CN105648498A - Method for preparing copper-loaded microporous nano antibacterial bio-coating on surface of medical titanium-based metal - Google Patents
Method for preparing copper-loaded microporous nano antibacterial bio-coating on surface of medical titanium-based metal Download PDFInfo
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- CN105648498A CN105648498A CN201610088197.8A CN201610088197A CN105648498A CN 105648498 A CN105648498 A CN 105648498A CN 201610088197 A CN201610088197 A CN 201610088197A CN 105648498 A CN105648498 A CN 105648498A
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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
- C25D11/024—Anodisation under pulsed or modulated current or potential
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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
- A61L27/54—Biologically active materials, e.g. therapeutic substances
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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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- 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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
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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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Abstract
The invention relates to a method for preparing a copper containing biological ceramic film on the surface of medical titanium-based metal through a micro-arc oxidation technology. The method comprises the steps that firstly, a copper containing electrolyte is prepared; and then the titanium-based metal serves as an anode, stainless steel serves as a cathode, plasma pulse high-energy electro discharge treatment is carried out in the previously prepared copper containing electrolyte by controlling pulse voltage, frequencies, the duty ratio and other micro-arc oxidation parameters, and a copper-loaded microporous nano antibacterial bio-coating closely combined with a base body can be generated on the surface of the titanium-based metal. By means of forming of the biological ceramic film, the antibacterial biological activity of the medical titanium-based metal is obviously improved, and the defects and shortcomings of the medical titanium-based metal serving as a biomedical material are effectively overcome. The raw materials adopted in the method are environment-friendly and free of toxicity and pollution. A preparation process is simple, and operation is convenient. The production efficiency is high, and the method is suitable for industrial production.
Description
Art
The preparation method that the present invention relates to the copper-loaded porous nano antibacterial biological coating of medical titanium based metal surfaces, this bioactive ceramics film not only has excellent mechanical property, and make medical titanium Base Metal have antibacterial biological coating, it is particularly well-suited to the surface modification of bone tissue restoration or alternate material.
Background technology
Fast development along with economic society, the sclerous tissues's damage caused by wound, infection or tumor etc. is increasing, the raising of living standards of the people simultaneously, people are more and more higher to the requirement of hard tissue repair and substitution material, and these factors force research worker to seek outward appearance and the more superior biomaterial of performance.
Infection is biomaterial graft failure main cause in vivo, also it is the biggest problem of puzzlement Clinical Surgery doctor, this is wherein both relevant with the misoperation in operation, also change with embedded material position local environment, affect microbial growth, add the probability that antibacterial infects, therefore, if biomaterial itself is provided with antibacterial biological coating, not only can reduce implantation body's inflammation to occur, improve the biological activity of embedded material, shorten bone healing time, enter postoperative organization healing, improve the success rate of operation, alleviate patient's burden in spirit and material, and effectively overcome the series of problems that antibiotic a large amount of use causes.
Copper is one of mineral-type long acting antibiotic biological coating material of being employed the earliest, obtains extensive use because having good environment compatibility and antibacterial biological coating persistency. Copper-bearing antibacterial biological coating material is primarily referred to as to load to copper ion prepares antibacterial biological coating material on carrier, in recent years, the research about copper antibacterial biological coating performance causes concern gradually.
Tradition hard tissue substituting and internal fixation material such as stainless steel and other metal materials wearability and poor biocompatibility, easily aging, and also elastic modelling quantity is big, is easily generated " stress shielding ", causes osteoporosis and fracture delayed union, limits its clinical practice; And the macromolecular materials such as polylactic acid are poor due to mechanical strength and abrasion resistance properties, it is difficult to bear bigger heavy burden;Although ceramic material such as silicon carbide ceramics has excellent anti-wear performance, but the mechanical property of itself is too poor, it is easy to chipping. Titanium and titanium-based metal are current one of most widely used embedded materials clinically, its relative density is little, mechanical strength is high, corrosion-resistant and anti-fatigue performance is good, but titanium and alloy material thereof are " biologically inert " material, biological activity is poor, lack bone inductive effect, and to be absent from surrounding tissue that strong chemical is combined be field of planting one of unsolved difficult problem always, also many problems are brought, such as fracture delayed union, Aseptic Loosening etc. implanting in human body.
