CN107998445A - A kind of surface modification porous tantalum biomaterial and preparation method thereof - Google Patents
A kind of surface modification porous tantalum biomaterial and preparation method thereof Download PDFInfo
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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
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
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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
- A61L27/32—Phosphorus-containing materials, e.g. apatite
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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
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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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
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/18—Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
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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
- A61L2420/00—Materials or methods for coatings medical devices
- A61L2420/02—Methods for coating medical devices
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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
Abstract
The present invention relates to a kind of surface modification porous tantalum biomaterial and preparation method thereof, belong to biology medical material technical field.The present invention is modified tantalum piece surface using electrochemical anodic oxidation technology, the porous tantalum pentoxide layer of the three-dimensional perforation loose structure with micro/nano-scale has been prepared, pore size is controllable, the arrangement in hole, it is connective good, and hydroxyapatite layer is further constructed in oxidation layer surface, significantly increase protein adsorption, cellular invasion and propagation, improve biocompatibility and osteoconductive, produce the microenvironment for being conducive to cell growth, promote sticking for Human primary osteoblasts, propagation, differentiation and mineralising, bone tissue is promoted to be grown into porous tantalum to form the bone-implant interface of uniqueness, significantly increase stability and function of the implant in bone tissue, accelerate the Integrated implant at bone-implant interface, significantly increase stability of the implant in bone tissue, and there is high corrosion resistance energy, with bright application prospect.
Description
Technical field
The present invention relates to a kind of surface modification porous tantalum biomaterial and preparation method thereof, belong to bio-medical material technology
Field.
Background technology
Biomedical metallic material is a kind of by bio-medical material of the metal or alloy as matrix, also known as surgery use
Metal material or medical metal material, belong to bio-inert material, it is that damage is diagnosed, treated and replaced to organism
Tissue, organ or the material for promoting its function.Common medical metal material mainly includes following several classes：Stainless steel, cobalt-based close
Gold, titanium alloy etc..Relative to traditional metal material, ceramic material, high molecular material etc., bio-medical material development time is not
Long, people are also stranger to it, but bio-medical material research is to health very important meaning.
Porous metal material makes its corrosion behavior be different from conventional dense metal due to its unique loose structure.It is porous
Structure causes the local corrosion of metal, thus the corrosion resistance of porous metals is generally less than congruent dense metal.Surface area
Not influence the single factor of porous metals corrosion rate.Usual crevice corrosion depends on material geometry, and spot corrosion relies on
It is a kind of complicated local corrosion in the corrosion behavior of material composition and structure, thus porous metals implant, corrosion rate is not
It is directly proportional to metal real table area, but the pattern, structure and porosity with hole have close ties.Also scientist points out corruption
It is approximate with porous metals specific surface area directly proportional to lose speed, although the reason is that small and isolated hole surface area is small, easily in hole
Interior delay ion, consumes oxygen, and galvanic interaction occurs；And high porosity, the intercommunicating pore of big opening are conducive to oneself of material
By flowing and carrying out component exchange, spot corrosion and crevice corrosion occurrence probability reduce, and cause local corrosion to mitigate.It is to be understood that
Aperture, the shape in hole, structure and quantity synthesis work corrosion behavior, thus can obtain different porositys to more
Mesoporous metal corrosion resistance influences result.The corrosion resistance of Porous Metals Used as Biomaterials can be improved by appropriate surface treatment
Energy.
Its research not only has important science and theory significance, but also has important application value.It is because biological
Material is from life angle, and lifeless material is changed into the material with certain life property.This is not only material supply section
Major transformation in terms of, and to illustrating the essence to interact between material and living matter, promote the development of life science
Also will play a role in promoting.
The content of the invention
The technical problems to be solved by the invention：The pore size prepared for porous niobium biomaterial is uncontrollable, hole
Arrangement, connective also uncontrollable, multilevel hole material intensity, the problem of toughness is limited, there is provided a kind of surface modification porous tantalum life
Thing material and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of surface modification porous tantalum biomaterial, the biomaterial are heat-treated system using tantalum piece as substrate after anodic oxidation
Into the tantalum piece of nano surface hole array modification, hydroxyapatite coating layer is re-formed.
