CN103451631A - Antibacterial stainless steel and preparation method thereof - Google Patents
Antibacterial stainless steel and preparation method thereof Download PDFInfo
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- CN103451631A CN103451631A CN2013104286319A CN201310428631A CN103451631A CN 103451631 A CN103451631 A CN 103451631A CN 2013104286319 A CN2013104286319 A CN 2013104286319A CN 201310428631 A CN201310428631 A CN 201310428631A CN 103451631 A CN103451631 A CN 103451631A
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Abstract
The invention discloses antibacterial stainless steel and a preparation method thereof. The method comprises the steps of ultrasonic deoiling, pickling, diffusion coating, flushing and drying. According to the method, a nano-titanium-dioxide antibacterial material is formed on the surface of stainless steel through diffusion coating, the preparation cost is low, the process is simple, and the bonding force between an antibacterial layer and a stainless steel base body is strong. Different from that antibacterial elements are added into the stainless steel, nano titanium dioxide is formed on the surface of the stainless steel through diffusion coating, so that the mechanical properties of the stainless steel are not affected, and the processability of a stainless-steel material is not changed. Different from ionic antibacterial materials, nano titanium dioxide is non-toxic and harmless and can not release metal ions to a contact environment during the process of disinfecting bacteria or inhibiting bacterial growth; meanwhile, the catalytic disinfection capacity of nano titanium dioxide is strong, so that harmful bacteria, such as Escherichia coli, staphylococcus aureus and the like, can be effectively disinfected.
Description
Technical field
The present invention relates to the stainless 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 unwanted bacteria as pathogenic bacterium especially serious threat the mankind's health, the attention of people to environment of living in and self health, promoted the research and development of anti-biotic material and antimicrobial product.Stainless steel is because it has good processibility and solidity to corrosion, the multiplex tableware container of making.Give Stainless steel cutlery container anti-microbial property and can effectively extend the quality guarantee period of held food on the one hand, guarantee people's healthy edible food; Can effectively widen the scope of application of tableware container on the other hand, make originally only for container or the vessel of making food, also to can be used to hold and preserve food.
The research of anti-bacteria stainless steel at present mainly is divided into two lines, and a kind of is in stainless steel base, to add antiseptic elements to enter Cu or Ag etc., generates the solid solution phase of copper by specific heat treatment or ageing treatment in tissue, as ε-Cu phase.In use the Cu ion constantly discharges kill bacteria from this sosoloid.The defect of this alloy-type anti-bacteria stainless steel is because copper content reaches a certain amount of anti-microbial property that just there will be, so its production cost is higher; ε-Cu can bring the variation of tissue in the thermal treatment precipitation process simultaneously, produces the problem of corrosion resistance nature reduction, poor processability.Another kind method is to take stainless steel as matrix, to there is the coated materials of antibacterial to stainless steel surface by techniques such as spraying, roller coat, so-gel, ion implantation, observing and controlling sputters, this method can overcome the alloy-type anti-bacteria stainless steel due to the antibiotic defect that causes corrosion stability and poor processability of separating out mutually, but, because it is had relatively high expectations to Preparation equipment, Technology, in actual production, be difficult to be used widely.
Nano titanium oxide has good anti-microbial property, at present in building, the existing application of textile industry.But the technology that makes stainless steel possess anti-microbial property at stainless steel surface plating nano-titania photocatalyst antibiotic layer has no report.
Summary of the invention
One of purpose of the present invention is to provide a kind of chemical depositing Ni-P-nano titanic oxide to prepare the method for anti-bacteria stainless steel, and to solve, above-mentioned tooling cost is high, Preparation equipment and Technology require high problem.
The technical scheme adopted is: a kind of preparation method of anti-bacteria stainless steel comprises the following steps:
(1) ultrasonic oil removing, adopt organic reagent and remove the greasy dirt of stainless steel surface under ultrasonic environment;
(2) pickling, the stainless steel after ultrasonic oil removing carries out pickling in mineral acid;
(3) plating adds titanium fluoric acid ammonium, boric acid and deionized water to be mixed with plating solution in container, then keeps solution temperature at 40 ℃, and the stainless steel after pickling is placed in to the plating of plating solution;
(4) rinse drying, plating completes the post-flush surface, then dry, obtains.
The technical program first adopts the mode of ultrasonic oil removing and pickling, remove the passive film of stainless steel surface, and produce the activation point at stainless steel surface, and then carry out plating in the plating liquid be mixed with by titanium fluoric acid ammonium, boric acid and deionized water, clean again and dry, can be at stainless steel surface plating nanometer titanium dioxide antibiotic material, thisly take titanium dioxide and prepare the method for anti-bacteria stainless steel as antimicrobial component adopts electroless plating, preparation cost is low, and the requirement of Preparation equipment and Technology is all lower.
As preferred technical scheme, in step (1) before, stainless steel surface is polished.
Before with chemical reagent, carrying out ultrasonic decontamination, first carry out pure physical technology of removing pollution.The instrument of polishing can adopt sand paper, and sand paper is preferably first used 1000 purpose dry sand paper with 800 purpose dry sand paper again.The purpose of polishing sample is to remove most of passivation of stainless steel surface, makes the bonding force of the antibiotic layer of the anti-bacteria stainless steel product that finally makes and stainless steel base stronger.
