CN109183023A - The preparation method and titanium exemplar of titanium surface porosity layer - Google Patents
The preparation method and titanium exemplar of titanium surface porosity layer Download PDFInfo
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- CN109183023A CN109183023A CN201811130144.3A CN201811130144A CN109183023A CN 109183023 A CN109183023 A CN 109183023A CN 201811130144 A CN201811130144 A CN 201811130144A CN 109183023 A CN109183023 A CN 109183023A
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- 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
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
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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
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
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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
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
- A61L27/306—Other specific inorganic materials not covered by A61L27/303 - A61L27/32
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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
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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
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
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Abstract
The present invention relates to the preparation method of titanium surface porosity layer and titanium exemplars, first prepare slurry, and the target surface for treating coating exemplar carries out grinding process and ultrasonic cleaning；Coating exemplar is treated again carried out cold treatment；Target surface to coating exemplar is impregnated in the slurry, or the slurry is coated on target surface；After the solidification of the slurry of target surface, polishes target surface, then carry out freeze-drying process, remove the non-metallic part of target surface；Then it is sintered, after cooling, successively polishes, cleans, is dry, obtaining porous structure layer.Preparation method of the invention can cover one layer of porous layer with biomimetic features on titanium surface, and hole is changed into long straight hole pattern by general circular hole；This kind of biomimetic porous structure sheaf is applied to titanium alloy bone, can promote the growth of bone tissue and the transmission of body fluid, and the structure of porous material can reduce its whole elasticity modulus, avoid the osteanabrosis as caused by " stress shielding " and corrupted.
Description
Technical field
The present invention relates to the preparation method of titanium surface porosity layer and titanium exemplars, in particular to are applied to biology implantation material
The titanium exemplar of material.
Background technique
Titanium alloy is because elasticity modulus is low, good biocompatibility, mechanical performance and excellent corrosion resistance, it is easy to by human body
Tissue receives, and is widely applied in oral surgery and orthopaedics, due to the structure and elastic surface of titanium alloy and bone tissue shakiness
Fixed, elasticity modulus biomechanical property mismatches, generates abrasive dust and without adverse consequences such as blood supplies.Titanium alloy is made into
Biological implantation material with surface porosity causes the great interest of people, because not only can be with by adjusting porosity
Its intensity and elasticity modulus is set to match with natural bone, and its open-celled structure allows new bone tissue raw into POROUS TITANIUM hole
Long, the interfacial area of such bone and implant greatly increases, in addition the mechanical interlock action between bone and porous surface, can be obvious
Increase implant and bone interface shear strength, implant is made to be fixed together with bone tissue.
The preparation method of titanium alloy surface porous structure mainly has at present: micro-arc oxidation, shot-peening aciding, powder metallurgy
Method, hot spray process etc..The technological means of porous structure made above, can be by adjusting the logical of reasonable state modulator material surface
Cell size and porosity, but be difficult to obtain the pore appearance of similar people's bone stratiform connection, the growth of new bone tissue is influenced, the present invention
Technology by plating the porous layers of one layer of biomimetic features in titanium alloy surface, make the new material of preparation and the structure of natural bone and
Performance is more nearly.
Patent CN102586786A first passes through shot-peening acid etching, then passes through anodic oxidation, in pure titanium sample surface system
The porous layer of standby one layer of classification.The metal surface porous layer of this method preparation, process flow is complicated, the controllable model of surface porosity factor
Enclose relatively narrow, hole pattern is single, the more difficult homogenization of distribution of pores.
First Ti, Al metal powder is uniformly mixed patent CN107385429A by suitable volumes percentage, after dry, is used
The mixed-powder is sprayed on alloy surface by the technique of cold spraying, and alloy aggregate material is immersed in lye later, wherein applying
It upward, is dried after finally taking out, obtains porous layer in layer side.The metal surface porous layer of this method preparation, production
Low efficiency, porosity are influenced by cold spray process, and pore appearance is difficult to control, generally unidirectional through-hole, and distribution of pores is more difficult
One changes.
