CN103451602A - Surface treatment process of bioactive metallic titanium implant having multistage micro-pit structure - Google Patents
Surface treatment process of bioactive metallic titanium implant having multistage micro-pit structure Download PDFInfo
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- CN103451602A CN103451602A CN201210166610XA CN201210166610A CN103451602A CN 103451602 A CN103451602 A CN 103451602A CN 201210166610X A CN201210166610X A CN 201210166610XA CN 201210166610 A CN201210166610 A CN 201210166610A CN 103451602 A CN103451602 A CN 103451602A
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Abstract
The invention relates to a surface treatment process of a bioactive metallic titanium implant having a multistage micro-pit structure, and the surface treatment process comprises the following steps: pretreatment, sandblasting treatment, acid etching treatment, sputtering treatment and glow discharge treatment; according to the surface treatment process, a multistage micro-pit three-dimensional structure having a bioactive tantalum coating is formed on the surface of the metallic titanium implant, so that the binding strength between the tantalum coating and the metallic titanium implant is very good, the tantalum coating is not easy to shed, shedding of the tantalum coating during or after an implantation process is avoided, the biological activity of the metal titanium implant can be improved, bone deposition of the surface of the metal titanium implant is accelerated, the tissue healing time is shortened, and through the formation of synostosis between the metal titanium implant and a surrounding bone tissue, the effect of improvement of the stability of the metal titanium implant can be achieved.
Description
Technical field
The present invention relates to a kind of metal titanium implant surface treatment process, particularly a kind of have a multistage dimple structure biological activity tantalum coating metal titanium implant process of surface treatment.
Background technology
The titanium or titanium alloy material has had more than 30 year history for body implant, is also the materials such as topmost orthopaedics implant, Stomatological Department implant now.Titanium or titanium alloy is as embedded material, particularly permanent implanted material is as joint prosthesis, artificial intervertebral disk, tooth metal titanium implant etc., must make tissue and metal titanium implant surface generation direct effect, just can make implant and surrounding tissue merge, and form good synostosis.Along with the development of biomedical engineering and process for treating surface, by various modem technologies, to the titanium or titanium alloy surface modification, can significantly improve biocompatibility, biological activity, resistance to corrosion of embedded material etc.And to make osseous tissue and implant form synostosis fast, and must form certain roughness on the kind of plant surface, also need to have extraordinary wetting ability and high surface energy, and material has extraordinary biological activity simultaneously.Meet at above 3 and can promote adhesion, the quickening bone apposition of scleroblast on the property implanted surface, make implant and body bone tissue form good synostosis, shorten healing time.Present stage, the treatment process of routine generally comprised: anodic oxidation, spraying technology, acid treatment, alkaline purification, thermal treatment etc.But the metal titanium implant surface wetting ability after their processing, biological activity is poor, the deficiencies such as knitting cycle length.These all can't meet above-mentioned three conditioned disjunctions simultaneously is that complex technical process is arranged, and the production cycle is long, and cost is high can't realize the shortcomings such as scale operation.
Summary of the invention
The objective of the invention is to overcome the defect that prior art exists, a kind of easy, efficient method is provided, form the multistage micro-hole three-dimensional structure with bioactive tantalum coating at the metal titanium implant surface, to improve the biological activity of metal titanium implant, accelerate the bone apposition of metal titanium implant surface, shorten the organization healing time; And make to form synostosis between metal titanium implant and surrounding bone tissue, improve the effect of metal titanium implant stability.
The technical scheme that realizes the object of the invention is a kind of multistage dimple structure biological activity tantalum coating metal titanium implant process of surface treatment that has, and comprises the following steps:
A. pre-treatment: a metal titanium implant after the machining fine grinding is provided, and adopts successively acetone, dehydrated alcohol, purified water respectively the ultrasonic cleaning oil removal treatment to be carried out in the surface of metal titanium implant, each five minutes, and dry;
B. sandblasting: adopt 24～70 purpose white fused aluminas to carry out sandblasting to the surface of pretreated metal titanium implant, blasting pressure is 0.1～0.6Mpa, sandblast to metal titanium implant surface is uniform grey, makes the metal titanium implant surface form the porous three-dimensional structure; And carry out pure water ultrasonic cleaning, drying;
C. acid etching: the metal titanium implant after sandblasting is soaked in the mixing acid of the hydrochloric acid that sulfuric acid that concentration range is 50wt%～75wt% and concentration range are 8wt%～20wt%, carry out the heating in water bath processing at the temperature of 50～80 ℃, make the metal titanium implant surface form multistage dimple structure, and carry out pure water ultrasonic cleaning, drying;
D. splash is processed: adopt the Ar ion sputtering to clean, then adopting pure tantalum is target, forms one deck by magnetron sputtering on the surface in multistage micro-hole and is less than the thick tantalum coating of 3 μ m, and carry out pure water ultrasonic cleaning 5min;
E. glow discharge is processed: to the metal titanium implant after cleaning carry out that glow discharge is clean, γ ray sterilization, sterile packed.
