CN110284171A - A kind of preparation method of metal surface antimicrobial coating - Google Patents

A kind of preparation method of metal surface antimicrobial coating Download PDF

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Publication number
CN110284171A
CN110284171A CN201910641898.3A CN201910641898A CN110284171A CN 110284171 A CN110284171 A CN 110284171A CN 201910641898 A CN201910641898 A CN 201910641898A CN 110284171 A CN110284171 A CN 110284171A
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CN
China
Prior art keywords
preparation
metal surface
iodine
antimicrobial coating
coating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910641898.3A
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Chinese (zh)
Inventor
王万明
韩雪松
杨秀
陈能阜
肖杰
黄少斌
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ninth Oo Hospital Of Joint Logistics Support Force Of Chinese People's Liberation Army
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Ninth Oo Hospital Of Joint Logistics Support Force Of Chinese People's Liberation Army
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Application filed by Ninth Oo Hospital Of Joint Logistics Support Force Of Chinese People's Liberation Army filed Critical Ninth Oo Hospital Of Joint Logistics Support Force Of Chinese People's Liberation Army
Priority to CN201910641898.3A priority Critical patent/CN110284171A/en
Publication of CN110284171A publication Critical patent/CN110284171A/en
Pending legal-status Critical Current

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    • 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
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F3/00Brightening metals by chemical means
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34Pretreatment of metallic surfaces to be electroplated
    • 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
    • C25D9/06Electrolytic coating other than with metals with inorganic materials by anodic processes

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  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Apparatus For Disinfection Or Sterilisation (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a kind of preparations of metal surface antimicrobial coating, certain density Biodine is configured first, using metal as anode, using platinized platinum as cathode, distance is kept constant, the deposition of iodine, deposition current 20-200mA are carried out with constant temperature water bath control, time 10-120min obtains uniform iodine coating, and content of iodine is about 10% in coating.Present invention process step is simple, it is easily operated, obtained coating uniform, content of iodine is high, sample has a good antibacterial effect, application field include medical apparatus and instruments, medical instrument, implant material, in Bioexperiment vessel and daily life storage of food etc. in need keep sterile material surface.

