CN104562146B - 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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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 and in particular to a kind of with improving the resistance to of greasy property
Titanium alloy artificial joint head of mill ceramic coating and preparation method thereof.
Background technology
Abrasion is that joint prosthesis is aseptic loosens the principal element losing efficacy with late period, and current artificial joint head is mainly by cobalt alloy
Prepare with aluminium oxide ceramics, ceramic bulb has the advantages that wearability is high good with the wetability of knuckle synovia, but ceramic bulb
Essential fragility and high cost, affect it and extensively apply.Although cobalt alloy ball and socket joint has higher wearability, moistened due to internal
Cunning is bad, and metal is poor with the wetability of body fluid, difficult to form hydrldynamic pressure lubrication in the case of sliding speed is relatively low, in vivo often
It is in mixed lubricating state, coefficient of friction is higher.Therefore, a large amount of metal filings can still be produced during its use, metal grinds
Bits can penetrate into blood, and dissolves the harmful metal ions such as a large amount of cr-, causes soft tissue infection even can make in entire patient
Poison, has a strong impact on its reliability and service life.
Titanium alloy has the features such as good biocompatibility, rotproofness, high intensity, low-gravity, in medicine equipment and boat
Empty, spacecraft is widely used in field.But, because titanium alloy surface hardness is low, wear no resistance, thus limiting titanium alloy
Application on friction load bearing component.Authorize patent of invention " the titanium alloy artificial joint head surface oxygen of publication number cn1715439a
Change titanium to the preparation method of titanium nitride gradient wear resistant layer " adopt All directions ion implantation machine to titanium alloy ball and socket joint first with 600 ~ 700 DEG C
Target temperature, High dose implantation Nitrogen ion, titanium alloy joint head surface produce deep nitrizaton thing dispersion-strengtherning substrate；High dose again
Injection oxonium ion, forms ti-o-ti-n Gradient Film in titanium alloy joint head surface.Authorize sending out of publication number cn101804708a
Bright patent " ti-tin-cnx gradient multilayer film and preparation method thereof " adopts non-balance magnetically controlled sputter method to prepare by tin and amorphous
Cnx alternates the tin/cnx gradient multilayer transition layer of composition and the amorphous cnx film layer of graphite-like structure, has relatively low friction
Coefficient and wear rate.But both prepares the method complex process of wear-resistant coating, high cost.Authorize publication number cn
The patent of invention " medical titanium alloy hip joint bulb surface carburization process " of 100510156c is medical titanium alloy hip joint bulb
Put in vacuum cementation furnace, carburizing gas is done using acetylene, carburizing under 1300 DEG C of high temperature, because carburizing temperature is too high, can not
The joint ball head that causes avoiding deforms, and affects it actually used.The patent of invention authorizing publication number cn 101347358 b " carries resistance to
The mill titanium alloy artificial hip joint of ceramic coating and its manufacture method " on the capital sphere of titanium alloy and titanium alloy hip cup
Surface carries out spark and strengthens electrochemical oxidation generation abrasion-proof ceramic coat, obtains film thickness thickness, film and substrate combinating strength
Wear-resistant coating high, that mechanics bearing capacity is good, but the coated porous that the method obtains, its compactness need to be improved.Application number
201210049884.0 patent of invention " a kind of preparation method of microarc oxidation/hydrothermtreatment treatment composite film on surface of magnesium alloy " adopt
With follow-up hydro-thermal process, while oxide ceramic layer surface introduces calcium P elements, the hole of ceramic surface can also be entered
Row closure, effectively reduces the intrusion of corrosive medium.But, obtaining this composite film needs multi step strategy, and technique is loaded down with trivial details, and after
The film layer of continuous deposition is easily peeled off in use, loses plugging effect.
Content of the invention
After joint replacement, capsular ligament be removed, knuckle synovia deficiency replacement joint lubricating status can be led to not good and
Unstable wear and titanium alloy wear no resistance it is impossible to do joint first order issue.It is an object of the invention to provide a kind of wear-resistant ceramic applies
Layer titanium alloy artificial joint head and preparation method thereof, this artificial joint head imitates native articular cartilage porous water-bearing structure and lubrication
Function, improves lubrication by surface micropore array texture, and micropore can also capture abrasive dust, reduces abrasive wear, improves simultaneously and closes
Section header and the wearability of mortar.Make face coat finer and close using two step plasma electrolysis oxidation process.The surface band of the present invention
The titanium alloy artificial joint head having texture and ceramic composite coating not only has the abrasive resistance of ceramic articulation head, also has improvement profit
Function that is sliding, reducing the abrasion of fricting couple piece cotyla, and its cost is substantially less than ceramic articulation head.