In the described step a of technique scheme, the ultrasonic cleaning of acetone, dehydrated alcohol, purified water is respectively carried out 2 times.
In the described step b of technique scheme, the spray gun in the sandblasting process and metal titanium implant axial 30 °～90 °, spray is apart from being 5～12cm, the sandblast time is 5～15s.
In the described step b of technique scheme, the roughness Ra of the metal titanium implant surface after sandblasting between 2-5 μ m, the one-level pit that the pit diameter of the vesicular structure after sandblasting is 10～40 μ m.
In the described step c of technique scheme, the time of magnetron sputtering is 20～30min, and temperature is 220～300 ℃, and power is 80～100W.
In the described step c of technique scheme, multistage dimple structure have the secondary pit of 2～4 μ m and 1 μ m following three, the level Four pit.
The surface of the described metal titanium implant of technique scheme has screw thread, and the metal titanium implant can be the implant of cylindricality or taper.
After adopting technique scheme, the present invention has following positive effect:
(1) the present invention's tantalum coating as thin as a wafer is embedded in the surface in multistage micro-hole, make between tantalum coating and matrix and there is extraordinary bonding strength, difficult drop-off, avoided tantalum coating coming off at implantation process and after implanting, the tantalum coating has extraordinary biological activity, can accelerate the healing rate between tissue and implant, shorten healing stage.
(2) the present invention compares with additive method, by step and the mode of adjusting whole treatment scheme; The kind of preferred sandblast sand used, granular size, pressure, and kind, the proportioning of acid, make its surface there is better surface tissue, the dimple structure of multistage micron, this dimple structure is beneficial to the deposition of tantalum coating very much, makes between the tantalum coatings and substrate and has extraordinary bonding strength.While tantalum coating does not as thin as a wafer change the multistage dimple structure after the sandblast acid etching, the wetting ability that makes surface have, higher surface energy; Surface roughness Ra, at 2-5 μ m, has best bone guided, shortens the operation healing time, and implant and osseous tissue bonding strength are high.
(3) adopt the tantalum coating can reduce the usage quantity of precious metal tantalum, reduce costs, can take full advantage of the biological activity of tantalum again, promote the growth of tissue simultaneously.
The accompanying drawing explanation
For content of the present invention more easily is expressly understood, below according to specific embodiment also by reference to the accompanying drawings, the present invention is further detailed explanation, wherein
Fig. 1 be metal titanium implant surface of the present invention through the white fused alumina sandblasting---sulfuric acid and mixed in hydrochloric acid sour water are bathed the SEM figure after processing;
Fig. 2 is that through the white fused alumina sandblasting,---sulfuric acid and mixed in hydrochloric acid sour water are bathed processing---SEM after sputter process schemes metal titanium implant surface of the present invention.
Embodiment
(embodiment 1)
In the present embodiment, the step of the threaded metal titanium implant of processing cylindricality is:
A. pre-treatment: a metal titanium implant after the machining fine grinding is provided, and adopts successively acetone, dehydrated alcohol, purified water respectively the ultrasonic cleaning oil removal treatment to be carried out to each 2 times in the surface of metal titanium implant, each five minutes; In order to clean up and oil removing, then dry.
