CN109106982A - A kind of preparation method of titanium aluminium base hydroxyl apatite biological painting - Google Patents

A kind of preparation method of titanium aluminium base hydroxyl apatite biological painting Download PDF

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Publication number
CN109106982A
CN109106982A CN201811017839.0A CN201811017839A CN109106982A CN 109106982 A CN109106982 A CN 109106982A CN 201811017839 A CN201811017839 A CN 201811017839A CN 109106982 A CN109106982 A CN 109106982A
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Prior art keywords
titanium
aluminium
hydroxyl apatite
aluminium base
base hydroxyl
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CN201811017839.0A
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Chinese (zh)
Inventor
陈伟
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Zhangjiagang City Fook New Mstar Technology Ltd
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Zhangjiagang City Fook New Mstar Technology Ltd
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Priority to CN201811017839.0A priority Critical patent/CN109106982A/en
Publication of CN109106982A publication Critical patent/CN109106982A/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/28Materials for coating prostheses
    • A61L27/30Inorganic materials
    • A61L27/306Other specific inorganic materials not covered by A61L27/303 - A61L27/32
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/28Materials for coating prostheses
    • A61L27/30Inorganic materials
    • A61L27/32Phosphorus-containing materials, e.g. apatite
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C24/00Coating starting from inorganic powder
    • C23C24/08Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/082Coating starting from inorganic powder by application of heat or pressure and heat without intermediate formation of a liquid in the layer
    • C23C24/085Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
    • C23C24/087Coating with metal alloys or metal elements only
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00Electrolytic coating other than with metals
    • C25D9/04Electrolytic coating other than with metals with inorganic materials
    • C25D9/08Electrolytic coating other than with metals with inorganic materials by cathodic processes
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2420/00Materials or methods for coatings medical devices
    • A61L2420/02Methods for coating medical devices
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2420/00Materials or methods for coatings medical devices
    • A61L2420/06Coatings containing a mixture of two or more compounds

Abstract

The invention discloses a kind of preparation methods of titanium aluminium base hydroxyl apatite biological painting, it include: (1) by mass ratio is that 5~15:25~35:1 aluminium powder, dehydrated alcohol, sodium alginate are uniformly mixed, 2~4h of ball milling, gained slurry is mixed with dehydrated alcohol according to volume ratio 1:2~4,3~5h of ultrasonic disperse obtains aluminium powder suspension;(2) under 400~500 DEG C of inert atmosphere conditions, by the way of thermal spraying, by above-mentioned aluminium powder suspension spray in pretreated titanium sheet, obtain the titanium sheet containing aluminium layer, wherein the aluminium layer with a thickness of 0.5~1.5mm;(3) 0.1~1mol/L calcium nitrate solution and 0.01~0.1mol/L phosphoric acid solution are mixed, sodium hydroxide is used to adjust the pH value of mixed solution as 4~5, it is anode by cathode, graphite of the titanium sheet containing aluminium layer, 30~50min of electro-deposition under certain condition obtains titanium aluminium base hydroxyl apatite biological painting.The titanium aluminium base hydroxyl apatite biological painting that method in the present invention is prepared is well combined with matrix, has preferable bioactivity.

