CN108815581B - Preparation method of double-nano hydroxyapatite/titanium composite gradient coating - Google Patents
Preparation method of double-nano hydroxyapatite/titanium composite gradient coating Download PDFInfo
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- CN108815581B CN108815581B CN201810702628.4A CN201810702628A CN108815581B CN 108815581 B CN108815581 B CN 108815581B CN 201810702628 A CN201810702628 A CN 201810702628A CN 108815581 B CN108815581 B CN 108815581B
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052588 hydroxylapatite Inorganic materials 0.000 title claims abstract description 53
- 239000010936 titanium Substances 0.000 title claims abstract description 51
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 51
- 239000011248 coating agent Substances 0.000 title claims abstract description 50
- 238000000576 coating method Methods 0.000 title claims abstract description 50
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 title claims abstract description 48
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 27
- 239000002245 particle Substances 0.000 claims abstract description 23
- 238000010288 cold spraying Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000005516 engineering process Methods 0.000 claims abstract description 9
- 229910000883 Ti6Al4V Inorganic materials 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000005488 sandblasting Methods 0.000 claims description 4
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 3
- 229910052586 apatite Inorganic materials 0.000 claims description 2
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 claims description 2
- 238000007788 roughening Methods 0.000 claims 1
- 238000007873 sieving Methods 0.000 claims 1
- 239000011159 matrix material Substances 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000002054 transplantation Methods 0.000 abstract description 2
- 238000005507 spraying Methods 0.000 description 16
- 239000007789 gas Substances 0.000 description 12
- 238000000151 deposition Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 210000001519 tissue Anatomy 0.000 description 5
- 239000007921 spray Substances 0.000 description 4
- 238000005336 cracking Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 238000001659 ion-beam spectroscopy Methods 0.000 description 2
- 238000004372 laser cladding Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000011664 nicotinic acid Substances 0.000 description 2
- 238000007750 plasma spraying Methods 0.000 description 2
- 230000008439 repair process Effects 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 2
- 238000005452 bending Methods 0.000 description 1
- 239000003462 bioceramic Substances 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010290 vacuum plasma spraying Methods 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/56—Porous materials, e.g. foams or sponges
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
- A61L27/306—Other specific inorganic materials not covered by A61L27/303 - A61L27/32
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
- A61L27/32—Phosphorus-containing materials, e.g. apatite
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/12—Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Medicinal Chemistry (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Transplantation (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Veterinary Medicine (AREA)
- Dermatology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
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- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
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- Other Surface Treatments For Metallic Materials (AREA)
Abstract
本发明公开了一种双纳米羟基磷灰石/钛复合梯度涂层的制备方法，包括如下步骤：将纳米结构的羟基磷灰石与钛粉末在惰性气体保护下通过机械球磨制备羟基磷灰石含量在30vol.％～70vol.％的羟基磷灰石/钛复合粉末，筛分，收集粒径在10～30μm的羟基磷灰石/钛复合粉末；对Ti6Al4V基体进行喷砂粗化处理，采用冷喷涂技术在基体材料表面沉积一层厚度为50～100μm的微米多孔钛涂层；然后在多孔钛涂层表面采用冷喷涂技术制备羟基磷灰石/钛复合涂层。本发明可实现相结构和成分移植，有利于控制粒子间结合，提高层间结合，所制备的涂层致密性好，且操作简单、成本较低，特别适用于工业应用推广。The invention discloses a preparation method of a double nano-hydroxyapatite/titanium composite gradient coating, comprising the following steps: preparing the hydroxyapatite by mechanical ball milling of nano-structured hydroxyapatite and titanium powder under the protection of inert gas Hydroxyapatite/titanium composite powder with a content of 30vol.%～70vol.%, sieve, and collect the hydroxyapatite/titanium composite powder with a particle size of 10～30μm; the Ti6Al4V matrix is sandblasted and roughened, using A layer of micro-porous titanium coating with a thickness of 50-100 μm is deposited on the surface of the base material by cold spraying technology; then a hydroxyapatite/titanium composite coating is prepared on the surface of the porous titanium coating by cold spraying technology. The invention can realize phase structure and component transplantation, is beneficial to control the bonding between particles and improve the bonding between layers, the prepared coating has good compactness, simple operation and low cost, and is especially suitable for industrial application promotion.