B. sandblasting: adopt 24～70 purpose white fused aluminas to carry out sandblasting to the surface of pretreated metal titanium implant, axial 45 ° of spray gun metal titanium implant, the sandblast time is 8s, blasting pressure is 0.5Mpa, the spray distance is 10cm, sandblast to metal titanium implant surface is uniform grey, makes the metal titanium implant surface form the porous three-dimensional structure, and roughness Ra is 3 μ m; The one-level pit that the pit diameter of vesicular structure is 10～40 μ m, and carry out pure water ultrasonic cleaning, drying;
C. acid etching: the metal titanium implant after sandblasting is soaked in the mixing acid of the hydrochloric acid that sulfuric acid that concentration is 63wt% and concentration are 10wt%, carry out heating in water bath and process 10min at the temperature of 60 ℃, make the metal titanium implant surface form multistage dimple structure, multistage dimple structure have the secondary pit of 2～4 μ m and 1 μ m following three, the level Four pit, then carry out pure water ultrasonic cleaning, drying;
D. splash is processed: adopt the Ar ion sputtering to clean, then adopting pure tantalum is target, magnetron sputtering 20min, magnetron sputtering pressure is 0.3Pa, temperature is 250 ℃, power is 80W, forms one deck by magnetron sputtering on the surface in multistage micro-hole and is less than the thick tantalum coating of 3 μ m, then carries out pure water ultrasonic cleaning 5min;
E. glow discharge is processed: to the metal titanium implant after cleaning carry out that glow discharge is clean, γ ray sterilization, sterile packed.
(embodiment 2)
In the present embodiment, the step of the threaded metal titanium implant of processing cylindricality is:
A. pre-treatment: a metal titanium implant after the machining fine grinding is provided, and adopts successively acetone, dehydrated alcohol, purified water respectively the ultrasonic cleaning oil removal treatment to be carried out to each 2 times in the surface of metal titanium implant, each five minutes; In order to clean up and oil removing, then dry.
B. sandblasting: adopt 24～70 purpose white fused aluminas to carry out sandblasting to the surface of pretreated metal titanium implant, axial 45 ° of spray gun metal titanium implant, the sandblast time is 8s, blasting pressure is 0.5Mpa, the spray distance is 10cm, sandblast to metal titanium implant surface is uniform grey, makes the metal titanium implant surface form the porous three-dimensional structure, and roughness Ra is 3 μ m; The one-level pit that the pit diameter of vesicular structure is 10～40 μ m, and carry out pure water ultrasonic cleaning, drying;
C. acid etching: the metal titanium implant after sandblasting is soaked in the mixing acid of the hydrochloric acid that sulfuric acid that concentration is 49wt% and concentration are 18wt%, carry out heating in water bath and process 15min at the temperature of 80 ℃, make the metal titanium implant surface form multistage dimple structure, multistage dimple structure have the secondary pit of 2～4 μ m and 1 μ m following three, the level Four pit, then carry out pure water ultrasonic cleaning, drying;
D. splash is processed: adopt the Ar ion sputtering to clean, then adopting pure tantalum is target, magnetron sputtering 20min, magnetron sputtering pressure is 0.4Pa, temperature is 220 ℃, power is 100W, forms one deck by magnetron sputtering on the surface in multistage micro-hole and is less than the thick tantalum coating of 3 μ m, then carries out pure water ultrasonic cleaning 5min;
E. glow discharge is processed: to the metal titanium implant after cleaning carry out that glow discharge is clean, γ ray sterilization, sterile packed.
(embodiment 3)
In the present embodiment, the step of the threaded metal titanium implant of processing cylindricality is:
A. pre-treatment: a metal titanium implant after the machining fine grinding is provided, and adopts successively acetone, dehydrated alcohol, purified water respectively the ultrasonic cleaning oil removal treatment to be carried out to each 2 times in the surface of metal titanium implant, each five minutes; In order to clean up and oil removing, then dry.
B. sandblasting: adopt 24～70 purpose white fused aluminas to carry out sandblasting to the surface of pretreated metal titanium implant, axial 60 ° of spray gun metal titanium implant, the sandblast time is 8s, blasting pressure is 0.4Mpa, the spray distance is 8cm, sandblast to metal titanium implant surface is uniform grey, makes the metal titanium implant surface form the porous three-dimensional structure, and roughness Ra is 4 μ m; The one-level pit that the pit diameter of vesicular structure is 10～40 μ m, and carry out pure water ultrasonic cleaning, drying;
C. acid etching: the metal titanium implant after sandblasting is soaked in the mixing acid of the hydrochloric acid that sulfuric acid that concentration is 56wt% and concentration are 12wt%, carry out heating in water bath and process 10min at the temperature of 70 ℃, make the metal titanium implant surface form multistage dimple structure, multistage dimple structure have the secondary pit of 2～4 μ m and 1 μ m following three, the level Four pit, then carry out pure water ultrasonic cleaning, drying;
D. splash is processed: adopt the Ar ion sputtering to clean, then adopting pure tantalum is target, magnetron sputtering 30min, magnetron sputtering pressure is 0.3Pa, temperature is 300 ℃, power is 100W, forms one deck by magnetron sputtering on the surface in multistage micro-hole and is less than the thick tantalum coating of 3 μ m, then carries out pure water ultrasonic cleaning 5min;
E. glow discharge is processed: to the metal titanium implant after cleaning carry out that glow discharge is clean, γ ray sterilization, sterile packed.
