CN103451631B - A kind of anti-bacteria stainless steel and preparation method thereof - Google Patents
A kind of anti-bacteria stainless steel and preparation method thereof Download PDFInfo
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- CN103451631B CN103451631B CN201310428631.9A CN201310428631A CN103451631B CN 103451631 B CN103451631 B CN 103451631B CN 201310428631 A CN201310428631 A CN 201310428631A CN 103451631 B CN103451631 B CN 103451631B
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Abstract
The invention discloses a kind of anti-bacteria stainless steel and preparation method thereof, wherein, preparation process includes ultrasonic oil removing, pickling, plating and flushing and dries, this method is at stainless steel surfaces plating nanometer titanium dioxide antibiotic material, preparation cost is low, technique is simple, and antibiotic layer is strong with the adhesion of stainless steel base. This method is different from rustless steel and adds antiseptic elements, do not affect stainless mechanical performance at stainless steel surfaces plating nano titanium oxide, do not change the processing characteristics of stainless steel. This method is different from ion-type anti-biotic material, nano titanium oxide is nontoxic, is killing or in bacteria growing inhibiting process, will not to release metal ions in contact environment, its catalytically bactericidal process ability is strong simultaneously, can effectively kill the noxious bacteria such as escherichia coli, staphylococcus aureus.
Description
Technical field
The present invention relates to rustless steel technical field, in particular to a kind of anti-bacteria stainless steel and preparation method thereof.
Background technology
In the modern life, people face the invasion of microorganism constantly, and the health of the mankind in noxious bacteria such as pathogenic bacterium serious threat especially, people's attention to local environment and own health, have promoted the research and development of anti-biotic material and antimicrobial product. Rustless steel has good processability and corrosion resistance due to it, and be used for makes tableware container more. Give the quality guarantee period that Stainless steel cutlery container anti-microbial property can extend held food on the one hand effectively, it is ensured that health of people edible food; Can effectively widen on the other hand the scope of application of tableware container, make original only container or vessel for making food also can be used to hold and preserve food.
The research of current anti-bacteria stainless steel is broadly divided into two lines, and one is to add antiseptic elements in stainless steel base to enter Cu or Ag etc., is generated the solid solution phase of copper in the tissue by specific heat treatment or Ageing Treatment, such as ε-Cu phase. In use Cu ion constantly discharges from this solid solution and kills antibacterial. This alloy-type anti-bacteria stainless steel has the drawback that therefore its production cost is higher owing to copper content reaches a certain amount of just to there will be anti-microbial property; ε-Cu can bring the change of tissue in heat treatment precipitation process simultaneously, the problem producing decay resistance reduction, poor processability. Another kind of method is with rustless steel for matrix, by techniques such as spraying, roller coat, so-gel, ion implanting, observing and controlling sputterings, the material with antibacterial functions is coated on stainless steel surfaces, this method can overcome alloy-type anti-bacteria stainless steel to precipitate out, due to antibacterial phase, the defect causing corrosion stability and poor processability, but owing to it is higher to Preparation equipment, process specifications, it is difficult to be used widely in actual production.
Nano titanium oxide has excellent anti-microbial property, at present in building, the existing application of textile industry.But make the technology that rustless steel possesses anti-microbial property have no report at stainless steel surfaces plating nano-titania photocatalyst antibiotic layer.
Summary of the invention
An object of the present invention is in that a kind of method providing chemical depositing Ni-P-nano titanic oxide to prepare anti-bacteria stainless steel, to solve that above-mentioned processing cost is high, Preparation equipment and the high problem of process specifications.
The technical scheme adopted is: the preparation method of a kind of anti-bacteria stainless steel, comprises the following steps:
(1) ultrasonic oil removing, adopts organic reagent and removes the greasy dirt of stainless steel surfaces under ultrasonic environment;
(2) pickling, the rustless steel after ultrasonic oil removing carries out pickling in mineral acid;
(3) plating, adds titanium fluoric acid ammonium, boric acid and deionized water in a reservoir and is configured to plating solution, then keep solution temperature at 40 DEG C, the rustless steel after pickling is placed in plating in plating solution;
(4) flushing is dry, and plating completes afterflush surface, then dries, and to obtain final product.