Description

A kind of preparation method of metal surface antimicrobial coating
Technical field
The invention belongs to coating antibacterial fields, and in particular to a kind of preparation method of metal surface antimicrobial coating.
Background technique
Surface covering will receive the infringement of microorganism while playing decoration and protective effect to ground, in coating table Face forms bacterial plaque, so that coating is lost adhesive force, or even cause coating shedding, influences the defencive function and decorative effect of coating.Separately On the one hand, the bacterial plaque of coating surface can infect disease, cause high risks to human health.And antimicrobial coating can be to avoid above-mentioned Situation occurs.
The antimicrobial coating of metal surface is formed by physico-chemical process on surface by adding antibacterial agent in the solution Antimicrobial coating.Currently, common antibacterial agent mainly has inorganic antiseptic, organic antibacterial agent and natural antibacterial agent three big in coating Class.But these anti-biotic materials have different problems, such as limited chemical stability, the local inflammation as caused by material composition The features such as reaction and coating, which lack, controls release dynamics, cytotoxicity, thermal stability is poor.Iodine is one kind of thyroid hormone Ingredient is most important element needed for all organisms.Iodine has proved to be a kind of wide spectrum, efficiently, quick-acting bactericide, to people Body is harmless.Iodine has been widely used as a kind of bactericidal disinfectant material, but the antimicrobial coating as metal material surface Research and application are also fewer.Toshiharu professor Shirai of Japanese Kanazawa university is to Titanium Alloy Screw surface It carries out anodized generation perforated membrane and is subsequently filled the iodine coating with antibacterial action, there is good antibacterial effect.So And the process requirement first carries out anodized to metal surface, complex process is expensive.The present invention metal surface into Row directly covers iodine, and simple process is low in cost, works well.
Summary of the invention
In order to solve the deficiencies in the prior art, the purpose of the present invention is to provide a kind of broad-spectrum antiseptic, antibiotic rate it is high Metal surface antimicrobial coating and preparation method thereof, it is intended to improve the anti-microbial property of metal material.
In order to realize above-mentioned technical purpose, the technical solution of the present invention is as follows:
1) by metal surface be polishing to surface it is smooth after with EtOH Sonicate clean 1-30min, then in HF and HNO3Mixture Middle progress chemical polishing (HF and HNO3Volume ratio=1:3) 1-20min;
2) a certain amount of iodine substance is weighed, is dissolved in deionized water, configuration concentration is the solution of 500-10000ppm, stirs 1- 30min obtains electrolyte;
3) it using metal as anode, using platinized platinum as cathode, keeps between cathode anode at a distance of 2cm, using above-mentioned solution as electrolyte, water Bath control constant temperature carries out iodine deposition;
4) obtained sample ultrasonic cleaning post package is saved;
The step 1) metal includes iron, stainless steel, titanium or titanium alloy, aluminium alloy, magnesium alloy, cobalt-base alloys, nickel alloy, tantalum, Any one in niobium, zirconium-based metallic material;
The step 2 includes povidone iodine, HIO containing iodine compound3、KIO3、KIO4, the soluble iodides such as KI;
The step 3) water-bath controls 5-80 DEG C of constant temperature;
The step 3) deposition current is 20-200mA, time 10-120min;
Further, above-mentioned preparation method is applied to prepare medical apparatus and instruments, medical instrument, implant material, biology in fact Test vessel, in food preservation sterilizable material.
The study found that content of iodine has a significant impact to the anti-microbial property of sample in coating.The present invention uses above-mentioned technical side Case is controlled using Biodine as electrolyte by condition, is prepared for one layer of uniform iodine coating in metal surface.
The present invention has the advantages that
(1) preparation technology of coating is simple, and the time is short;
(2) coating uniform and content of iodine height;
(3) good anti-bacterial effect, antibiotic rate can achieve 90% or more.
Detailed description of the invention:
Fig. 1 is the primary sample of sample and post-depositional sample drawing in embodiment 3.
Specific embodiment:
The present invention is further elaborated with reference to the accompanying drawings and detailed description:
A kind of preparation of metal surface antimicrobial coating, comprising the following steps:
1) by metal surface be polishing to surface it is smooth after with EtOH Sonicate clean 1-30min, then in HF and HNO3Mixture Middle progress chemical polishing (HF and HNO3Volume ratio=1:3) 1-20min;
2) a certain amount of iodine substance is weighed, is dissolved in deionized water, configuration concentration is the solution of 500-10000ppm, stirs 1- 30min obtains electrolyte;
3) using metal as anode, using platinized platinum as cathode, distance is kept constant, using above-mentioned solution as electrolyte, water-bath controls constant temperature 5-80 DEG C of progress iodine deposition, deposition current 20-200mA, time 10-120min;
4) obtained sample ultrasonic cleaning post package is saved.
Embodiment 1
A kind of preparation of metal surface antimicrobial coating, comprising the following steps:
1) by stainless steel surface be polishing to surface it is smooth after with EtOH Sonicate clean 10min, then in HF and HNO3Mixture Middle progress chemical polishing (HF and HNO3Volume ratio=1:3) 5min;
2) a certain amount of povidone iodine is weighed, is dissolved in deionized water, configuration concentration is the solution of 500ppm, stirs 30min, obtains To electrolyte;
3) it using stainless steel as anode, using platinized platinum as cathode, keeps at a distance of 2cm between anode cathode, using above-mentioned solution as electrolyte, Water-bath controls 5 DEG C of progress iodine depositions of constant temperature, deposition current 30mA, time 20min;
4) obtained sample ultrasonic cleaning post package is saved, content of iodine is 10.14% in coating;
5) sample is subjected to antibacterial test, antibiotic rate 93%.
Embodiment 2
A kind of preparation of metal surface antimicrobial coating, comprising the following steps:
1) by Mg alloy surface be polishing to surface it is smooth after with EtOH Sonicate clean 30min, then in HF and HNO3Mixture Middle progress chemical polishing (HF and HNO3Volume ratio=1:3) 10min;
2) a certain amount of KI is weighed, is dissolved in deionized water, configuration concentration is the solution of 2000ppm, stirs 10min, obtains electricity Solve liquid;
3) it using magnesium alloy as anode, using platinized platinum as cathode, keeps at a distance of 2cm between anode cathode, using above-mentioned solution as electrolyte, Water-bath controls 30 DEG C of progress iodine depositions of constant temperature, deposition current 20mA, time 60min;
4) obtained sample ultrasonic cleaning post package is saved, content of iodine is 9.39% in coating;
5) sample is subjected to antibacterial test, antibiotic rate 91%.
Embodiment 3
A kind of preparation of metal surface antimicrobial coating, comprising the following steps:
1) by titanium alloy surface be polishing to surface it is smooth after with EtOH Sonicate clean 20min, then in HF and HNO3Mixture Middle progress chemical polishing (HF and HNO3Volume ratio=1:3) 20min;
2) a certain amount of KIO is weighed3, it is dissolved in deionized water, configuration concentration is the solution of 5000ppm, stirs 20min, obtains Electrolyte;
3) it with Ti-alloy anode, using platinized platinum as cathode, keeps between anode cathode at a distance of 2cm, using above-mentioned solution as electrolyte, water Bath control 50 DEG C of progress iodine depositions of constant temperature, deposition current 100mA, time 120min;
4) obtained sample ultrasonic cleaning post package is saved, content of iodine is 10.68% in coating;
5) sample is subjected to antibacterial test, antibiotic rate 94%.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with Modification, is all covered by the present invention.