The purpose 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 characterised in that: this artificial joint head includes surface and is formed
The titanium alloy ball and socket joint body of microwell array texture, is provided with anti-friction wear-resistant ceramic coating, institute in titanium alloy ball and socket joint body surface
The top layer stating anti-friction wear-resistant ceramic coating is dense ceramic layers through hard nanometer particle filling perforation and sealing of hole.
In the present invention, described anti-friction wear-resistant ceramic coating adopts two step plasma electrolysis oxidation process preparations, anti-friction wear-resistant
Ceramic coating gross 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 depth h=10～55 μm, micropore area occupation rate s=5%～35%.
A kind of preparation method of abrasion-proof ceramic coat titanium alloy artificial joint head it is characterised in that the method concrete steps such as
Under:
1) titanium alloy ball and socket joint body outer round surface is polished to minute surface；
2) surface-texturing process, formation rule microwell array texture are carried out to the titanium alloy ball and socket joint body of polishing；Institute
The microwell array texture stated is prepared by laser ablation, photoetching electrochemical micromachining and mechanical indentation method, described microwell array texture
It 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 depth h=
10～55 μm, micropore area occupation rate s=5%～35%.
3) adopt hf-hno3The titanium alloy ball and socket joint body surface with microwell array texture for the solution cleaning；
4) with the titanium alloy ball and socket joint body with microwell array texture as anode, it is immersed in silicate/phosphate solution
In, first step plasma electrolysis oxidation process is carried out using high-pressure pulse direct current source；Wherein sodium metasilicate (na2sio3) concentration 6-
10g/l, ten phosphate dihydrate sodium (na3po4·12h2O) concentration 6-10g/l.Described first step plasma electrolysis oxidation is processed, electricity
Source voltage is 500-600v, pulse frequency 400-800hz, dutycycle 10%-20%, process time 30-60min, obtains oxidation pottery
Porcelain thickness is 10-35 μm.
5) the titanium alloy ball and socket joint body of first step plasma electrolysis oxidation process will be completed, be immersed in hard containing nanometer
In the silicate/phosphate suspension of grain, carry out second step plasma electrolysis oxidation process；Described containing nanometer hard particles
Silicate/phosphate suspension, the op emulsifying dispersant wherein containing 0.1-0.5g/l, its nanometer of hard particles are titanium dioxide
Silicon, aluminum oxide or silicon nitride nano ceramic particle, particle diameter is 1 ~ 100 nm, and content is 10-20g/l.Described second step etc. from
Sub- electrolytic oxidation process, supply voltage 550-650v, pulse frequency 400-800hz, dutycycle 10%-20%, process time 30-
60min, obtains oxidation ceramic layer gross thickness and is 15-55 μm, and wherein the density of filling perforation containing nano particle oxidation ceramic layer thickness is 5-
15μm.
6) surface grinding is carried out to the titanium alloy ball and socket joint body completing the process of second step plasma electrolysis oxidation, except going
The rough layer on surface, then polishing, obtain abrasion-proof ceramic coat titanium alloy artificial joint head.
In the present invention, microwell array texture is the rule processing formation with mortar cup on the surface that titanium alloy ball and socket joint is contacted
Microwell array；Oxide ceramic coating is the hardening oxidation layer using two step plasma electrolysis oxidation process preparations, and is compounded in and knits
On structure surface；Two step method plasma electrolysis oxidation process is first to be carried out using silicate/phosphate mixed solution as electrolyte
First step plasma electrolysis oxidation is processed, then carries out the using the silicate/phosphate suspension containing nano particle as electrolyte
Second oxidation is processed.