The technical program first adopts the mode of ultrasonic oil removing and pickling, remove the passivating film of stainless steel surfaces, and produce activation point at stainless steel surfaces, then the plating liquid being configured to by titanium fluoric acid ammonium, boric acid and deionized water again carries out plating, clean again and dry, can at stainless steel surfaces plating nanometer titanium dioxide antibiotic material, this method adopting chemical deposition to prepare anti-bacteria stainless steel for antimicrobial component with titanium dioxide, preparation cost is low, and the requirement of Preparation equipment and Technology is all relatively low.
As preferred technical scheme, before step (1), stainless steel surfaces is polished.
Before carrying out ultrasonic decontamination with chemical reagent, first carry out pure physical technology of removing pollution. Polishing instrument can adopt sand paper, sand paper preferably first with the dry sand paper of 800 orders again with the dry sand paper of 1000 orders. The purpose of polishing sample is to remove most of passivation of stainless steel surfaces, and the antibiotic layer making the last anti-bacteria stainless steel product prepared is higher with the adhesion of stainless steel base.
As preferred technical scheme, after step (1), before step (2), also adopt NaOH, NaCO3、Na3PO4And NaSiO4Preparation chemistry degreasing fluid, the rustless steel after then step (1) being processed is placed in the electrochemical deoiling liquid prepared and carries out electrochemical deoiling.
This step purpose is that logical peralkaline chemical reagent carries out oil removing, removes stainless steel surfaces oils and fats and dirt further, reaches to purify further the purpose of rustless steel sample surfaces.
As preferred technical scheme, the organic reagent in step (1) is the one in acetone, ethyl acetate. Can also adopting surfactant, the action principle of such reagent is that stainless steel surfaces Organic substance is had stronger solvability, can remove surface and oil contaminant to greatest extent. The addition of organic reagent, is advisable just covering rustless steel sample. Main purpose is to remove lubricating oil that surface of the work remains in machining or storing process, antirust oil, oils and fats or the dirt such as antiscuffing paste.
As preferred technical scheme, in step (1), the time of ultrasonic oil removing is 8～15 minutes. It is more preferably 10～15 minutes. Such preferred time, oil removing can be made on the one hand more thorough, also take into account the efficiency of whole technique on the other hand.
After ultrasonic oil removing, it is preferred to use washes of absolute alcohol, then adopt deionized water to dry up, then carry out next step. Adopt more preferably 6～10 minutes washes of absolute alcohol time, more preferably 8 minutes.Such preferred time, cleaning can be made on the one hand more thorough, also take into account the efficiency of whole technique on the other hand.
As preferred technical scheme, in step (2), the process of pickling is: first pickling 1 minute in hydrochloric acid solution, then activates 30 seconds in sulfuric acid solution. Adopt such acid pickling step and time, remove passivating film, produce the better effects if of activation point.
As further preferred technical scheme, it is polishing to stainless surface roughness less than Ra0.050, makes surface of the work have mirror effect. Such roughness controls, it is possible to remove stainless steel surfaces passivation to greatest extent, makes have stronger adhesion between antibiotic layer and the stainless steel base of the last anti-bacteria stainless steel product prepared, takes into account the aesthetic property of workpiece simultaneously.
As further preferred technical scheme, described electrochemical deoiling liquid, NaOH concentration is 60g/L, NaCO3Concentration is 30g/L, Na3PO4Concentration is 20g/L, NaSiO4Concentration is 8g/L. Test of many times shows, under this concentration conditions, deoiling effect is ideal.
The temperature of electrochemical deoiling liquid is preferably 60 DEG C. Appropriate heating, can further improve oil removing quality.
The time of electrochemical deoiling is preferably 20～40 minutes, more preferably 30～40 minutes. Such time controls to ensure that oil removing is more thorough on the one hand, also takes into account the efficiency of technique on the other hand.
As preferred technical scheme, in step (3), composition and the ratio of described plating solution be, by percentage to the quality, and titanium fluoric acid ammonium: boric acid: deionized water=3.3:3.1:100. Under this proportioning, titanium dioxide antibiotic layer is higher with the adhesion of stainless steel base, and cementation coating flat smooth.
As preferred technical scheme, in step (3), the plating time is 48～60 hours.
The thickness controlling guarantee cementation coating on the one hand of such plating time and robustness, also take into account the efficiency of technique on the other hand.
The two of the purpose of the present invention are in that the anti-bacteria stainless steel providing above-mentioned method to prepare.