Patent CN103147111A, CN107460521A directly carries out micro-arc oxidation treatment to titanium alloy surface, obtains micro-
The porous layer of fine pore distribution, but the hole of its porous layer is smaller, connectivity is poor, it is difficult to which suitable cell is grown into, reduction pair
Reparation rate of basic stitch etc..
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides the preparation method and titanium exemplar of a kind of titanium surface porosity layer,
To obtain the porous layer with biomimetic features.
In order to solve the above-mentioned technical problem, technical scheme is as follows:
The preparation method of titanium surface porosity layer, includes the following steps:
S1, slurry is prepared, it is spare；
Wherein, metal powder is contained in the slurry, the metal powder is in suspended state in the slurry；The metal powder packet
Include titanium valve and/or Titanium Powder；
The target surface for treating coating exemplar carries out grinding process, is then cleaned by ultrasonic, spare；
S2, to by S1, treated carried out cold treatment to coating exemplar；
S3, the target surface to coating exemplar that supercooling is disposed is impregnated in the slurry, or the slurry is applied
It is overlying on the target surface to coating exemplar that supercooling is disposed；
S4, after target surface slurry solidification after, polish the target surface of exemplar, then carry out freeze-drying process,
Remove the non-metallic part of target surface；
S5, the exemplar by S5 processing is sintered, after cooling, successively polishes, cleans, is dry, obtains porous structure
Layer.
Further, the slurry includes metal powder and suspension, and wherein suspension includes bonding agent 1-5wt%, de-bubble
Agent 0.1-0.3wt%, suspending agent 2-10wt% and water 84.7-96.9wt%.Preferably, the water is deionized water.Water is as biology
The Main Tissues ingredient of body has preferable biocompatibility, non-toxic to humans, and uses other chemical solutions as solvent,
Such as down alkene, then it may be harmful to the human body.Further, deionized water can effectively avoid the introducing of impurity element, thus high
Pore communication, the structure stability after improving implantation.
Further, the bonding agent is polyvinyl alcohol；The defrother is the fourth tertiary alcohol；The suspending agent is gelatin.
Further, volume fraction is 10-45% to the metal powder in the slurry.The discovery of applicant's repetition test, volume
Score is too low, and the porous layer mechanical performance prepared is poor, easy delamination, and distribution of pores is uneven；Volume fraction is too high, system
Standby porous layer pore appearance out is smaller, and the pore structure of connection is destroyed, it is difficult to realize the good combination with biological tissue, gold
Belong to powder in the slurry volume fraction be 10-45% when, ideal effect can be obtained.
Further, as needed, other metal powders, such as aluminium powder can be added in the slurry.
Further, in S1, the preparation method of slurry are as follows: water, bonding agent and suspending agent are mixed according to the ratio first, added
Metal powder after ball milling 3-9h, after defrother is added, continues ball milling 1-3h, obtains slurry.Ball-milling Time is too short, powder and molten
The undercompounding of agent is allowed to be not easy to be formed uniform pore structure, and Ball-milling Time is too long, reduces working efficiency, may make to starch
Material is contaminated, and the present invention can make metal powder and solvent well-mixed same by the reasonable selection to Ball-milling Time
When, avoid slurry contaminated.
Further, in S1, the target surface to coating exemplar is polishing to 800 or 1000 mesh.
Further, in S2, the temperature for crossing cold treatment is -10 ~ -50 DEG C.Temperature control can be passed through according to different temperatures demand
Sample temperature is adjusted in device.
Further, in S4, during freeze-drying process, controlled at 30 ~ 70 DEG C.
In S4, when polishing, it should be noted that do not destroy the porous appearance structure of structure sheaf；Wherein, non-metallic part refers mainly to starch
The substances such as bonding agent, defrother, suspending agent in material.