Compared with prior art, the advantage of the present invention:
Surface texturing techniques and two step plasma electrolysis oxidation technology are combined by the present invention, outside titanium alloy ball and socket joint
Circular surfaces prepare texturing/ceramic composite coating.Surface Texture can be as the reservoir of knuckle synovia, in sliding friction process
The middle thickness providing lubricant to friction surface, increasing lubricating film, realizes hydrldynamic pressure lubrication.Plasma electrolysis oxidation ceramic layer
The inflammation that causes because of the abrasion of titanium alloy joint head surface can be reduced as wearing layer and the problems such as ball and socket joint loosens.Adopt
With two step plasma electrolysis oxidation handling process, not only further increase thickness of ceramic coating, and the nanometer in electrolyte
Particle has carried out filling perforation density to loose porous oxide ceramic outer layer.The secondary hole sealings such as the hydro-thermal process follow-up with tradition are processed
Technology is compared, and the present invention is electrolysed oxidation technology using two step ions and carries out electrolytic oxidation and nano particle filling perforation, sealing of hole simultaneously,
Further increase the thickness of oxide ceramic coating, because hard nanometer ceramic particle filling perforation, sealing of hole are in ion electrolytic oxidation
In carry out, more preferably, surface filling perforation, sealing of hole layer compactness are higher, Ke Yijin for the binding ability of nano particle and porous oxidation pottery
One step improves hardness and the wearability of ceramic layer.
The present invention makes the ball and socket joint surface ceramic deposition with microwell array texture using two step plasma electrolysis oxidation process,
Not only obtain the ceramic layer that thickness reaches 55 μm, and its top layer has hard nanometer ceramic particle filling perforation sealing of hole, thickness to reach 15 μm
Dense ceramic layers.The present invention not only has the abrasive resistance of ceramic articulation head, after displacement also have increase lubrication film thickness and
Rigidity, improves the function of lubricating status, and surface micropore can also capture abrasive dust simultaneously, reduces abrasive wear.Therefore, band of the present invention
There is the abrasion-proof ceramic coat artificial joint head improving greasy property to not only increase the wearability of itself, and can substantially reduce and rub
Wipe the abrasion of couple cotyla, and its cost is substantially less than full ceramic articulation head.
Brief description
Fig. 1 is the structural representation of the present invention.
Fig. 2 is a portion partial enlarged drawing in Fig. 1.
Specific 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
It is confined to described embodiment.
Embodiment 1:
A kind of abrasion-proof ceramic coat titanium alloy artificial joint head, this artificial joint head includes surface and forms microwell array texture
2 titanium alloy ball and socket joint body 1, is provided with anti-friction wear-resistant ceramic coating 3 on titanium alloy ball and socket joint body 1 surface, and anti-friction wear-resistant is made pottery
The top layer of porcelain coating 3 is the dense ceramic layers 4 through hard nanometer particle 5 filling perforation and sealing of hole.Hard nanometer particle is sio2?
Grain.
A kind of nanometer sio2The titanium alloy artificial joint head surface texture of particle filling perforation and sealing of hole and ceramic wear-resistant coating
Preparation method, concrete preparation process is as follows:
1) titanium alloy ball and socket joint body periphery is processed by shot blasting；
2) using laser etching techniques, titanium alloy ball and socket joint body surface is carried out with texturing process, formation rule micropore battle array
Row, wherein d=400 μm of micro-pore diameter, h=30 μm of micropore depth, micropore area occupation rate s=35%.
3) adopt hf-hno3The ball and socket joint that solution cleaning is processed through texturing, removes the oxide on surface；
4) carry out first step plasma electrolysis oxidation process in silicate/phosphate mixed electrolytic solution, electrolyte is siliceous
Sour sodium 6g/l, sodium phosphate 10g/l, supply voltage is 500v, pulse frequency 400hz, dutycycle 10%, process time 60min；
5) it is being 10 μm of nanometers sio containing granularity2Carry out second step plasma electric in the silicate/phosphate suspension of particle
Solution oxidation processes, sodium metasilicate and phosphoric acid sodium content are constant, op emulsifying agent 0.1g/l, nanometer sio2Particle 10g/l, voltage 550v,
Pulse frequency 400hz, dutycycle 10%, process time 60min；
(6) the titanium alloy ball and socket joint with Surface Texture and ceramic layer is carried out with surface grinding and polishing, obtains light
Sliding ceramic layer, obtains 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 al with embodiment 1, hard nanometer particle2o3?
Grain.