The technical scheme of anti-bacteria stainless steel is prepared owing to have employed above-mentioned chemical depositing Ni-P-nano titanic oxide, the invention has the beneficial effects as follows: at stainless steel surfaces plating nanometer titanium dioxide antibiotic material, preparation cost is low, and technique is simple, and antibiotic layer is strong with the adhesion of stainless steel base. This method is different from rustless steel and adds antiseptic elements, do not affect stainless mechanical performance at stainless steel surfaces plating nano titanium oxide, do not change the processing characteristics of stainless steel. This method is different from ion-type anti-biotic material, nano titanium oxide is nontoxic, is killing or in bacteria growing inhibiting process, will not to release metal ions in contact environment, its catalytically bactericidal process ability is strong simultaneously, can effectively kill the noxious bacteria such as escherichia coli, staphylococcus aureus.
Accompanying drawing explanation
Fig. 1 is the stainless micro-organization chart of the embodiment of the present invention 1;
Fig. 2 is the SEM figure of the anti-bacteria stainless steel that the embodiment of the present invention 1 prepares;
Fig. 3 is the XRD spectra of the titanium dioxide antibiotic layer on the anti-bacteria stainless steel surface that the embodiment of the present invention 1 prepares;
Fig. 4 is the outside drawing of the anti-bacteria stainless steel that the embodiment of the present invention 1 prepares;
Fig. 5 is the outside drawing of the anti-bacteria stainless steel that the embodiment of the present invention 2 prepares;
Fig. 6 is the outside drawing of the anti-bacteria stainless steel that the embodiment of the present invention 3 prepares;
Fig. 7 is the outside drawing of the anti-bacteria stainless steel that the embodiment of the present invention 4 prepares.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of anti-bacteria stainless steel, comprises the following steps:
(1) taking rustless steel, stainless microstructure is shown in Fig. 1, adopts acetone and removes the greasy dirt of stainless steel surfaces under ultrasonic environment, and ultrasonic time is 8 minutes;
(2) pickling, the rustless steel after ultrasonic oil removing in hydrochloric acid 2 minutes, carry out pickling;
(3) plating, adds titanium fluoric acid ammonium and boric acid in a reservoir and deionized water is configured to plating solution, then keeps solution temperature at 40 DEG C, is placed in plating solution by the rustless steel after pickling plating 48 hours;
(4) flushing is dry, and plating completes afterflush surface, then dries, and to obtain final product.
Fig. 2 is SEM figure (i.e. scanning electron microscope (SEM) photograph) of the anti-bacteria stainless steel prepared, and as can be seen from Figure 2, contains a large amount of titania in stainless steel surfaces coating, and in point-like or fusiform, and it is uniformly distributed in rustless steel sample surfaces;
Fig. 3 be the titanium dioxide antibiotic layer on obtained anti-bacteria stainless steel surface XRD spectra (i.e. X-ray diffraction spectrogram), the spectral peak from Fig. 3 can be seen that, antibiotic layer be mainly composed of anatase titanium dioxide.
Fig. 4 is the outward appearance photo of anti-bacteria stainless steel sample prepared by the present embodiment.
Embodiment 2
The preparation method of a kind of anti-bacteria stainless steel, comprises the following steps:
(1) rustless steel is taken, with the sand papering stainless steel surfaces of 1000 orders so that it is the roughness on surface is Ra0.045;
(2) adopting ethyl acetate and remove the greasy dirt of stainless steel surfaces under ultrasonic environment, the amount of ethyl acetate is just cover rustless steel sample, and ultrasonic time is 15 minutes;
(3) with NaOH, NaCO3、Na3PO4And NaSiO4Preparation chemistry degreasing fluid, wherein NaOH concentration is 50g/L, NaCO3Concentration is 35g/L, Na3PO4Concentration is 30g/L, NaSiO4Concentration is 6g/L, and the temperature of electrochemical deoiling liquid remains 50 DEG C, is placed in electrochemical deoiling liquid 20 minutes by the sample after step (2) processes;
(4) pickling, sample pickling 1 minute in hydrochloric acid solution after step (3) is processed, then be positioned in sulfuric acid solution and activate 30 seconds, wherein the volumetric concentration of hydrochloric acid solution is 20%, and the volumetric concentration of sulfuric acid solution concentration is 5%.
(5) plating, add titanium fluoric acid ammonium, boric acid and deionized water in a reservoir and be configured to plating solution, then keep solution temperature at 40 DEG C, it is placed in plating solution by the rustless steel after pickling plating 60 hours, composition and the ratio of described plating liquid are, by percentage to the quality, titanium fluoric acid ammonium: boric acid: deionized water=3.3:3.1:100;
(6) then use deionized water rinsing surface, then natural air drying, to obtain final product.