It is smooth that the tantalum piece need to be polishing to surface through carborundum paper, soaks with corrosive liquid that to remove surface dirty after ultrasonic cleaning
Contaminate thing.
The corrosive liquid is that mass fraction is 40% hydrogen fluoride solution and mass fraction is 98% sulfuric acid solution by volume 1：2
~1：8 mixing.
The anodic oxidation electrochemical treatments are that platinized platinum is cathode using tantalum piece as anode, soak in the electrolytic solution and lead to
Electricity, it is 50 ~ 100mA/cm to control current density2, aoxidize 30 ~ 60min.
The electrolyte is by 10 ~ 20 parts by weight corrosive liquids, 400 ~ 800 parts by weight ethylene glycol, 400 ~ 800 parts by weight deionizations
Water forms.
The heat treatment process is to be warming up to 450 ~ 500 DEG C of 1 ~ 2h of insulation reaction with 5 DEG C/min.
The hydroxyapatite coating layer is that the tantalum piece for modifying nano surface hole array is soaked in sodium hydroxide solution, 60
15 ~ 20h of isothermal holding at ~ 80 DEG C, 1 ~ 2h of heating reaction, is immersed in simulated body fluid after being cooled to room temperature, 36.5 after taking-up
20 ~ 30h is cultivated at DEG C to be made.
The heating reaction process is to be warming up to 300 ~ 350 DEG C of 1 ~ 2h of isothermal holding with 5 DEG C/min.
A kind of preparation method of surface modification porous tantalum biomaterial, concretely comprises the following steps：
（1）Take a diameter of 10 ~ 15mm, thickness is the tantalum piece of 0.3 ~ 0.5mm, smooth, the ultrasound that is polishing to surface with carborundum paper
It is dry after cleaning to pre-process tantalum piece；
（2）By mass fraction be 40% hydrogen fluoride solution and mass fraction is 98% sulfuric acid solution by volume 1：2~1：8 mixing, obtain
Corrosive liquid；
（3）Corrosive liquid, ethylene glycol are taken, adds in deionized water and is uniformly mixed, obtain electrolyte；
（4）Pretreatment tantalum piece is immersed in 1 ~ 3s in corrosive liquid, using tantalum piece as anode after washes clean, platinized platinum is cathode, is soaked
Steep in the electrolytic solution and be powered, it is 50 ~ 100mA/cm to control current density2, drying is washed after aoxidizing 30 ~ 60min, is heat-treated
The tantalum piece of nano surface hole array modification；
（5）In the tantalum piece immersion sodium hydroxide solution that nano surface hole array is modified, at 60 ~ 80 DEG C isothermal holding 15 ~
20h, 1 ~ 2h of heating reaction, is immersed in simulated body fluid after being cooled to room temperature after taking-up, and 20 ~ 30h is cultivated at 36.5 DEG C, obtains table
Porous tantalum biomaterial is modified in face.
Compared with other methods, advantageous effects are the present invention：
The present invention is modified tantalum piece surface using electrochemical anodic oxidation technology, and the three-dimensional with micro/nano-scale has been prepared and has passed through
The porous tantalum pentoxide layer of logical loose structure, pore size is controllable, and hole is arranged, is connective good, and oxidation layer surface into
One step has constructed hydroxyapatite layer, significantly increases protein adsorption, cellular invasion and propagation, improves biocompatibility and bone passes
The property led, produces and is conducive to the microenvironment of cell growth, promote Human primary osteoblasts stick, breed, breaking up and mineralising, promote
Grown into bone tissue into porous tantalum to form the bone-implant interface of uniqueness, it is steady in bone tissue to significantly increase implant
Qualitative and function, accelerates the Integrated implant at bone-implant interface, significantly increases stability of the implant in bone tissue, and have
There is high corrosion resistance energy, there is bright application prospect.