Above-described specific embodiment; purpose of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (7)
1. one kind has multistage dimple structure bioactive metal titanium implant process of surface treatment, it is characterized in that, comprises the following steps:
A. pre-treatment: a metal titanium implant after the machining fine grinding is provided, and adopts successively acetone, dehydrated alcohol, purified water respectively the ultrasonic cleaning oil removal treatment to be carried out in the surface of metal titanium implant, each five minutes, and dry;
B. sandblasting: adopt 24～70 purpose white fused aluminas to carry out sandblasting to the surface of pretreated metal titanium implant, blasting pressure is 0.1～0.6Mpa, sandblast to metal titanium implant surface is uniform grey, make the metal titanium implant surface form the porous three-dimensional structure, and carry out pure water ultrasonic cleaning, drying;
C. acid etching: the metal titanium implant after sandblasting is soaked in the mixing acid of the hydrochloric acid that sulfuric acid that concentration range is 50wt%～75wt% and concentration range are 8wt%～20wt%, carry out the heating in water bath processing at the temperature of 50～80 ℃, make the metal titanium implant surface form multistage dimple structure, and carry out pure water ultrasonic cleaning, drying;
D. splash is processed: adopt the Ar ion sputtering to clean, then adopting pure tantalum is target, forms one deck by magnetron sputtering on the surface in multistage micro-hole and is less than the thick tantalum coating of 3 μ m, and carry out pure water ultrasonic cleaning 5min;
E. glow discharge is processed: to the metal titanium implant after cleaning carry out that glow discharge is clean, γ ray sterilization, sterile packed.
2. according to claim 1 have a multistage dimple structure bioactive metal titanium implant process of surface treatment, and it is characterized in that: in described step a, the ultrasonic cleaning of acetone, dehydrated alcohol, purified water is respectively carried out 2 times.
3. according to claim 1 have a multistage dimple structure bioactive metal titanium implant process of surface treatment, it is characterized in that: in described step b, spray gun in the sandblasting process and metal titanium implant axial 30 °～90 °, spray is apart from being 5～12cm, the sandblast time is 5～15s.
4. according to claim 3 have a multistage dimple structure bioactive metal titanium implant process of surface treatment, it is characterized in that: in described step b, the roughness Ra of the metal titanium implant surface after sandblasting between 2-5 μ m, the one-level pit that the pit diameter of the vesicular structure after sandblasting is 10～40 μ m.
5. according to claim 1 have a multistage dimple structure bioactive metal titanium implant process of surface treatment, and it is characterized in that: in described step c, the time of magnetron sputtering is 20～30min, and temperature is 220～300 ℃, and power is 80～100W.
6. according to claim 5 have a multistage dimple structure bioactive metal titanium implant process of surface treatment, it is characterized in that: in described step c, multistage dimple structure have the secondary pit of 2～4 μ m and 1 μ m following three, the level Four pit.
7. according to claim 1 have a multistage dimple structure bioactive metal titanium implant process of surface treatment, and it is characterized in that: the surface of described metal titanium implant has screw thread, and the metal titanium implant can be the implant of cylindricality or taper.