Description

A kind of preparation method of titanium aluminium base hydroxyl apatite biological painting
Technical field
The present invention relates to field of material technology, more particularly to a kind of preparation side of titanium aluminium base hydroxyl apatite biological painting Method.
Background technique
With the development of modern material technology of preparing, biomaterial because have body tissue is repaired, substitute with again Raw property has become one of the focus of current field of biomedicine research.Biological hard tissue substitute material is earliest It using body bone, Animal Bone, developed to later using stainless steel and high molecule plastic, since there are dissolveds, corrosion and tired for stainless steel Labor problem, plastics have that stability difference and intensity are low.Therefore the bottleneck for causing biomaterial to develop, bioceramic go out It is existing, the deficiency of existing alternative materials is improved, because of its many advantages, bioceramic is provided with vast potential for future development.
Hydroxyapatite HA is identical as the inanimate matter material composition of human body hard tissue (bone and tooth), can be direct after implanting With bon e formation synostosis, interface bond strength meets or exceeds the intensity of bone and implant itself between bone, but due to Simple HA crystal brittleness is big, flexural strength is low, is not suitable for being used as the biggish hard tissue repair of carrying and substitution.Therefore, metal The research of base coating material is come into being.
For hydroxyapatite coating layer prosthese at present in wide clinical application, existing coat preparing technology has plasma spraying, Ion beam deposition, Laser cladding, discharge plasma sintering, coatingSintering process etc..But as clinic overhauls the increasing of case It is more, also show that some drawbacks, such as the bond strength deficiency between coating and metallic matrix.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of preparation method of titanium aluminium base hydroxyl apatite biological painting, It is able to solve problems of the prior art.
Summary of the invention
It is existing to overcome the purpose of the present invention is to provide a kind of preparation method of titanium aluminium base hydroxyl apatite biological painting Deficiency in technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of titanium aluminium base hydroxyl apatite biological painting, comprising:
(1) be 5~15:25~35:1 aluminium powder by mass ratio, dehydrated alcohol, sodium alginate are uniformly mixed, ball milling 2~ 4h, gained slurry are mixed with dehydrated alcohol according to volume ratio 1:2~4, and 3~5h of ultrasonic disperse obtains aluminium powder suspension;
(2) under 400~500 DEG C of inert atmosphere conditions, by the way of thermal spraying, by above-mentioned aluminium powder suspension spray In pretreated titanium sheet, obtain the titanium sheet containing aluminium layer, wherein the aluminium layer with a thickness of 0.5~1.5mm;
(3) 0.1~1mol/L calcium nitrate solution and 0.01~0.1mol/L phosphoric acid solution are mixed, using sodium hydroxide tune The pH value for saving mixed solution is 4~5, is anode by cathode, graphite of the titanium sheet containing aluminium layer, under certain condition electro-deposition 30 ~50min obtains titanium aluminium base hydroxyl apatite biological painting.
Preferably, in step (1), the aluminium powder, the dehydrated alcohol, the sodium alginate mass ratio be 10:30:1.
Preferably, in step (1), ultrasonic power is 800~1200W.
Preferably, in step (2), the pressure in thermal spray process is 0.2~0.6MPa, and temperature is 300~500 DEG C, spray Away from for 10~20mm.
Preferably, in step (2), the inert atmosphere is nitrogen atmosphere or argon atmosphere.
Preferably, in step (3), certain condition is 20~30 DEG C of temperature, 1~5mA/cm of current density2, constant current it is heavy Product.
Compared with the prior art, the advantages of the present invention are as follows: the titanium aluminium base hydroxyl phosphorus that the method in the present invention is prepared Lime stone biological coating is well combined with matrix, has preferable bioactivity.
Specific embodiment
The present invention is described further by the following example: according to following embodiments, the present invention may be better understood. However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of titanium aluminium base hydroxyl apatite biological painting, comprising:
(1) be 5~15:25~35:1 aluminium powder by mass ratio, dehydrated alcohol, sodium alginate are uniformly mixed, ball milling 2~ 4h, gained slurry are mixed with dehydrated alcohol according to volume ratio 1:2~4, and 3~5h of ultrasonic disperse obtains aluminium powder suspension;
(2) under 400~500 DEG C of inert atmosphere conditions, by the way of thermal spraying, by above-mentioned aluminium powder suspension spray In pretreated titanium sheet, obtain the titanium sheet containing aluminium layer, wherein the aluminium layer with a thickness of 0.5~1.5mm;