Description
Technical Field
The invention relates to the field of coating preparation, in particular to a preparation method of a double nano hydroxyapatite/titanium composite gradient coating.
Background
The hard tissue transplant material is a composite structure of human organ repair materials and needs to have good biological performance and certain toughness. Hydroxyapatite is often used as a biological coating material for metal surfaces such as titanium alloy and the like due to good biological properties, however, pure hydroxyapatite has the problems of poor mechanical properties, low fracture toughness and bending strength, structural change of components caused by high temperature influence in the preparation process, low bonding strength caused by mismatch of thermal expansion coefficients of the pure hydroxyapatite and a metal substrate, stress cracking and the like, so that the development of coating components, structural design and preparation technology is needed, the generation of phase change, tissue change and harmful phases in the coating formation process is inhibited, the performance difference is alleviated, the residual stress is reduced, the interface bonding of the coating is enhanced, and the regulation and control of the coating tissue structure and the mechanical properties are realized. Meanwhile, researches show that compared with common hydroxyapatite, the nano hydroxyapatite has better adsorption performance and biocompatibility and is very similar to the hydroxyapatite in human bones and teeth in structure and crystal form.
The main methods for preparing the bioceramic coating at present include a bionic method, an ion beam sputtering method, a sol-gel method, a laser cladding method, an electrochemical deposition method, a plasma spraying method and the like. The bionic method and the ion beam sputtering method can realize the component control of the deposited coating, but the process parameters are not easy to control, and the bonding strength of the coating and the metal matrix interface is low. The sol-gel method has the problems of deposition efficiency and influence on the bonding strength and structural integrity of the coating due to shrinkage cracking during drying. The electrochemical deposition has the problems that the component structure of the coating is sensitive to the deposition conditions such as the temperature of electrolyte and the like, the bonding strength is low and sintering cracking occurs. The laser cladding has the problems of high-temperature decomposition and harmful generation of hydroxyapatite and the like. Plasma spraying is a common method for preparing biological ceramic coatings such as hydroxyapatite and the like, vacuum plasma spraying is applied to preparation of a repair biological apatite coating, but the problems of phase change, brittle fracture and the like are easy to occur in a high-temperature process, and the coating with a surface nano structure is not easy to prepare.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a double nano hydroxyapatite/titanium composite gradient coating, which can realize phase structure and component transplantation, is beneficial to controlling the combination among particles and improving the combination among layers, has good compactness of the prepared coating, simple operation and lower cost, and is particularly suitable for industrial application and popularization.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a double nano hydroxyapatite/titanium composite gradient coating comprises the following steps:
s1, preparing hydroxyapatite/titanium composite powder with the hydroxyapatite content of 30-70 vol.% by mechanically ball milling the nanostructured hydroxyapatite and titanium powder under the protection of inert gas (pure argon), wherein the particle size of the hydroxyapatite is 10-20 nm, and the particle size of the titanium particles is 20-40 nm;
s2, screening the obtained hydroxyapatite/titanium composite powder, and collecting the hydroxyapatite/titanium composite powder with the particle size of 10-30 microns;
s3, carrying out sand blasting and coarsening pretreatment on a base material, wherein the base material is Ti6Al4V titanium alloy;
s4, depositing a layer of micron porous titanium coating with the thickness of 50-100 mu m on the surface of the pretreated base material by a cold spraying technology;
s5, depositing the hydroxyapatite/titanium composite powder collected in the step S2 on the surface of the porous micron titanium coating by a cold spraying technology to form a hydroxyapatite/titanium composite coating with the thickness of 50-150 microns, wherein the powder feeding amount is 100-150 g/min.
Further, the particle size of the hydroxyapatite/titanium composite powder in the step S1 is controllable.
Furthermore, hydroxyapatite and titanium particles in the hydroxyapatite/titanium composite coating are both nano-structure powder.
The invention has the following beneficial effects:
according to the invention, a porous micron titanium coating is deposited between the hydroxyapatite/titanium composite coating and the substrate through cold spraying, so that the interlayer binding force is improved;
the invention transplants the phase structure and the components of the powder into the coating through the cold spraying technology, inhibits the growth of the nano-crystalline grains and avoids the decomposition or phase change phenomenon caused by the high temperature, thereby improving the bioactivity and the stability of the coating.