A kind of nanometer al2o3The titanium alloy artificial joint head surface texture of particle filling perforation and sealing of hole and ceramic wear-resistant coating
Preparation method, concrete preparation process is as follows:
1) titanium alloy ball and socket joint periphery is processed by shot blasting；
2) texturing process, formation rule micropore battle array are carried out using photoetching electrochemical micromachining technology to titanium alloy ball and socket joint
Row, d=100 μm of micro-pore diameter, h=10 μm of micropore depth, micropore area occupation rate s=20%.
3) adopt hf-hno3The ball and socket joint that solution cleaning is processed through texturing, removes the oxide on surface；
4) carry out first step plasma electrolysis oxidation process in silicate/phosphate mixed electrolytic solution, electrolyte is siliceous
Sour sodium 8g/l, sodium phosphate 8g/l, supply voltage is 550v, pulse frequency 600hz, dutycycle 15%, process time 45min；
5) it is being 40 μm of nanometers al containing granularity2o3Carry out second step plasma in the silicate/phosphate suspension of particle
Electrolytic oxidation process, sodium metasilicate and phosphoric acid sodium content are constant, op emulsifying agent 0.3g/l, nanometer al2o3Particle 15g/l, voltage
600v, pulse frequency 600hz, dutycycle 15%, process time 45min；
6) the titanium alloy ball and socket joint with Surface Texture and ceramic layer is carried out with surface grinding and polishing, obtains smooth
Ceramic layer.
Embodiment 3:
A kind of nanometer si3n4The titanium alloy artificial joint head surface texture of particle filling perforation and sealing of hole and ceramic wear-resistant coating
Preparation method, concrete preparation process is as follows:
1) titanium alloy ball and socket joint periphery is processed by shot blasting；
2) texturing process, formation rule microwell array, micro-pore diameter d are carried out using mechanical indentation method titanium alloy ball and socket joint
=1000 μm, h=55 μm of micropore depth, micropore area occupation rate s=5%.
3) adopt hf-hno3The ball and socket joint that solution cleaning is processed through texturing, removes the oxide on surface；
4) carry out first step plasma electrolysis oxidation process in silicate/phosphate mixed electrolytic solution, electrolyte is siliceous
Sour sodium 10g/l, sodium phosphate 6g/l, supply voltage is 600v, pulse frequency 800hz, dutycycle 20%, process time 30min；
5) it is being 80 μm of nanometers si containing granularity3n4Carry out second step plasma in the silicate/phosphate suspension of particle
Electrolytic oxidation process, sodium metasilicate and phosphoric acid sodium content are constant, op emulsifying agent 0.5g/l, nanometer si3n4Particle 20g/l, voltage
650v, pulse frequency 800hz, dutycycle 20%, process time 30min；
6) the titanium alloy ball and socket joint with Surface Texture and ceramic layer is carried out with surface grinding and polishing, obtains smooth
Ceramic layer.
Claims (6)
1. a kind of abrasion-proof ceramic coat titanium alloy artificial joint head it is characterised in that: this artificial joint head include surface formed micro-
Titanium alloy ball and socket joint body (1) of hole array texture (2), is provided with anti-friction wear-resistant pottery on titanium alloy ball and socket joint body (1) surface
Coating (3), the top layer of described anti-friction wear-resistant ceramic coating (3) is the fine and close pottery through (5) filling perforation of hard nanometer particle and sealing of hole
Enamel coating (4)；Described anti-friction wear-resistant ceramic coating (3) adopts two step plasma electrolysis oxidation process preparations, and anti-friction wear-resistant pottery applies
Layer (3) gross thickness is 25-55 μm, and the thickness of surface compact ceramic layer (4) is 10-15 μm；Described microwell array texture (2) is circle
Shape micropore and be evenly distributed on titanium alloy ball and socket joint body (1) sphere, micro-pore diameter d=50～1000 μm, micropore depth h=10
～55 μm, micropore area occupation rate s=5%～35%.
2. abrasion-proof ceramic coat titanium alloy artificial joint head according to claim 1 it is characterised in that: described hard nanometer
Particle (5) is silica, aluminum oxide or silicon nitride nano ceramic particle, and particle diameter is 1～100 nm.