Further, in S5, when sintering processes, exemplar is placed under inert atmosphere or vacuum condition, first at 200-500 DEG C
Under the conditions of be sintered 0.5-2h, then be sintered 1-4h under the conditions of 1100-1300 DEG C.In this way, multi-steps sintering, on the one hand can make in sample
Organic matter volatilization it is clean, improve end properties；On the other hand, it is ensured that the stability of sample porous structure；Another further aspect
It can guarantee that sample tissue is in controllable state, avoid the rate of heat addition too fast, caused grain size is uneven, and structural stress is larger etc.
Harm.
Further, in S5, when sintering processes, exemplar is placed under inert atmosphere or vacuum condition, first 10 °C/min
Heating rate be warming up to 200-500 DEG C, be sintered 0.5-2h, then 1100-1300 is warming up to the heating rate of 2 ~ 5 °C/min
DEG C, it is sintered 1-4h.
Titanium exemplar, at least one surface of the titanium exemplar have the porous structure prepared by preparation method as described above
Layer.
The present invention makes the new material and nature of preparation by plating the porous layers of one layer of biomimetic features in titanium alloy surface
The structure and performance of bone are more nearly.
Preparation method through the invention can cover one layer of porous layer with biomimetic features on titanium surface, and hole is by one
As circular hole be changed into long straight hole pattern (see figure 4), penetrate into substrate material surface, and hole spacing-controllable, porosity is adjusted
Range is larger；This kind of biomimetic porous structure sheaf is applied to titanium alloy bone, can promote the growth of bone tissue and the transmission of body fluid, and
The structure of porous material can reduce its whole elasticity modulus, avoid the osteanabrosis as caused by " stress shielding " and corrupted.
The preparation method of titanium surface porosity layer provided by the invention, the ingredient by deploying slurry make titanium valve in solution
In be uniformly dispersed, and uniformly apply and be covered with substrate material surface, subsequent freezing processing can control ice crystal nucleation rate, knot in slurry
Crystalline form state, growth rate reunite the titanium valve in slurry together, later by it so that the growth interface by ice crystal pushes
In ice crystal distil removal, and be sintered, finally obtain porous biomimetic features on titanium surface.Above-mentioned technological means can be former by changing
Material mixes accounting, preparation technology parameter, to a wide range the pore size and porosity of controlled material superficial layer, to adapt to difference
Age bracket and the material of each tissue necrosis position replace.By means of the present invention, the porosity of the porous structure layer on titanium surface
Range between 5 ~ 85%, pore layer spacing range is between 10 ~ 300 μm.
The porous layer of technology preparation through the invention, pore structure is similar with the structure of people's bone, the energy after being implanted into human body
Promote the growth of bone tissue and the transmission of body fluid, while being also beneficial to the dipping of incitant, plays and accelerate organization healing and life
Long effect.
The preparation method of titanium surface porosity layer of the invention, process flow is simple, lower to equipment requirement, can be very fast
Landform changes production capacity in batch.
Detailed description of the invention
Fig. 1 is a kind of preparation method flow chart of titanium surface porosity layer of the invention.
Fig. 2 is the SEM figure of the porous structure layer obtained in embodiment 1.
Fig. 3 is the SEM figure of the porous structure layer obtained in embodiment 2.
Fig. 4 is the illustraton of model of porous structure layer of the invention.
Specific embodiment
Below with reference to embodiment, the present invention will be described in detail.