The coating prepared by the method has the advantages of good compactness, simple operation and lower cost, and is particularly suitable for industrial application and popularization.
Detailed Description
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described in detail below with reference to examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Hydroxyapatite powder with the particle size of 10nm and titanium powder with the particle size of 20nm are selected and mechanically ball-milled under the protection of inert gas (pure argon gas) to prepare hydroxyapatite/titanium composite powder with the volume fraction of nano hydroxyapatite of 30 vol.%, wherein the ball-material ratio is 15: 1, the rotating speed is 150rpm, and the ball-milling time is 6 hours; carrying out sand blasting and coarsening treatment on a Ti6Al4V matrix, and then depositing a porous micron titanium coating with the thickness of about 100 microns on the surface of the Ti6Al4V matrix by adopting a cold spraying system, wherein the spraying powder adopts micron titanium particles with the particle size of-200 meshes, and the spraying gas adopts N2The accelerating gas pressure is 2.0MPa, the powder feeding gas pressure is 2.2MPa, the spraying temperature is 250 ℃, the spraying distance is 10mm, and the moving speed of a spray gun is 100 mm/s; then preparing a hydroxyapatite/titanium composite coating on the surface of the porous titanium coating by adopting a cold spraying technology, wherein the thickness of the coating is 50 mu m, and N is adopted as spraying gas2The accelerating gas pressure is 1.6MPa, the powder feeding pressure is 1.8MPa, the spraying temperature is 300 ℃, the spraying distance is 10mm, and the moving speed of the spray gun is 5 mm/s.
The X-ray diffraction analysis shows that the phase structure and the tissue structure of the hydroxyapatite/titanium composite gradient coating are the same as those of the original spraying powder.
Example 2
Hydroxyapatite powder with the particle size of 20nm and titanium powder with the particle size of 30nm are selected to prepare hydroxyapatite/titanium composite powder with the volume fraction of nano hydroxyapatite of 70 vol.% by mechanical ball milling under the protection of inert gas (pure argon), wherein the ball-to-material ratio is 15: 1, the rotating speed is 150rpm, and the ball milling time is 6 hours; carrying out sand blasting and coarsening treatment on a Ti6Al4V matrix, and then depositing a porous micron titanium coating with the thickness of about 100 microns on the surface of the Ti6Al4V matrix by adopting a cold spraying system, wherein the spraying powder adopts micron titanium particles with the particle size of-200 meshes, and the spraying gas adopts N2The accelerating gas pressure is 1.8MPa, the powder feeding gas pressure is 2.0MPa, the spraying temperature is 350 ℃, the spraying distance is 10mm, and the moving speed of a spray gun is 100 mm/s; then preparing hydroxyapatite/titanium on the surface of the porous titanium coating by adopting a cold spraying technologyThe thickness of the composite coating is 50 mu m, and N is adopted as spraying gas2The accelerating gas pressure is 2.0MPa, the powder feeding gas pressure is 2.2MPa, the spraying temperature is 400 ℃, the spraying distance is 10mm, and the moving speed of the spray gun is 10 mm/s.
The X-ray diffraction analysis shows that the phase structure and the tissue structure of the hydroxyapatite/titanium composite gradient coating are the same as those of the original spraying powder.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (4)
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| CN113304314A (en) * | 2021-05-26 | 2021-08-27 | 西安交通大学第二附属医院 | Porous polyether-ether-ketone-based coating material and preparation method thereof |
| CN114949355B (en) * | 2022-04-12 | 2023-05-23 | 宁波大学 | Ossicle and cartilage integrated auditory ossicle implant and manufacturing method thereof |
| CN116024562A (en) * | 2023-01-16 | 2023-04-28 | 西安建筑科技大学 | A kind of human bone implant and its preparation method |
| CN117862515B (en) * | 2024-03-13 | 2024-06-18 | 江苏威拉里新材料科技有限公司 | A method for preparing titanium alloy composite powder for denture coating |
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| CN105018924A (en) * | 2014-11-14 | 2015-11-04 | 中国兵器工业第五二研究所 | Preparation method of hydroxylapatite coating on surface of titanium alloy matrix |
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