CN105780088A - Preparation method of TiO2 antibacterial coating layer on medical stainless steel surface - Google Patents

Preparation method of TiO2 antibacterial coating layer on medical stainless steel surface Download PDF

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Publication number
CN105780088A
CN105780088A CN201610171057.7A CN201610171057A CN105780088A CN 105780088 A CN105780088 A CN 105780088A CN 201610171057 A CN201610171057 A CN 201610171057A CN 105780088 A CN105780088 A CN 105780088A
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CN
China
Prior art keywords
stainless steel
tio
medical stainless
coating
minutes
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Pending
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CN201610171057.7A
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Chinese (zh)
Inventor
张磊
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张磊
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Priority to CN201610171057.7A priority Critical patent/CN105780088A/en
Publication of CN105780088A publication Critical patent/CN105780088A/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
    • A61L31/00Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/08Materials for coatings
    • A61L31/082Inorganic materials
    • A61L31/088Other specific inorganic materials not covered by A61L31/084 or A61L31/086
    • 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
    • A61L31/00Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/14Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/34Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
    • 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
    • A61L2420/00Materials or methods for coatings medical devices
    • A61L2420/02Methods for coating medical devices

Abstract

The invention relates to a preparation method of a TiO2 antibacterial coating layer on a medical stainless steel surface. A container for accommodating anodic oxidation solution is put in a water bath pot for stirring; stainless steel is put in; an anode is connected for electrifying; the voltage rises; after the voltage is kept, the electricity is cut off to take out a titanium alloy; and the titanium alloy is thermally treated to obtain the TiO2 antibacterial coating layer with a surface area of 40-80 m2/g. The anodic oxidation solution consists of 0.01-6% of NaH2PO4, 0.05-6% of HClO4, 0.01-3% of AgNO3, 0.5-3% of nanometer TiO2 particles and the balance of water. The preparation method adopts a sand blasting surface treatment process to largely increase the surface area of the stainless steel to improve the sterilization efficiency, and uses electromagnetic stirring and ultrasonic stirring for improving a stirring effect to effectively and uniformly disperse the components of the solution so as to prepare the TiO2 antibacterial coating layer with high specific surface area.