In view of traditional biological surface treatment technology of material such as plasma spraying and electrochemical deposition etc., to there is the bond strength of coating and matrix low, the problems such as coating uniformity and the more difficult control of stability, and differential arc oxidization technique has high-efficiency environment friendly, easy to operate, coating and substrate combinating strength are high, the advantages such as the porous ceramics coating material containing required function element can be formed by high temperature sintering and discharge breakdown effect at coating surface, therefore the present invention mainly adopts differential arc oxidization technique to process titanium-based metal, it is effectively improved the bond strength of coating and matrix, obtain the bioceramic film with high-efficiency antimicrobial biological coating performance simultaneously.
Summary of the invention
The invention aims to solve existing titanium-based metal surface by micro-arc oxidation prepare in the method for copper-loaded porous nano antibacterial biological coating and need titanium-based metal is carried out pretreatment, complex process, cost are high, and the problem that the coating obtained is low with substrate combinating strength. The invention provides a kind of method preparing copper-loaded porous nano antibacterial biological coating at medical titanium based metal surfaces.
The present invention medical titanium based metal surfaces prepare copper-loaded porous nano antibacterial biological coating method through the following steps that realize: one, medical titanium Base Metal is sequentially carried out deoxidation film, oil removal treatment; Two, the sodium hydroxide of the preparation copper gluconate of electrolyte: 0.5-2g/L, 2-8g/L, the sodium hexameta phosphate of 3-10g/L, 1-3g/L sodium citrate, solvent is deionized water; Three, the medical titanium Base Metal after processing with step one is for anode, fix with fixture in the electrolyte immersing step 2 configuration, stainless steel electrolytic liquid bath is negative electrode, adopt the pulse power, arranging electrical quantity is: pulse voltage 200-500V, pulse frequency 100-600Hz, dutycycle are 10-30%, carry out differential arc oxidation 5-30min, be namely prepared into copper-loaded porous nano antibacterial biological coating on titanium-based metal surface.
In the electrolyte of step 2 of the present invention, sodium hexameta phosphate can also replace with sodium phosphate, and the mass concentration of sodium polyphosphate is 2-10g/L.
In the electrolyte of step 2, sodium hexameta phosphate can also replace with sodium polyphosphate, and the mass concentration of sodium phosphate is 5-12g/L.
The present invention adopts constant current mode to carry out differential arc oxidation, and voltage change range is 200-500V.
Present invention process flow process is simple, by choosing suitable bath composition and respective concentration, control differential arc oxidation relevant parameter, the preparation of copper-loaded porous nano antibacterial biological coating can be achieved at medical titanium based metal surfaces, it it is a kind of metallurgical binding between this coating and substrate, there is stronger adhesion, the present invention not only increases corrosion resistance and the biocompatibility of medical titanium Base Metal, the more important thing is and make medical titanium Base Metal possess antibacterial biological coating biology activity, promote the combination of medical titanium Base Metal embedded material and osseous tissue, this coating and matrix have higher bond strength, expand the range of application of medical titanium Base Metal.
Accompanying drawing explanation
Fig. 1 is the SEM picture of the copper-loaded porous nano antibacterial biological coating prepared on titanium-based metal surface in detailed description of the invention one.
Detailed description of the invention
Technical solution of the present invention is not limited to act detailed description of the invention set forth below, also includes the combination in any between each detailed description of the invention.
Detailed description of the invention one: present embodiment medical titanium based metal surfaces prepare copper-loaded porous nano antibacterial biological coating method through the following steps that realize: one, medical titanium Base Metal is sequentially carried out deoxidation film, oil removal treatment; Two, the sodium hydroxide of the preparation copper gluconate of electrolyte: 0.5-2g/L, 2-8g/L, the sodium hexameta phosphate of 3-10g/L, 1-3g/L sodium citrate, solvent is deionized water; Three, the medical titanium Base Metal after processing with step one is for anode, fix with fixture in the electrolyte immersing step 2 configuration, stainless steel electrolytic liquid bath is negative electrode, adopt the pulse power, arranging electrical quantity is: pulse voltage 200-500V, pulse frequency 100-600Hz, dutycycle are 10-30%, carry out differential arc oxidation 5-30min, be namely prepared into copper-loaded porous nano antibacterial biological coating on titanium-based metal surface.