Embodiment
Taking a diameter of 10 ~ 15mm, thickness is the tantalum piece of 0.3 ~ 0.5mm, and it is smooth to be polishing to surface with carborundum paper, then according to
Secondary to be cleaned by ultrasonic 10 ~ 15min with acetone, ethanol, deionized water, washing, which finishes, to be placed in drying box, dry at 50 ~ 60 DEG C
2 ~ 3h, obtains pretreatment tantalum piece, and it is 40% hydrogen fluoride solution to take 10 ~ 20mL mass fractions, and 40 ~ 80mL mass fractions are molten for 98% sulfuric acid
Liquid, is uniformly mixed to obtain corrosive liquid, takes 10 ~ 20g corrosive liquids, and 400 ~ 800g ethylene glycol, adds in 400 ~ 800g deionized waters, with
300 ~ 400r/min stirs 10 ~ 15h, obtains electrolyte, and pretreatment tantalum piece is immersed in 1 ~ 3s in corrosive liquid, deionization is used after taking-up
Water washing to cleaning solution is in neutrality, then using tantalum piece as anode, platinized platinum is cathode, is soaked in the electrolytic solution and is powered, control electricity
Current density is 50 ~ 100mA/cm2, aoxidize to take out after 30 ~ 60min and be washed with deionized to cleaning solution and be in neutrality, then be placed in dry
In dry case, be transferred at 60 ~ 80 DEG C after dry 3 ~ 5h in Muffle furnace, with 5 DEG C/min be warming up to 450 ~ 500 DEG C of insulation reactions 1 ~
2h, be cooled to room temperature nano surface hole array modification tantalum piece, the tantalum piece that nano surface hole array is modified, is immersed in quality
Fraction is that 15 ~ 20h of isothermal holding at 60 ~ 80 DEG C, 300 ~ 350 are warming up to after taking-up with 5 DEG C/min in 2% sodium hydroxide solution
DEG C, 1 ~ 2h of isothermal holding, is immersed in simulated body fluid after being cooled to room temperature, and 20 ~ 30h is cultivated at 36.5 DEG C, obtains surface modification
Porous tantalum biomaterial.
Example 1
Taking a diameter of 10mm, thickness is the tantalum piece of 0.3mm, and it is smooth to be polishing to surface with carborundum paper, then successively with acetone, second
Alcohol, deionized water are cleaned by ultrasonic 10min, and washing, which finishes, to be placed in drying box, and dry 2h, obtains pretreatment tantalum piece at 50 DEG C,
It is 40% hydrogen fluoride solution to take 10mL mass fractions, and 40mL mass fractions are 98% sulfuric acid solution, is uniformly mixed to obtain corrosive liquid, takes
10g corrosive liquids, 400g ethylene glycol, adds in 400g deionized waters, stirs 10h with 300r/min, obtains electrolyte, will pre-process tantalum
Piece is immersed in 1s in corrosive liquid, is washed with deionized to cleaning solution and is in neutrality after taking-up, then using tantalum piece as anode, platinized platinum is
Cathode, soaks in the electrolytic solution and is powered, it is 50mA/cm to control current density2, take out and be washed with deionized water after aoxidizing 30min
Wash to cleaning solution and be in neutrality, then be placed in drying box, be transferred in Muffle furnace after dry 3h at 60 DEG C, be warming up to 5 DEG C/min
450 DEG C of insulation reaction 1h, be cooled to room temperature nano surface hole array modification tantalum piece, the tantalum that nano surface hole array is modified
Piece, is immersed in mass fraction as in 2% sodium hydroxide solution, the isothermal holding 15h at 60 DEG C, is warming up to after taking-up with 5 DEG C/min
300 DEG C, isothermal holding 1h, is immersed in simulated body fluid after being cooled to room temperature, and cultivates 20h at 36.5 DEG C, it is more to obtain surface modification
Hole tantalum biomaterial.