Description

Medical stainless steel surface TiO2Method for preparing antibiotic coating
Technical field
The present invention relates to a kind of TiO for technical field of metal2Coating production, particularly A kind of medical stainless steel antibacterial surface coating production.
Background technology
Nano-TiO2Coating is due to the light transfer characteristic of its uniqueness, high catalysis activity, high chemistry surely Qualitative, the feature such as nontoxic, it is widely used to sewage disposal, air cleaning and photovoltaic solar cells The field such as exploitation.
Metal surface coated with nano TiO2The method of coating mainly have anodic oxidation, plasma spraying, colloidal sol- Gel etc..
At medical field, the TiO of titanium alloy implant surfaces2Coating is to be prepared by anodizing, this Coating prepared by technique and matrix have good adhesion.Stainless steel is due to its good shaping, resistance to With etc. performance extensively apply the nail of medical field, operation tray etc..As one can be prepared on its surface Layer has the TiO of good interface adhesion2Coating, will the function such as, anti-infection antibacterial for equipment surfaces Realize significant.
Through the literature search of prior art is found: Zalnezhad etc. are at " Ceramic International " Vol.14:P2785~2793, the article " TiO that 2015 deliver2nanotube Coating on stainless steel 304for biomedical applications ", article describe head First pass through physical vaporous deposition at 304 stainless steel surfaces sedimentary Titaniums, subsequently titanium is carried out sun Pole aoxidizes to obtain nano-TiO2The method of pipe.Although surface adhesion can be prepared by the method Good TiO2Nanotube, in place of there is also some shortcomings in addition to preparation cost height, due to TiO2Receive Mitron mutually relies on, and the effective surface area that can receive illumination is on the low side, causes the germicidal efficiency on its surface On the low side.
Summary of the invention
The present invention is directed to above-mentioned deficiency of the prior art, it is provided that a kind of stainless steel with high-specific surface area Antibacterial surface coating production so that TiO2The specific surface area of coating is 40-80m2/ g, to enter one Step improves TiO2Germicidal efficiency.
The present invention is achieved by the following technical solutions, and the present invention is by straight for surface treated stainless steel Connect anodic oxidation, comprise the following steps:
The first step, puts in water-bath by the container filling anodic oxidation solution, starts stirring;
Described anodic oxidation solution, its composition weight percent content is: NaH2PO40.01~6%, HClO40.05~6%, AgNO30.01~3%, nano-TiO2Particle 0.5~3%, remaining is water;
Described water-bath, its temperature is in the range of 5 DEG C~10 DEG C.
Described stirring, its mode is electromagnetic agitation, ultrasonic agitation.Described nanoparticle size 5~ In the range of 20nm.
Second step, puts into anodic oxidation solution by the stainless steel after surface treated, is energized after connecing anode, After voltage rises to required voltage, after keeping voltage a period of time, stainless steel is taken out in power-off;
Described surface processes, and its method is sand-blast.
Described voltage is 5V~80V, and pressure rising time is 5 seconds~2 minutes.
Described holding voltage time is 5 minutes~60 minutes.
3rd step, cools down after being processed by stainless steel hot, and i.e. obtaining surface area is 40-80m2The TiO of/g2 Antimicrobial coating.
Described heat treatment temperature is 350 DEG C~550 DEG C, and heat treatment time is 60 minutes~180 minutes.
Described cooling, its mode is air cooling.
Compared with other technique, the present invention, by direct for surface treated stainless steel anodic oxidation, adopts Stainless surface area can be greatly increased with process of surface treatment, improve germicidal efficiency;Electromagnetism is utilized to stir Mix, ultrasonic agitation can improve stirring efficiency, makes the composition of solution effectively evenly disperse, and preparation is provided There is the TiO of high-specific surface area2Coating, its specific surface area is 40-80m2/g。
Detailed description of the invention
Below embodiments of the invention are elaborated: the present embodiment with technical solution of the present invention is being Implement under premise, give detailed embodiment and concrete operating process, but the present invention Protection domain is not limited to following embodiment.
Embodiment 1
Preparing matrix is 304 stainless high-specific surface area TiO2Sterilization coating, preparation process is as follows:
NaH will be filled2PO40.01%, HClO46%, AgNO33%, 20nm-TiO2Particle 0.5% The beaker of anodic oxidation solution put into the water-bath that solution temperature is 10 DEG C, start electromagnetic agitation; Corrosion resistant plate after blasting treatment is put into and connects anode and be stepped up voltage, by voltage liter after 2 minutes To 80V, keep voltage after 5 minutes, to take out corrosion resistant plate, dried corrosion resistant plate is carried out at heat Reason, heat treatment temperature is 550 DEG C, and the time is 60 minutes, i.e. obtains high-specific surface area TiO after air cooling2 Antimicrobial coating.Prepared catalysis material is carried out specific surface area test, and specific surface area is 40m2/g。
Embodiment 2
Preparing matrix is 316 stainless high-specific surface area TiO2Sterilization coating, preparation process is as follows:
NaH will be filled2PO46%, HClO40.01%, AgNO30.01%, 15nm-TiO2Particle The water-bath that temperature is 5 DEG C put into by the beaker of the anodic oxidation solution of 2%, starts ultrasonic agitation;Will Corrosion resistant plate after blasting treatment is put into and is connect anode and be stepped up voltage, is risen to by voltage after 5 seconds 45V, keeps voltage to take out corrosion resistant plate after 30 minutes, is heat-treated by dried corrosion resistant plate, Heat treatment temperature is 450 DEG C, and the time is 120 minutes, i.e. obtains high-specific surface area TiO after air cooling2 Antimicrobial coating.Prepared catalysis material is carried out specific surface area test, and specific surface area is 60m2/g。
Embodiment 3
Preparing matrix is 316 stainless high-specific surface area TiO2Sterilization coating, preparation process is as follows:
NaH will be filled2PO43%, HClO43%, AgNO31%, 5nm-TiO2Particle 3% The water-bath that temperature is 8 DEG C put into by the beaker of anodic oxidation solution, starts ultrasonic agitation;Will be through overspray Corrosion resistant plate after sand processes is put into and is connect anode and be stepped up voltage, after 60 seconds, voltage is risen to 5V, Keep voltage after 60 minutes, to take out corrosion resistant plate, dried corrosion resistant plate is heat-treated, at heat Reason temperature is 350 DEG C, and the time is 180 minutes, i.e. obtains high-specific surface area TiO after air cooling2Antibacterial Coating.Prepared catalysis material is carried out specific surface area test, and specific surface area is 80m2/g。