(3) 0.1~1mol/L calcium nitrate solution and 0.01~0.1mol/L phosphoric acid solution are mixed, using sodium hydroxide tune The pH value for saving mixed solution is 4~5, is anode by cathode, graphite of the titanium sheet containing aluminium layer, under certain condition electro-deposition 30 ~50min obtains titanium aluminium base hydroxyl apatite biological painting.
Wherein, in above-mentioned steps (1), the aluminium powder, the dehydrated alcohol, the sodium alginate mass ratio be 10:30: 1;Ultrasonic power is 800~1200W, it is preferred that ultrasonic power 1000W.
Wherein, in above-mentioned steps (2), the pressure in thermal spray process is 0.2~0.6MPa, and temperature is 300~500 DEG C, Spray is away from being 10~20mm, it is preferred that pressure 0.4MPa, temperature are 400 DEG C, are sprayed away from for 15mm;The inert atmosphere is nitrogen Atmosphere or argon atmosphere.
Wherein, in above-mentioned steps (3), certain condition is 20~30 DEG C of temperature, 1~5mA/cm of current density2, constant current it is heavy Product, it is preferred that 25 DEG C of temperature, current density 3mA/cm2
Following preparation methods that titanium aluminium base hydroxyl apatite biological painting in the present invention is illustrated with specifically embodiment.
Embodiment 1
(1) by mass ratio be 5:25:1 aluminium powder, dehydrated alcohol, sodium alginate be uniformly mixed, ball milling 2h, gained slurry with Dehydrated alcohol is mixed according to volume ratio 1:2, and ultrasonic disperse 3h obtains aluminium powder suspension;
(2) under the conditions of 400 DEG C of argon atmosphere, by the way of thermal spraying, by above-mentioned aluminium powder suspension spray pre- In processed titanium sheet, the titanium sheet containing aluminium layer is obtained, wherein the pressure with a thickness of 0.5mm, in thermal spray process of the aluminium layer Power is 0.2MPa, and temperature is 300 DEG C, and spray is away from for 10mm;
(3) 0.1mol/L calcium nitrate solution and 0.01mol/L phosphoric acid solution are mixed, it is molten to adjust mixing using sodium hydroxide The pH value of liquid be 4, be anode by cathode, graphite of the titanium sheet containing aluminium layer, temperature be 20 DEG C, current density 1mA/cm2、 Constant current electro-deposition 30min obtains titanium aluminium base hydroxyl apatite biological painting.
Embodiment 2
(1) aluminium powder, dehydrated alcohol, sodium alginate of mass ratio 10:30:1 are uniformly mixed, ball milling 3h, gained slurry with Dehydrated alcohol is mixed according to volume ratio 1:3, and ultrasonic disperse 4h obtains aluminium powder suspension;
(2) under the conditions of 450 DEG C of argon atmosphere, by the way of thermal spraying, by above-mentioned aluminium powder suspension spray pre- In processed titanium sheet, the titanium sheet containing aluminium layer is obtained, wherein the pressure with a thickness of 1mm, in thermal spray process of the aluminium layer For 0.4MPa, temperature is 400 DEG C, and spray is away from for 15mm;
(3) 0.5mol/L calcium nitrate solution and 0.05mol/L phosphoric acid solution are mixed, it is molten to adjust mixing using sodium hydroxide The pH value of liquid be 4.5, be anode by cathode, graphite of the titanium sheet containing aluminium layer, temperature be 25 DEG C, current density 3mA/ cm2, constant current electro-deposition 40min, obtain titanium aluminium base hydroxyl apatite biological painting.
Embodiment 3
(1) aluminium powder, dehydrated alcohol, sodium alginate that mass ratio is 15:35:1 are uniformly mixed, ball milling 4h, gained slurry It is mixed with dehydrated alcohol according to volume ratio 1:4, ultrasonic disperse 5h obtains aluminium powder suspension;
(2) under the conditions of 500 DEG C of argon atmosphere, by the way of thermal spraying, by above-mentioned aluminium powder suspension spray pre- In processed titanium sheet, the titanium sheet containing aluminium layer is obtained, wherein the pressure with a thickness of 1.5mm, in thermal spray process of the aluminium layer Power is 0.6MPa, and temperature is 500 DEG C, and spray is away from for 20mm;
(3) 1mol/L calcium nitrate solution and 0.1mol/L phosphoric acid solution are mixed, mixed solution is adjusted using sodium hydroxide PH value be 5, be anode by cathode, graphite of the titanium sheet containing aluminium layer, temperature be 30 DEG C, current density 5mA/cm2, it is permanent Electric current electro-deposition 50min obtains titanium aluminium base hydroxyl apatite biological painting.
The titanium aluminium base hydroxyl apatite biological painting that method in the present invention is prepared is well combined with matrix, have compared with Good bioactivity.The titanium aluminium base hydroxyl apatite biological painting intensity that method in the present invention is prepared is tough up to 58MPa Property is up to 0.92MPam1/2
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive Property include so that include a series of elements process, method, article or equipment not only include those elements, but also Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic Element.