Fig. 5 is shown in by the outward appearance photo of the anti-bacteria stainless steel of gained.
Embodiment 3
The preparation method of a kind of anti-bacteria stainless steel, comprises the following steps:
(1) rustless steel is taken, first with the sand paper of 800 orders, then with the sand papering stainless steel surfaces of 1000 orders so that it is the roughness on surface is Ra0.042;
(2) adopting acetone and remove the greasy dirt of stainless steel surfaces under ultrasonic environment, the amount of acetone is just cover rustless steel sample, and ultrasonic time is 12 minutes; After ultrasonic oil removing, then with washes of absolute alcohol 6 minutes, then dry up after cleaning with deionized water;
(3) with NaOH, NaCO3、Na3PO4And NaSiO4Preparation chemistry degreasing fluid, wherein NaOH concentration is 60g/L, NaCO3Concentration is 30g/L, Na3PO4Concentration is 20g/L, NaSiO4Concentration is 8g/L, and the temperature of electrochemical deoiling liquid remains 60 DEG C, is placed in electrochemical deoiling liquid 30 minutes by the sample after step (2) processes;
(4) pickling, sample pickling 1 minute in hydrochloric acid solution after step (3) is processed, then be positioned in sulfuric acid solution and activate 30 seconds, wherein the volumetric concentration of hydrochloric acid solution is 30%, and the volumetric concentration of sulfuric acid solution concentration is for for 8%.
(5) plating, add titanium fluoric acid ammonium and boric acid in a reservoir and deionized water is configured to plating solution, then keep solution temperature at 40 DEG C, it is placed in plating solution by the rustless steel after pickling plating 50 hours, composition and the ratio of described plating liquid are, by percentage to the quality, titanium fluoric acid ammonium: boric acid: deionized water=3.3:3.1:100;
(6) then use deionized water rinsing surface, then natural air drying, to obtain final product.
Fig. 6 is shown in by the outward appearance photo of the anti-bacteria stainless steel of gained.
Embodiment 4
The preparation method of a kind of anti-bacteria stainless steel, comprises the following steps:
(1) rustless steel is taken, first with the sand paper of 800 orders, then with the sand papering stainless steel surfaces of 1000 orders so that it is the roughness on surface is Ra0.046;
(2) adopting acetone and remove the greasy dirt of stainless steel surfaces under ultrasonic environment, the amount of acetone is just cover rustless steel sample, and ultrasonic time is 5 minutes; After ultrasonic oil removing, then with washes of absolute alcohol 5 minutes, then dry up after cleaning with deionized water;
(3) with NaOH, NaCO3、Na3PO4And NaSiO4Preparation chemistry degreasing fluid, wherein NaOH concentration is 55g/L, NaCO3Concentration is 40g/L, Na3PO4Concentration is 15g/L, NaSiO4Concentration is 10g/L, and the temperature of electrochemical deoiling liquid remains 40 DEG C, is placed in electrochemical deoiling liquid 15 minutes by the sample after step (2) processes;
(4) pickling, sample pickling 1 minute in hydrochloric acid solution after step (3) is processed, then be positioned in sulfuric acid solution and activate 30 seconds, wherein the volumetric concentration of hydrochloric acid solution is 36%, and the volumetric concentration of sulfuric acid solution concentration is for for 12%.
(5) plating, add titanium fluoric acid ammonium and boric acid in a reservoir and deionized water is configured to plating solution, then keep solution temperature at 40 DEG C, it is placed in plating solution by the rustless steel after pickling plating 50 hours, composition and the ratio of described plating liquid are, by percentage to the quality, titanium fluoric acid ammonium: boric acid: deionized water=4.5:2.1:100;
(6) then use deionized water rinsing surface, then natural air drying, to obtain final product.
Fig. 7 is shown in by the outward appearance photo of the anti-bacteria stainless steel of gained.
The above, it it is only presently preferred embodiments of the present invention, not the technical scope of the present invention is imposed any restrictions, therefore every any trickle amendment, equivalent variations and modification above example made according to the technical spirit of the present invention, all still fall within the scope of technical solution of the present invention.
