted
3solution cleaning is with the titanium alloy ball and socket joint body surface of microwell array texture;
4) with the titanium alloy ball and socket joint body with microwell array texture for anode, be immersed in silicate/phosphate solution, adopt high-pressure pulse direct current source carry out the process of the first step plasma electrolysis oxidation;
5) will the titanium alloy ball and socket joint body of the first step plasma electrolysis oxidation process be completed, and be immersed in the silicate/phosphate suspension liquid containing nanometer hard particles, carry out the process of second step plasma electrolysis oxidation;
6) carry out surface grinding to the titanium alloy ball and socket joint body completing the process of second step plasma electrolysis oxidation, remove the rough layer of outside surface, then polished finish, obtains abrasion-proof ceramic coat titanium alloy artificial joint head.
6. the preparation method of abrasion-proof ceramic coat titanium alloy artificial joint head according to claim 5, it is characterized in that: step 2) in, described microwell array texture is prepared by laser ablation, photoetching electrochemical micromachining or mechanical pressing in method, described microwell array texture is made up of in the distribution of titanium alloy ball and socket joint body spherical uniform circular micropore, micro-pore diameter D=50 ~ 1000 μm, micropore degree of depth h=10 ~ 55 μm, micropore area occupation rate S=5% ~ 35%.
7. the preparation method of abrasion-proof ceramic coat titanium alloy artificial joint head according to claim 5, is characterized in that: in step 4), in silicate/phosphate solution, and sodium silicate silicate 6-10g/L, ten phosphate dihydrate na concn 6-10g/L; Described the first step plasma electrolysis oxidation process, voltage of supply is 500-600V, pulse-repetition 400-800Hz, dutycycle 10%-20%, treatment time 30-60min, and obtaining ceramic oxide layer thickness is 10-35 μm.
8. the preparation method of abrasion-proof ceramic coat titanium alloy artificial joint head as claimed in claim 5, it is characterized in that: in step 5), the described silicate/phosphate suspension liquid containing nanometer hard particles, OP emulsifying dispersant wherein containing 0.1-0.5g/L, its nanometer hard particles is silicon-dioxide, aluminum oxide or silicon nitride nano ceramic particle, particle diameter is 1 ~ 100 nm, and content is 10-20g/L; Described second step plasma electrolysis oxidation process, voltage of supply 550-650V, pulse-repetition 400-800Hz, dutycycle 10%-20%, treatment time 30-60min, obtaining oxidation ceramic layer total thickness is 15-55 μm, and wherein containing nano particle filling perforation density ceramic oxide layer thickness is 5-15 μm.
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| CN107029284A (en) * | 2017-06-03 | 2017-08-11 | 张文平 | A kind of artificial joint material |
| CN107829123A (en) * | 2017-10-09 | 2018-03-23 | 深圳市中科摩方科技有限公司 | A kind of aluminium alloy of surface duplex coating and its preparation method and application |
| CN108472408A (en) * | 2015-12-29 | 2018-08-31 | Zm精密牙科技术有限责任公司 | Orthopaedic implant |
| CN112545715A (en) * | 2020-11-23 | 2021-03-26 | 西安交通大学 | Artificial joint-oriented directional aggregation lubrication method of field dilute solution |
| CN113350570A (en) * | 2021-06-17 | 2021-09-07 | 湘潭大学 | Artificial joint with self-repairing textured composite film structure and preparation method thereof |
| CN113774460A (en) * | 2021-09-30 | 2021-12-10 | 中山大学 | Preparation method of titanium alloy plasma electrolytic oxidation composite coating |
| CN114807836A (en) * | 2022-03-08 | 2022-07-29 | 沈阳建筑大学 | Preparation method of textured artificial joint composite coating |
| US20220364253A1 (en) * | 2020-04-24 | 2022-11-17 | Cirrus Materials Science Limited | Method to apply color coatings on alloys |
| CN115961283A (en) * | 2023-02-08 | 2023-04-14 | 重庆大学 | Preparation method of protective coating for alloy surface |
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| CN108472408A (en) * | 2015-12-29 | 2018-08-31 | Zm精密牙科技术有限责任公司 | Orthopaedic implant |
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| CN114807836A (en) * | 2022-03-08 | 2022-07-29 | 沈阳建筑大学 | Preparation method of textured artificial joint composite coating |
| CN115961283A (en) * | 2023-02-08 | 2023-04-14 | 重庆大学 | Preparation method of protective coating for alloy surface |
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