Claims (11)

1. a medical stainless steel surface TiO2Method for preparing antibiotic coating, it is characterised in that include with Lower step:
The first step, puts in water-bath by the container filling anodic oxidation solution, starts stirring;
Described anodic oxidation solution, its composition weight percent content is: NaH2PO40.01~6%, HClO40.05~6%, AgNO30.01~3%, nano-TiO2Particle 0.5~3%, remaining is water;
Second step, puts into anodic oxidation solution by the stainless steel after surface treated, is energized after connecing anode, Boost in voltage, after keeping voltage, titanium alloy is taken out in power-off;
3rd step, cools down after being processed by stainless steel hot, and i.e. obtaining surface area is 40-80m2The TiO of/g2 Antimicrobial coating.
Medical stainless steel surface TiO the most according to claim 12Method for preparing antibiotic coating, It is characterized in that, in the first step, described water-bath, its temperature is in the range of 5 DEG C~10 DEG C.
Medical stainless steel surface TiO the most according to claim 1 and 22Antimicrobial coating preparation side Method, is characterized in that, in the first step, described stirring, its mode is electromagnetic agitation or ultrasonic agitation.
Medical stainless steel surface TiO the most according to claim 1 and 22Antimicrobial coating preparation side Method, is characterized in that, in the first step, described nano particle, its size is in the range of 5~20nm.
Medical stainless steel surface TiO the most according to claim 12Method for preparing antibiotic coating, It is characterized in that, in second step, described surface processes, and its method is sand-blast.
Medical stainless steel surface TiO the most according to claim 1 or 52Antimicrobial coating preparation side Method, is characterized in that, in second step, described voltage is 5V~80V.
Medical stainless steel surface TiO the most according to claim 1 or 52Antimicrobial coating preparation side Method, is characterized in that, in second step, pressure rising time is 5 seconds~2 minutes.
Medical stainless steel surface TiO the most according to claim 1 or 52Antimicrobial coating preparation side Method, is characterized in that, in second step, described holding voltage time is 5 minutes~60 minutes.
Medical stainless steel surface TiO the most according to claim 12Method for preparing antibiotic coating, It is characterized in that, in the 3rd step, described heat treatment temperature is 350 DEG C~550 DEG C.
10. according to the medical stainless steel surface TiO described in claim 1 or 92Antimicrobial coating preparation side Method, is characterized in that, in the 3rd step, described heat treatment time is 60 minutes~180 minutes.
11. according to the medical stainless steel surface TiO described in claim 1 or 92Antimicrobial coating preparation side Method, is characterized in that, in the 3rd step, described cooling, its mode is air cooling.
CN201610171057.7A 2016-03-15 2016-03-15 Preparation method of TiO2 antibacterial coating layer on medical stainless steel surface Pending CN105780088A (en)

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Application Number Priority Date Filing Date Title
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CN105780088A true CN105780088A (en) 2016-07-20

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108060446A (en) * 2017-12-14 2018-05-22 马鞍山新徽铝业有限公司 A kind of electrolysis treatment fluid
CN111647926A (en) * 2020-05-14 2020-09-11 东南大学 Preparation method of antibacterial aluminum alloy by anodic oxidation

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103290417A (en) * 2013-05-22 2013-09-11 太原理工大学 Preparation method of titanium dioxide (TiO2) nanotube film on stainless steel surface

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103290417A (en) * 2013-05-22 2013-09-11 太原理工大学 Preparation method of titanium dioxide (TiO2) nanotube film on stainless steel surface

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
詹玮婷: "不锈钢表面微、纳米薄膜的制备及光催化和抗菌性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108060446A (en) * 2017-12-14 2018-05-22 马鞍山新徽铝业有限公司 A kind of electrolysis treatment fluid
CN111647926A (en) * 2020-05-14 2020-09-11 东南大学 Preparation method of antibacterial aluminum alloy by anodic oxidation

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Application publication date: 20160720

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