3. the preparation method of abrasion-proof ceramic coat titanium alloy artificial joint head according to claim 1 is it is characterised in that be somebody's turn to do
Method specifically comprises the following steps that
1) titanium alloy ball and socket joint body outer round surface is polished to minute surface；
2) surface-texturing process, formation rule microwell array texture are carried out to the titanium alloy ball and socket joint body of polishing；
3) adopt hf-hno3The titanium alloy ball and socket joint body surface with microwell array texture for the solution cleaning；
4) with the titanium alloy ball and socket joint body with microwell array texture as anode, it is immersed in silicate/phosphate solution, adopts
Carry out first step plasma electrolysis oxidation process with high-pressure pulse direct current source；
5) the titanium alloy ball and socket joint body of first step plasma electrolysis oxidation process will be completed, be immersed in containing nanometer hard particles
In silicate/phosphate suspension, carry out second step plasma electrolysis oxidation process；
6) surface grinding is carried out to the titanium alloy ball and socket joint body completing the process of second step plasma electrolysis oxidation, go exterior surface
Rough layer, then polishing, obtain abrasion-proof ceramic coat titanium alloy artificial joint head.
4. abrasion-proof ceramic coat titanium alloy artificial joint head according to claim 3 preparation method it is characterised in that: step
In rapid 2), described microwell array texture is prepared by laser ablation, photoetching electrochemical micromachining or mechanical indentation method, described micro-
Hole 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 depth h=10～55 μm, micropore area occupation rate s=5%～35%.
5. abrasion-proof ceramic coat titanium alloy artificial joint head according to claim 3 preparation method it is characterised in that: step
In rapid 4), in silicate/phosphate solution, sodium silicate silicate 6-10g/l, ten phosphate dihydrate na concn 6-10g/l；Described
One step plasma electrolysis oxidation is processed, and supply voltage is 500-600v, pulse frequency 400-800hz, dutycycle 10%-20%, place
Reason time 30-60min, obtains oxidation ceramic layer thickness and is 10-35 μm.
6. abrasion-proof ceramic coat titanium alloy artificial joint head as claimed in claim 3 preparation method it is characterised in that: step
In rapid 5), the described silicate/phosphate suspension containing nanometer hard particles, the op emulsification point wherein containing 0.1-0.5g/l
Powder, its nanometer of hard particles are silica, aluminum oxide or silicon nitride nano ceramic particle, and particle diameter is 1 ~ 100 nm, content
For 10-20g/l；Described second step plasma electrolysis oxidation is processed, supply voltage 550-650v, pulse frequency 400-800hz,
Dutycycle 10%-20%, process time 30-60min, obtain oxidation ceramic layer gross thickness and be 15-55 μm, wherein fill out containing nano particle
Density oxidation ceramic layer thickness in hole is 5-15 μm.
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| US12018396B2 (en) * | 2020-04-24 | 2024-06-25 | Cirrus Materials Science Ltd | Method to apply color coatings on alloys |
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| DE102015016895B3 (en) * | 2015-12-29 | 2017-05-24 | Zm Präzisionsdentaltechnik Gmbh | knee replacement |
| CN107029284B (en) * | 2017-06-03 | 2020-06-26 | 郑超 | Artificial joint material |
| CN107829123B (en) * | 2017-10-09 | 2020-05-12 | 深圳市中科摩方科技有限公司 | Aluminum alloy with double-layer coating on surface and preparation method and application thereof |
| 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 |
| CN113350570B (en) * | 2021-06-17 | 2022-03-08 | 湘潭大学 | Artificial joint with self-repairing textured composite film structure and preparation method thereof |
| CN113774460B (en) * | 2021-09-30 | 2023-04-21 | 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 |
| CN115961283B (en) * | 2023-02-08 | 2024-06-25 | 重庆大学 | Preparation method of protective coating for alloy surface |
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| CN101230474A (en) * | 2007-11-05 | 2008-07-30 | 南昌航空大学 | Method for depositing composite ceramic film by differential arc oxidation |
| CN101254138B (en) * | 2008-03-28 | 2010-06-02 | 西北有色金属研究院 | Micropore processing method of bone repairing body rough surface |
| CN103211666B (en) * | 2013-04-25 | 2016-05-18 | 南京理工大学 | A kind of joint prosthesis load-bearing surface micropore texture that improves lubricated and anti-wear performance |
| CN103498181A (en) * | 2013-09-04 | 2014-01-08 | 沈阳理工大学 | Preparation method of self-lubricating wear-resistant coating on surfaces of titanium and titanium alloy |
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