Embodiment 1
In the present embodiment, titanium surface porosity layer the preparation method is as follows:
Firstly, the exemplar to coating is cleaned up, surface is polishing to 1000 mesh by sand paper, places into ultrasonic wave pond Zhong Chu
Reason；By deionized water and 1wt.% polyvinyl alcohol, the heating stirring in 60 °C of water-baths, until polyvinyl alcohol is completely dissolved,
Then by the titanium valve (D of 30vol.%50=45 μm) it is put into the revolving speed ball milling of 100rpm 6 hours in the mixing tank for fill slurry, so
The two drop tert-butyl alcohols are added, and afterwards with 20rpm low speed ball milling 2 hours, until size performance is uniform everywhere；Exemplar is cooling in liquid nitrogen
To -30 °C, then it is immersed in slurry tank, and adjusting temperature control device makes material temperature be maintained at -25 °C or so, to slurry
Start to take out exemplar after ten minutes in surface solidification；It is put into freeze drying box, at 50 °C, pressure is controlled in 5Pa for temperature control
Left and right is taken out after 12 hours dry；Base sample is sintered, overall process leads to argon gas protection, first with the heating rate of 5 °C/min by
Room temperature rises to 400 °C, keeps the temperature 1h, then proceedes to rise to 1200 °C with the heating rate of 5 °C/min, after keeping the temperature 2h, furnace cooling；
It polishes sintered sample surface, ultrasonic cleaning is finally dried, and porous structure layer is obtained.Sample surfaces are carried out
SEM characterization finds that its hole is long straight hole pattern, such as Fig. 2.
Embodiment 2
In the present embodiment, titanium surface porosity layer the preparation method is as follows:
Firstly, the exemplar to coating is cleaned up, surface is polished by sand paper, is placed into ultrasonic wave pond and is handled；To go from
Then sub- water and 3wt.% polyvinyl alcohol, the heating stirring in 60 °C of water-baths will until polyvinyl alcohol is completely dissolved
Titanium valve (the D of 20vol.%50=45 μm) it is put into the mixing tank for fill slurry with the revolving speed ball milling of 100rpm 6 hours, then it is added
Two drop tert-butyl alcohol defrothers, and with 20rpm low speed ball milling 2 hours, until size performance is uniform everywhere；Exemplar is cooling in liquid nitrogen
To -10 °C, then it is immersed in slurry tank, and adjusting temperature control device makes material temperature be maintained at -5 °C or so, to slurry
Start to take out exemplar after ten minutes in surface solidification；It is put into freeze drying box, at 50 °C, pressure is controlled in 5Pa for temperature control
Left and right is taken out after 12 hours dry；Base sample is sintered, overall process leads to argon gas protection, first with the heating rate of 5 °C/min by
Room temperature rises to 400 °C, keeps the temperature 1h, then proceedes to rise to 1200 °C with the heating rate of 5 °C/min, after keeping the temperature 2h, furnace cooling；
It polishes sintered sample surface, ultrasonic cleaning is dry.SEM characterization is carried out to sample surfaces, it is found that its hole is
Honeycomb, such as Fig. 3.
The content that above-described embodiment illustrates should be understood as that these embodiments are only used for being illustrated more clearly that the present invention, without
For limiting the scope of the invention, after the present invention has been read, those skilled in the art are to various equivalent forms of the invention
Modification each fall within the application range as defined in the appended claims.
Claims (10)
1. the preparation method of titanium surface porosity layer, which comprises the steps of:
S1, slurry is prepared, it is spare；
Wherein, metal powder is contained in the slurry, the metal powder is in suspended state in the slurry；The metal powder packet
Include titanium valve and/or Titanium Powder；
The target surface for treating coating exemplar carries out grinding process, is then cleaned by ultrasonic, spare；
S2, to by S1, treated carried out cold treatment to coating exemplar；
S3, the target surface to coating exemplar that supercooling is disposed is impregnated in the slurry, or the slurry is applied
It is overlying on the target surface to coating exemplar that supercooling is disposed；
S4, after target surface slurry solidification after, polish the target surface of exemplar, then carry out freeze-drying process,
Remove the non-metallic part of target surface；
S5, the exemplar by S5 processing is sintered, after cooling, successively polishes, cleans, is dry, obtains porous structure
Layer.
2. preparation method according to claim 1, which is characterized in that the slurry includes metal powder and suspension,
Middle suspension includes bonding agent 1-5wt%, defrother 0.1-0.3wt%, suspending agent 2-10wt% and water 84.7-96.9wt%.