In present embodiment, bath composition material is analytical pure, commercially available prod.
Present embodiment adopts constant current mode to carry out differential arc oxidation, and voltage change range is 200-500V.
Detailed description of the invention two: present embodiment and detailed description of the invention one are the difference is that the sodium hydroxide preparing the copper gluconate of electrolyte: 1-2g/L, 3-6g/L in step 2, the sodium hexameta phosphate of 5-8g/L, 2-3g/L sodium citrate, solvent is deionized water, and other step and parameter and detailed description of the invention one are identical.
Detailed description of the invention three: present embodiment and detailed description of the invention one or two are the difference is that the sodium hydroxide preparing the copper gluconate of electrolyte: 2g/L, 5g/L in step 2, the sodium hexameta phosphate of 6g/L, 2g/L sodium citrate, solvent is deionized water, and other step and parameter and detailed description of the invention one are identical.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three the difference is that arranging electrical quantity in step 3 be: pulse frequency 300-400Hz, dutycycle are 15-25%, and other step and one of parameter and detailed description of the invention one to three are identical.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four the difference is that arranging electrical quantity in step 3 be: pulse frequency 350Hz, dutycycle are 20%, and other step and one of parameter and detailed description of the invention one to three are identical.
Detailed description of the invention six: present embodiment and one of detailed description of the invention one to six are the difference is that carrying out differential arc oxidation 10-20min in step 3. Other step and one of parameter and detailed description of the invention one to five are identical.
Detailed description of the invention seven: present embodiment and one of detailed description of the invention one to six are the difference is that carrying out differential arc oxidation 15min in step 3. Other step and one of parameter and detailed description of the invention one to five are identical.
Detailed description of the invention eight: one of present embodiment and detailed description of the invention one to seven the difference is that the electrolyte of step 2 configuration be: the copper gluconate of 0.5-2g/L, 2-8g/L sodium hydroxide, the sodium phosphate of 2-10g/L, 1-3g/L sodium citrate, solvent is deionized water. Other step and one of parameter and detailed description of the invention one to seven are identical.
Detailed description of the invention nine: the electrolyte that present embodiment and detailed description of the invention eight configure the difference is that step 2 is: the copper gluconate of 1-2g/L, 3-6g/L sodium hydroxide, the sodium phosphate of 5-8g/L, 2-3g/L sodium citrate, solvent is deionized water.Other step and parameter are with to be embodied as eight identical.
Detailed description of the invention ten: the electrolyte that present embodiment and detailed description of the invention eight configure the difference is that step 2 is: the copper gluconate of 1g/L, 5g/L sodium hydroxide, the sodium phosphate of 6g/L, 3g/L sodium citrate, solvent is deionized water. Other step and parameter are with to be embodied as eight identical.
Detailed description of the invention 11: one of present embodiment and detailed description of the invention one to seven the difference is that the electrolyte of step 2 configuration be: the copper gluconate of 0.5-2g/L, 2-8g/L sodium hydroxide, the sodium polyphosphate of 5-12g/L, 1-3g/L sodium citrate. Other step and one of parameter and detailed description of the invention one to seven are identical.
Detailed description of the invention 12: the electrolyte that present embodiment and detailed description of the invention 11 configure the difference is that step 2 is: the copper gluconate of 1-2g/L, 3-7g/L sodium hydroxide, the sodium polyphosphate of 8-10g/L, 2-3g/L sodium citrate, solvent is deionized water. Other step and parameter and detailed description of the invention 11 are identical.
Detailed description of the invention 13: present embodiment be embodied as 11 the difference is that step 2 configuration electrolyte be: the copper gluconate of 2g/L, 5g/L sodium hydroxide, the sodium polyphosphate of 9g/L, 2g/L sodium citrate, solvent is deionized water. Other step and parameter and detailed description of the invention 11 are identical.