Example 2
Taking a diameter of 13mm, thickness is the tantalum piece of 0.4mm, and it is smooth to be polishing to surface with carborundum paper, then successively with acetone, second
Alcohol, deionized water are cleaned by ultrasonic 13min, and washing, which finishes, to be placed in drying box, and dry 2h, obtains pretreatment tantalum piece at 55 DEG C,
It is 40% hydrogen fluoride solution to take 15mL mass fractions, and 60mL mass fractions are 98% sulfuric acid solution, is uniformly mixed to obtain corrosive liquid, takes
15g corrosive liquids, 600g ethylene glycol, adds in 600g deionized waters, stirs 13h with 350r/min, obtains electrolyte, will pre-process tantalum
Piece is immersed in 2s in corrosive liquid, is washed with deionized to cleaning solution and is in neutrality after taking-up, then using tantalum piece as anode, platinized platinum is
Cathode, soaks in the electrolytic solution and is powered, it is 75mA/cm to control current density2, take out and be washed with deionized water after aoxidizing 45min
Wash to cleaning solution and be in neutrality, then be placed in drying box, be transferred in Muffle furnace after dry 4h at 70 DEG C, be warming up to 5 DEG C/min
475 DEG C of insulation reaction 1h, be cooled to room temperature nano surface hole array modification tantalum piece, the tantalum that nano surface hole array is modified
Piece, is immersed in mass fraction as in 2% sodium hydroxide solution, the isothermal holding 17h at 70 DEG C, is warming up to after taking-up with 5 DEG C/min
325 DEG C, isothermal holding 1h, is immersed in simulated body fluid after being cooled to room temperature, and cultivates 25h at 36.5 DEG C, it is more to obtain surface modification
Hole tantalum biomaterial.
Example 3
Taking a diameter of 15mm, thickness is the tantalum piece of 0.5mm, and it is smooth to be polishing to surface with carborundum paper, then successively with acetone, second
Alcohol, deionized water are cleaned by ultrasonic 15min, and washing, which finishes, to be placed in drying box, and dry 3h, obtains pretreatment tantalum piece at 60 DEG C,
It is 40% hydrogen fluoride solution to take 20mL mass fractions, and 80mL mass fractions are 98% sulfuric acid solution, is uniformly mixed to obtain corrosive liquid, takes
20g corrosive liquids, 800g ethylene glycol, adds in 800g deionized waters, stirs 15h with 400r/min, obtains electrolyte, will pre-process tantalum
Piece is immersed in 3s in corrosive liquid, is washed with deionized to cleaning solution and is in neutrality after taking-up, then using tantalum piece as anode, platinized platinum is
Cathode, soaks in the electrolytic solution and is powered, it is 100mA/cm to control current density2, take out and be washed with deionized water after aoxidizing 60min
Wash to cleaning solution and be in neutrality, then be placed in drying box, be transferred in Muffle furnace after dry 5h at 80 DEG C, be warming up to 5 DEG C/min
500 DEG C of insulation reaction 2h, be cooled to room temperature nano surface hole array modification tantalum piece, the tantalum that nano surface hole array is modified
Piece, is immersed in mass fraction as in 2% sodium hydroxide solution, the isothermal holding 20h at 80 DEG C, is warming up to after taking-up with 5 DEG C/min
350 DEG C, isothermal holding 2h, is immersed in simulated body fluid after being cooled to room temperature, and cultivates 30h at 36.5 DEG C, it is more to obtain surface modification
Hole tantalum biomaterial.
Surface modification porous tantalum biomaterial prepared by the present invention and the porous tantalum biomaterial of Beijing company production
It is detected, specific testing result such as following table table 1：
1 surface modification porous tantalum biomaterial performance of table characterizes
The surface modification porous tantalum biomaterial that as shown in Table 1 prepared by the present invention, porosity is high, and compression strength is high, elasticity modulus
Yield strength is high, and intervertebral fusion rate is fabulous, effectively facilitates the growth of bone tissue, has bright application prospect.