3. preparation method according to claim 2, which is characterized in that the bonding agent is polyvinyl alcohol；The defrother
For the fourth tertiary alcohol；The suspending agent is gelatin.
4. preparation method according to claim 2, which is characterized in that volume fraction is the metal powder in the slurry
10-45%。
5. preparation method according to claim 2, which is characterized in that in S1, the preparation method of slurry are as follows: first by water and viscous
It connects agent to mix according to the ratio, adds metal powder, after ball milling 3-9h, after defrother is added, continue ball milling 1-3h, obtain slurry.
6. preparation method according to claim 1, which is characterized in that in S1, the target surface to coating exemplar is polished
To 800 or 1000 mesh.
7. preparation method according to claim 1, which is characterized in that in S2, the temperature for crossing cold treatment is -10 ~ -50 DEG C.
8. preparation method according to claim 1, which is characterized in that in S4, during freeze-drying process, control temperature
It is 30 ~ 70 DEG C.
9. preparation method according to claim 1, which is characterized in that in S5, when sintering processes, exemplar is placed in indifferent gas
Under atmosphere or vacuum condition, 0.5-2h is first sintered under the conditions of 200-500 DEG C, then be sintered 1-4h under the conditions of 1100-1300 DEG C.
10. titanium exemplar, which is characterized in that at least one surface of the titanium exemplar has by any one of such as claim 1-9 institute
The porous structure layer for the preparation method preparation stated.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114055910A (en) * | 2021-11-01 | 2022-02-18 | 浙江时空道宇科技有限公司 | Honeycomb plate preparation device and method |
| RU2781873C1 (en) * | 2022-05-05 | 2022-10-19 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Саратовский государственный технический университет имени Гагарина Ю.А." (СГТУ имени Гагарина Ю.А.) | Method for forming metal oxide porous coatings on titanium products |
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| CN104800887A (en) * | 2014-01-24 | 2015-07-29 | 苏州博恩瑞科生物材料有限公司 | Porous titanium coating, titanium-containing multi-coating, preparation method and application thereof |
| CN107115560A (en) * | 2017-06-15 | 2017-09-01 | 中南大学湘雅三医院 | Biomimetic porous titanium implantses of antibacterial and its preparation method and application |
| CN107986811A (en) * | 2017-11-21 | 2018-05-04 | 西安理工大学 | The porous material of a kind of low temperature solidification with reference to obtained by orientation anneal and preparation method thereof |
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2018
- 2018-09-27 CN CN201811130144.3A patent/CN109183023B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104800887A (en) * | 2014-01-24 | 2015-07-29 | 苏州博恩瑞科生物材料有限公司 | Porous titanium coating, titanium-containing multi-coating, preparation method and application thereof |
| CN107115560A (en) * | 2017-06-15 | 2017-09-01 | 中南大学湘雅三医院 | Biomimetic porous titanium implantses of antibacterial and its preparation method and application |
| CN107986811A (en) * | 2017-11-21 | 2018-05-04 | 西安理工大学 | The porous material of a kind of low temperature solidification with reference to obtained by orientation anneal and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114055910A (en) * | 2021-11-01 | 2022-02-18 | 浙江时空道宇科技有限公司 | Honeycomb plate preparation device and method |
| RU2781873C1 (en) * | 2022-05-05 | 2022-10-19 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Саратовский государственный технический университет имени Гагарина Ю.А." (СГТУ имени Гагарина Ю.А.) | Method for forming metal oxide porous coatings on titanium products |
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Address after: 410205 7th floor, building B8, Lugu Enterprise Square, Yuelu District, Changsha City, Hunan Province Patentee after: Aerospace Science and Industry (Changsha) New Materials Research Institute Co.,Ltd. Address before: 410205 7th floor, building B8, Lugu Enterprise Square, Yuelu District, Changsha City, Hunan Province Patentee before: CHANGSHA ADVANCED MATERIALS INDUSTRIAL RESEARCH INSTITUTE Co.,Ltd. |