Claims (3)
1. the preparation method of the copper-loaded porous nano antibacterial biological coating of medical titanium based metal surfaces, it is characterised in that directly prepare the method for copper-loaded porous nano antibacterial biological coating at medical titanium based metal surfaces through the following steps that realize:, medical titanium Base Metal is sequentially carried out deoxidation film, oil removal treatment; Two, the sodium hydroxide of the preparation copper gluconate of electrolyte: 0.5-2g/L, 2-8g/L, the sodium hexameta phosphate of 3-10g/L, 1-3g/L sodium citrate, solvent is deionized water; Three, the medical titanium Base Metal after processing with step one is for anode, fix with fixture in the electrolyte immersing step 2 configuration, stainless steel electrolytic liquid bath is negative electrode, adopt the pulse power, arranging electrical quantity is: pulse voltage 200-500V, pulse frequency 100-600Hz, dutycycle are 10-30%, carry out differential arc oxidation 5-30min, be namely prepared into copper-loaded porous nano antibacterial biological coating on titanium-based metal surface.
2. the preparation method of the copper-loaded porous nano antibacterial biological coating of medical titanium based metal surfaces according to claim 1, it is characterized in that the electrolyte that step 2 configures is: the copper gluconate of 0.5-2g/L, 2-8g/L sodium hydroxide, the sodium phosphate of 2-10g/L, 1-3g/L sodium citrate, solvent is deionized water.
3. the preparation method of the copper-loaded porous nano antibacterial biological coating of medical titanium based metal surfaces according to claim 1, it is characterized in that the electrolyte that step 2 configures is: the copper gluconate of 0.5-2g/L, 2-8g/L sodium hydroxide, the sodium polyphosphate of 5-12g/L, 1-3g/L sodium citrate, solvent is deionized water.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110565144A (en) * | 2018-11-01 | 2019-12-13 | 赵全明 | Porous biological ceramic coating with antibacterial and bone-promoting functions and preparation method and application thereof |
CN112962132A (en) * | 2021-02-02 | 2021-06-15 | 山东省科学院新材料研究所 | Magnesium alloy ultrahigh-porosity micro-arc oxidation coating and preparation method and application thereof |
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CN101899700A (en) * | 2009-05-25 | 2010-12-01 | 佳木斯大学 | Preparation method of ultrasonic microarc oxidation silver-carrying antibiotic bioactive coating on magnesium and titanium surface |
CN103526261A (en) * | 2013-10-17 | 2014-01-22 | 赵全明 | Preparation method of zinc-containing micro-arc oxidation electrolyte and zinc-containing biological ceramic membrane |
CN104195617A (en) * | 2014-09-18 | 2014-12-10 | 赵全明 | Method for preparing zinc oxide antibacterial biological film on surface of medical titanium alloy |
CN104264204A (en) * | 2014-09-29 | 2015-01-07 | 赵全明 | Method for directly preparing micro-arc oxidation ceramic membrane containing zinc oxide on surface of magnesium alloy |
CN104674321A (en) * | 2013-11-29 | 2015-06-03 | 中国科学院金属研究所 | Preparation method and application of antibacterial bio-ceramic film with titanium or titanium alloy surface containing copper |
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- 2016-02-17 CN CN201610088197.8A patent/CN105648498A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101899700A (en) * | 2009-05-25 | 2010-12-01 | 佳木斯大学 | Preparation method of ultrasonic microarc oxidation silver-carrying antibiotic bioactive coating on magnesium and titanium surface |
CN103526261A (en) * | 2013-10-17 | 2014-01-22 | 赵全明 | Preparation method of zinc-containing micro-arc oxidation electrolyte and zinc-containing biological ceramic membrane |
CN104674321A (en) * | 2013-11-29 | 2015-06-03 | 中国科学院金属研究所 | Preparation method and application of antibacterial bio-ceramic film with titanium or titanium alloy surface containing copper |
CN104195617A (en) * | 2014-09-18 | 2014-12-10 | 赵全明 | Method for preparing zinc oxide antibacterial biological film on surface of medical titanium alloy |
CN104264204A (en) * | 2014-09-29 | 2015-01-07 | 赵全明 | Method for directly preparing micro-arc oxidation ceramic membrane containing zinc oxide on surface of magnesium alloy |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110565144A (en) * | 2018-11-01 | 2019-12-13 | 赵全明 | Porous biological ceramic coating with antibacterial and bone-promoting functions and preparation method and application thereof |
CN112962132A (en) * | 2021-02-02 | 2021-06-15 | 山东省科学院新材料研究所 | Magnesium alloy ultrahigh-porosity micro-arc oxidation coating and preparation method and application thereof |
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