Claims (6)

1. a kind of preparation method of titanium aluminium base hydroxyl apatite biological painting characterized by comprising
(1) be 5~15:25~35:1 aluminium powder by mass ratio, dehydrated alcohol, sodium alginate are uniformly mixed, 2~4h of ball milling, institute It obtains slurry to be mixed with dehydrated alcohol according to volume ratio 1:2~4,3~5h of ultrasonic disperse obtains aluminium powder suspension;
(2) under 400~500 DEG C of inert atmosphere conditions, by the way of thermal spraying, by above-mentioned aluminium powder suspension spray pre- In processed titanium sheet, obtain the titanium sheet containing aluminium layer, wherein the aluminium layer with a thickness of 0.5~1.5mm;
(3) 0.1~1mol/L calcium nitrate solution and 0.01~0.1mol/L phosphoric acid solution are mixed, is adjusted using sodium hydroxide mixed The pH value for closing solution is 4~5, is anode by cathode, graphite of the titanium sheet containing aluminium layer, electro-deposition under certain condition 30~ 50min obtains titanium aluminium base hydroxyl apatite biological painting.
2. the preparation method of titanium aluminium base hydroxyl apatite biological painting according to claim 1, which is characterized in that step (1) in, the aluminium powder, the dehydrated alcohol, the sodium alginate mass ratio be 10:30:1.
3. the preparation method of titanium aluminium base hydroxyl apatite biological painting according to claim 1, which is characterized in that step (1) in, ultrasonic power is 800~1200W.
4. the preparation method of titanium aluminium base hydroxyl apatite biological painting according to claim 1, which is characterized in that step (2) in, pressure in thermal spray process is 0.2~0.6MPa, and temperature is 300~500 DEG C, and spray is away from for 10~20mm.
5. the preparation method of titanium aluminium base hydroxyl apatite biological painting according to claim 1, which is characterized in that step (2) in, the inert atmosphere is nitrogen atmosphere or argon atmosphere.
6. the preparation method of titanium aluminium base hydroxyl apatite biological painting according to claim 1, which is characterized in that step (3) in, certain condition is 20~30 DEG C of temperature, 1~5mA/cm of current density2, galvanostatic deposition.
CN201811017839.0A 2018-09-02 2018-09-02 A kind of preparation method of titanium aluminium base hydroxyl apatite biological painting Withdrawn CN109106982A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2125333A1 (en) * 1994-06-07 1995-12-08 Robert D. Klassen Method for converting a coating of brushite to hydroxyapatite
CN101411892A (en) * 2007-10-19 2009-04-22 中国科学院金属研究所 Method for preparing hydroxylapatite/polylactic acid composite biological coating on surface of magnesium alloy
CN102501444A (en) * 2011-10-08 2012-06-20 山东大学 Titanium dioxide nanotube array-carbon nanotube-hydroxyapatite biological composite coating and preparation thereof
CN102631704A (en) * 2012-04-20 2012-08-15 中原工学院 Titanium-aluminium based hydroxyapatite coating and preparation method thereof
CN102631705A (en) * 2012-04-27 2012-08-15 中南大学 Lanthanum-doped hydroxyapatite compound coating and preparation method thereof
CN103014801A (en) * 2011-09-20 2013-04-03 天津市玄真生物医药科技发展有限公司 Electrodeposition preparation method for biomedical titanium base hydroxyapatite composite material
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Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2125333A1 (en) * 1994-06-07 1995-12-08 Robert D. Klassen Method for converting a coating of brushite to hydroxyapatite
CN101411892A (en) * 2007-10-19 2009-04-22 中国科学院金属研究所 Method for preparing hydroxylapatite/polylactic acid composite biological coating on surface of magnesium alloy
CN103014801A (en) * 2011-09-20 2013-04-03 天津市玄真生物医药科技发展有限公司 Electrodeposition preparation method for biomedical titanium base hydroxyapatite composite material
CN102501444A (en) * 2011-10-08 2012-06-20 山东大学 Titanium dioxide nanotube array-carbon nanotube-hydroxyapatite biological composite coating and preparation thereof
CN102631704A (en) * 2012-04-20 2012-08-15 中原工学院 Titanium-aluminium based hydroxyapatite coating and preparation method thereof
CN102631705A (en) * 2012-04-27 2012-08-15 中南大学 Lanthanum-doped hydroxyapatite compound coating and preparation method thereof
CN104651897A (en) * 2013-11-18 2015-05-27 南京理工大学 Method for preparing bioactive composite coating on surfaces of titanium and its alloy

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Application publication date: 20190101