Claims (7)

1. a kind of preparation method of metal surface antimicrobial coating, it is characterised in that: itself the following steps are included:
1) by metal surface be polishing to surface it is smooth after with dehydrated alcohol be cleaned by ultrasonic 1-30min, then in HF and HNO3Mixing Chemical polishing 1-20min is carried out in object;The HF and HNO3Volume ratio=1:3;
2) it weighs a certain amount of containing iodine compound, is dissolved in deionized water, stirs 1-30min, obtain electrolyte;
3) it using metal as anode, using platinized platinum as cathode, keeps anode cathode at a distance of 2cm, is with the solution that step 2 is prepared Electrolyte, water-bath control constant temperature and carry out iodine deposition;
4) obtained sample ultrasonic cleaning post package is saved.
2. a kind of preparation method of metal surface antimicrobial coating according to claim 1, it is characterised in that: described in step 1) Metal includes iron, stainless steel, titanium or titanium alloy, aluminium alloy, magnesium alloy, cobalt-base alloys, nickel alloy and tantalum, niobium, zirconium-based metallic material Any one in material.
3. a kind of preparation method of metal surface antimicrobial coating according to claim 1, it is characterised in that: described in step 2 Solution concentration containing iodine compound is 500ppm-1000ppm.
4. a kind of preparation method of metal surface antimicrobial coating according to claim 1, it is characterised in that: described in step 2 It is soluble iodide, including povidone iodine, HIO containing iodine compound3、KIO3、KIO4, any one in KI.
5. a kind of preparation method of metal surface antimicrobial coating according to claim 1, it is characterised in that: the step 3) It is 5-80 DEG C that water-bath, which controls thermostat temperature,.
6. a kind of preparation method of metal surface antimicrobial coating according to claim 1, it is characterised in that: the step 3) Deposition current 20-200mA, time 10-120min.
7. a kind of preparation method as described in claim 1-6 is any is preparing medical apparatus and instruments, medical instrument, implant material Application in material, Bioexperiment vessel, food preservation sterilizable material.
CN201910641898.3A 2019-07-16 2019-07-16 A kind of preparation method of metal surface antimicrobial coating Pending CN110284171A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109706494A (en) * 2019-03-04 2019-05-03 福州大学 A kind of new titanium alloy method for electroplating surface

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109706494A (en) * 2019-03-04 2019-05-03 福州大学 A kind of new titanium alloy method for electroplating surface

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
肖杰: "碘涂层骨科钛板制备及其体外抗菌实验", 《中国优秀硕士学位论文全文数据库医药卫生科技辑》 *

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Application publication date: 20190927

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