Claims (9)
1. a kind of surface modification porous tantalum biomaterial, it is characterised in that the biomaterial is using tantalum piece as substrate, through anodic oxygen
The tantalum piece of nano surface hole array modification is made in heat treatment after change, re-forms hydroxyapatite coating layer.
2. a kind of surface modification porous tantalum biomaterial as claimed in claim 1, it is characterised in that the tantalum piece need to be through carbonization
It is smooth that silica sand paper is polishing to surface, is soaked after ultrasonic cleaning with corrosive liquid and removes surface contaminant.
3. a kind of surface modification porous tantalum biomaterial as claimed in claim 2, it is characterised in that the corrosive liquid is quality
Fraction is 40% hydrogen fluoride solution and mass fraction is 98% sulfuric acid solution by volume 1：2~1：8 mixing.
A kind of 4. surface modification porous tantalum biomaterial as claimed in claim 1, it is characterised in that the anodic oxidation electrification
It is that platinized platinum is cathode using tantalum piece as anode to learn processing, and immersion in the electrolytic solution and is powered, control current density be 50 ~
100mA/cm2, aoxidize 30 ~ 60min.
A kind of 5. surface modification porous tantalum biomaterial as claimed in claim 4, it is characterised in that the electrolyte by 10 ~
20 parts by weight corrosive liquids, 400 ~ 800 parts by weight ethylene glycol, 400 ~ 800 parts by weight of deionized water composition.
6. a kind of surface modification porous tantalum biomaterial as claimed in claim 1, it is characterised in that the heat treatment process is
450 ~ 500 DEG C of 1 ~ 2h of insulation reaction are warming up to 5 DEG C/min.
A kind of 7. surface modification porous tantalum biomaterial as claimed in claim 1, it is characterised in that the hydroxyapatite coat
Layer is that the tantalum piece for modifying nano surface hole array is soaked in sodium hydroxide solution, and 15 ~ 20h of isothermal holding, takes at 60 ~ 80 DEG C
1 ~ 2h of heating reaction, is immersed in simulated body fluid after being cooled to room temperature after going out, and 20 ~ 30h is cultivated at 36.5 DEG C and is made.
A kind of 8. surface modification porous tantalum biomaterial as claimed in claim 5, it is characterised in that the heating reaction process
To be warming up to 300 ~ 350 DEG C of 1 ~ 2h of isothermal holding with 5 DEG C/min.
9. a kind of preparation method of surface modification porous tantalum biomaterial as described in claim 1 ~ 8 any one, its feature
It is, concretely comprises the following steps：
（1）Take a diameter of 10 ~ 15mm, thickness is the tantalum piece of 0.3 ~ 0.5mm, smooth, the ultrasound that is polishing to surface with carborundum paper
It is dry after cleaning to pre-process tantalum piece；
（2）By mass fraction be 40% hydrogen fluoride solution and mass fraction is 98% sulfuric acid solution by volume 1：2~1：8 mixing, obtain
Corrosive liquid；
（3）Corrosive liquid, ethylene glycol are taken, adds in deionized water and is uniformly mixed, obtain electrolyte；
（4）Pretreatment tantalum piece is immersed in 1 ~ 3s in corrosive liquid, using tantalum piece as anode after washes clean, platinized platinum is cathode, is soaked
Steep in the electrolytic solution and be powered, it is 50 ~ 100mA/cm to control current density2, drying is washed after aoxidizing 30 ~ 60min, is heat-treated
The tantalum piece of nano surface hole array modification；
（5）In the tantalum piece immersion sodium hydroxide solution that nano surface hole array is modified, at 60 ~ 80 DEG C isothermal holding 15 ~
20h, 1 ~ 2h of heating reaction, is immersed in simulated body fluid after being cooled to room temperature after taking-up, and 20 ~ 30h is cultivated at 36.5 DEG C, obtains table
Porous tantalum biomaterial is modified in face.
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