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Cited By (11)
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| CN103981523A (en) * | 2014-04-28 | 2014-08-13 | 大连大学 | Surface sand-blasting and acid-etching treatment method of super-hydrophilic Ti6Ai7Ni |
| CN104975335A (en) * | 2015-06-04 | 2015-10-14 | 西北有色金属研究院 | Preparation method of composite coating on surface of titanium alloy dental implant |
| CN106492280A (en) * | 2016-11-24 | 2017-03-15 | 北京华钽生物科技开发有限公司 | A kind of anti-infective, rub resistance, the high joint prosthesis product of biocompatibility and its manufacture method |
| CN106729990A (en) * | 2016-12-28 | 2017-05-31 | 上海交通大学医学院附属第九人民医院 | A kind of Novel Titanium surface of promotion Integrated implant and antibacterial ability |
| CN107345300A (en) * | 2017-06-01 | 2017-11-14 | 成都贝施美生物科技有限公司 | Planting body double acid-etching technique |
| CN107447216A (en) * | 2017-08-08 | 2017-12-08 | 江苏创英医疗器械有限公司 | A kind of dental implant surface processing method and equipment |
| CN107557715A (en) * | 2017-07-27 | 2018-01-09 | 芜湖微云机器人有限公司 | Improved bioactive metal titanium implant surface modification technology |
| EP3287150A1 (en) * | 2016-08-22 | 2018-02-28 | WALDEMAR LINK GmbH & Co. KG | Coating for an implant |
| CN114099777A (en) * | 2021-11-19 | 2022-03-01 | 湖南普林特医疗器械有限公司 | Multi-layer active coating for orthopedic implant and preparation method thereof |
| CN114308850A (en) * | 2021-11-29 | 2022-04-12 | 山东优纳贸易有限公司 | Method for processing aseptic bearing used in human body and animal body |
| CN115350324A (en) * | 2022-07-25 | 2022-11-18 | 上海市第六人民医院 | Titanium implant surface graphene coating with high load performance and preparation method and application thereof |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103981523A (en) * | 2014-04-28 | 2014-08-13 | 大连大学 | Surface sand-blasting and acid-etching treatment method of super-hydrophilic Ti6Ai7Ni |
| CN104975335A (en) * | 2015-06-04 | 2015-10-14 | 西北有色金属研究院 | Preparation method of composite coating on surface of titanium alloy dental implant |
| AU2017314997B2 (en) * | 2016-08-22 | 2022-03-10 | Waldemar Link Gmbh & Co. Kg | Coating for an implant |
| US12011354B2 (en) | 2016-08-22 | 2024-06-18 | Waldemar Link Gmbh & Co. Kg | Coating for an implant |
| US11484412B2 (en) | 2016-08-22 | 2022-11-01 | Waldemar Link Gmbh & Co. Kg | Coating for an implant |
| EP3287150A1 (en) * | 2016-08-22 | 2018-02-28 | WALDEMAR LINK GmbH & Co. KG | Coating for an implant |
| WO2018036843A1 (en) * | 2016-08-22 | 2018-03-01 | Waldemar Link Gmbh & Co. Kg | Coating for an implant |
| CN109789240A (en) * | 2016-08-22 | 2019-05-21 | 沃尔德马连接两合公司 | Coating for implantation material |
| CN106492280A (en) * | 2016-11-24 | 2017-03-15 | 北京华钽生物科技开发有限公司 | A kind of anti-infective, rub resistance, the high joint prosthesis product of biocompatibility and its manufacture method |
| CN106729990A (en) * | 2016-12-28 | 2017-05-31 | 上海交通大学医学院附属第九人民医院 | A kind of Novel Titanium surface of promotion Integrated implant and antibacterial ability |
| CN107345300A (en) * | 2017-06-01 | 2017-11-14 | 成都贝施美生物科技有限公司 | Planting body double acid-etching technique |
| CN107557715A (en) * | 2017-07-27 | 2018-01-09 | 芜湖微云机器人有限公司 | Improved bioactive metal titanium implant surface modification technology |
| CN107447216A (en) * | 2017-08-08 | 2017-12-08 | 江苏创英医疗器械有限公司 | A kind of dental implant surface processing method and equipment |
| CN114099777A (en) * | 2021-11-19 | 2022-03-01 | 湖南普林特医疗器械有限公司 | Multi-layer active coating for orthopedic implant and preparation method thereof |
| CN114308850A (en) * | 2021-11-29 | 2022-04-12 | 山东优纳贸易有限公司 | Method for processing aseptic bearing used in human body and animal body |
| CN115350324A (en) * | 2022-07-25 | 2022-11-18 | 上海市第六人民医院 | Titanium implant surface graphene coating with high load performance and preparation method and application thereof |
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Application publication date: 20131218 |