Claims (6)
1. the preparation method of an anti-bacteria stainless steel, it is characterised in that comprise the following steps:
(1) stainless steel surfaces is polished, be polishing to stainless surface roughness less than Ra0.050;
(2) ultrasonic oil removing, adopts organic reagent and removes the greasy dirt of stainless steel surfaces under ultrasonic environment;
(3) pickling, the rustless steel after ultrasonic oil removing carries out pickling in mineral acid, and the process of pickling is: first pickling 1 minute in hydrochloric acid solution, then activates 30 seconds in sulfuric acid solution;
(4) plating, add titanium fluoric acid ammonium and boric acid in a reservoir and deionized water is configured to plating solution, then keep solution temperature at 40 DEG C, rustless steel after pickling is placed in plating in plating solution, the plating time is 48～60 hours, composition and the ratio of described plating solution be, by percentage to the quality, and titanium fluoric acid ammonium: boric acid: deionized water=3.3:3.1:100;
(5) flushing is dry, and plating completes afterflush surface, then natural air drying, to obtain final product.
2. the preparation method of a kind of anti-bacteria stainless steel according to claim 1, it is characterised in that after step (2), before step (3), also adopts NaOH, NaCO3、Na3PO4And NaSiO4Preparation chemistry degreasing fluid, the rustless steel after then step (2) being processed is placed in the electrochemical deoiling liquid prepared and carries out electrochemical deoiling.
3. the preparation method of a kind of anti-bacteria stainless steel according to claim 1, it is characterised in that the organic reagent in step (2) is the one in acetone, ethyl acetate.
4. the preparation method of a kind of anti-bacteria stainless steel according to claim 1, it is characterised in that in step (2), the time of ultrasonic oil removing is 8～15 minutes.
5. the preparation method of a kind of anti-bacteria stainless steel according to claim 2, it is characterised in that described electrochemical deoiling liquid, NaOH concentration is 60g/L, NaCO3Concentration is 30g/L, Na3PO4Concentration is 20g/L, NaSiO4Concentration is 8g/L.
6. according to the preparation-obtained anti-bacteria stainless steel of the method for claim 1-5 any one.
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| CN104141133B (en) * | 2014-07-31 | 2016-04-06 | 厦门大学 | A kind of preparation method of anti-bacteria stainless steel material of Ionic Liquid Modified |
| CN106757074A (en) * | 2016-12-16 | 2017-05-31 | 安徽宝恒新材料科技有限公司 | A kind of processing method for improving stainless steel antibiotic property |
| CN109054486B (en) * | 2018-06-29 | 2020-11-10 | 安徽同益净化科技有限公司 | Method for preparing antibacterial stainless steel at normal temperature |
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| CN1663684A (en) * | 2004-03-02 | 2005-09-07 | 方侃 | Method for preparing nano titanium dioxide film |
| CN101215698A (en) * | 2007-12-28 | 2008-07-09 | 天津大学 | Method for preparing film surface of nanometer-stage thickness on red copper surface |
| CN101760737A (en) * | 2009-12-29 | 2010-06-30 | 天津大学 | Method for preparing enhanced heat-transfer and scale prevention coating of micron/nanometer titanium dioxide on stainless steel substrate |
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| JP2003063912A (en) * | 2001-08-22 | 2003-03-05 | Ulvac Japan Ltd | Antibacterial and antifouling material and manufacturing method for conductive and visible light sensitive titanium oxide |
| CN1786264A (en) * | 2005-11-01 | 2006-06-14 | 武汉理工大学 | Method of low temperature preparing C axle preferrel orientation titanium dioxide film |
| KR101189890B1 (en) * | 2010-05-17 | 2012-10-10 | 한국생산기술연구원 | Mesoporous TiO2 formed Electrode Using Gas Cluster Coating on stainless steel And Manufacturing Method and System Thereof |
| CN102527613B (en) * | 2012-02-17 | 2014-04-30 | 天津大学 | Liquid-phase deposition-impregnation preparation method of micro/nano low-surface hydrophobic composite anti-scaling coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1663684A (en) * | 2004-03-02 | 2005-09-07 | 方侃 | Method for preparing nano titanium dioxide film |
| CN101215698A (en) * | 2007-12-28 | 2008-07-09 | 天津大学 | Method for preparing film surface of nanometer-stage thickness on red copper surface |
| CN101760737A (en) * | 2009-12-29 | 2010-06-30 | 天津大学 | Method for preparing enhanced heat-transfer and scale prevention coating of micron/nanometer titanium dioxide on stainless steel substrate |
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