As preferred technical scheme, in step (1) afterwards, step (2) before, also adopts NaOH, NaCO
3, Na
3pO
4and NaSiO
4prepare chemical degreasing fluid, the stainless steel after then step (1) being processed is placed in prepared electrochemical deoiling liquid and carries out electrochemical deoiling.
This step purpose is that logical peralkaline chemical reagent carries out oil removing, further removes stainless steel surface grease and dirt, reaches the purpose of further purification stainless steel sample surfaces.
As preferred technical scheme, the organic reagent in step (1) is a kind of in acetone, ethyl acetate.Also can adopt tensio-active agent, the action principle of such reagent is that the stainless steel surface organism is had to stronger dissolving power, can remove to greatest extent surface and oil contaminant.The add-on of organic reagent, be advisable just to cover the stainless steel sample.Main purpose is to remove workpiece surface grease or dirts such as residual lubricating oil, slushing oil, rubbing paste in mechanical workout or storage process.
As preferred technical scheme, in step (1), the time of ultrasonic oil removing is 8～15 minutes.More preferably 10～15 minutes.The preferred time like this, can make oil removing more thorough on the one hand, also takes into account on the other hand the efficiency of whole technique.
After ultrasonic oil removing, preferably adopt dehydrated alcohol to clean, then adopt deionized water to dry up, then carry out next step.Adopt dehydrated alcohol scavenging period more preferably 6～10 minutes, more preferably 8 minutes.The preferred time like this, can make cleaning more thorough on the one hand, also takes into account on the other hand the efficiency of whole technique.
As preferred technical scheme, in step (2), the process of pickling is: first pickling 1 minute in hydrochloric acid soln, then activation 30 seconds in sulphuric acid soln.Adopt such acid pickling step and time, remove passive film, produce the better effects if that activates point.
As preferred technical scheme further, polishing to stainless surfaceness is less than Ra0.050, makes workpiece surface have mirror effect.Such roughness is controlled, and can remove to greatest extent the stainless steel surface passivation, makes to have stronger bonding force between the antibiotic layer of the anti-bacteria stainless steel product that finally makes and stainless steel base, takes into account the aesthetic property of workpiece simultaneously.
As preferred technical scheme further, described electrochemical deoiling liquid, NaOH concentration is 60g/L, NaCO
3concentration is 30g/L, Na
3pO
4concentration is 20g/L, NaSiO
4concentration is 8g/L.Test of many times shows, under this concentration conditions, deoiling effect is comparatively desirable.
The temperature of electrochemical deoiling liquid is preferably 60 ℃.Mildly heating, can further improve except oil quality.
The time of electrochemical deoiling is preferably 20～40 minutes, more preferably 30～40 minutes.Such time is controlled on the one hand and guarantees that oil removing is more thorough, also takes into account on the other hand the efficiency of technique.
As preferred technical scheme, in step (3), the composition of described plating solution and ratio be, by percentage to the quality, and titanium fluoric acid ammonium: boric acid: deionized water=3.3:3.1:100.Under this proportioning, the bonding force of titanium dioxide antibiotic layer and stainless steel base is stronger, and cementation coating is smooth smooth.
As preferred technical scheme, in step (3), the plating time is 48～60 hours.
The control of such plating time guarantees thickness and the soundness of cementation coating on the one hand, also takes into account on the other hand the efficiency of technique.
The anti-bacteria stainless steel that the method that two of purpose of the present invention is to provide above-mentioned prepares.
Owing to having adopted above-mentioned chemical depositing Ni-P-nano titanic oxide to prepare the technical scheme of anti-bacteria stainless steel, the invention has the beneficial effects as follows: at stainless steel surface plating nanometer titanium dioxide antibiotic material, preparation cost is low, and technique is simple, and the bonding force of antibiotic layer and stainless steel base is strong.Present method is different from adds antiseptic elements in stainless steel, at stainless steel surface plating nano titanium oxide, does not affect stainless mechanical property, does not change the processing characteristics of stainless steel.Present method is different from the ionic anti-biotic material, nano titanium oxide is nontoxic, kill or the bacteria growing inhibiting process in, can be to release metal ions in contact environment, its catalytically bactericidal process ability is strong simultaneously, can effectively kill the unwanted bacterias such as intestinal bacteria, streptococcus aureus.
The accompanying drawing explanation
The stainless micro-organization chart that Fig. 1 is the embodiment of the present invention 1;
The SEM figure that Fig. 2 is the anti-bacteria stainless steel that makes of the embodiment of the present invention 1;
Fig. 3 is the XRD spectra of the titanium dioxide antibiotic layer on the anti-bacteria stainless steel surface that makes of the embodiment of the present invention 1;
Fig. 4 is the outside drawing of the anti-bacteria stainless steel that makes of the embodiment of the present invention 1;
Fig. 5 is the outside drawing of the anti-bacteria stainless steel that makes of the embodiment of the present invention 2;
Fig. 6 is the outside drawing of the anti-bacteria stainless steel that makes of the embodiment of the present invention 3;
Fig. 7 is the outside drawing of the anti-bacteria stainless steel that makes of the embodiment of the present invention 4.
Embodiment
A kind of preparation method of anti-bacteria stainless steel comprises the following steps:
(1) get stainless steel, stainless microstructure is shown in Fig. 1, adopts acetone and remove the greasy dirt of stainless steel surface under ultrasonic environment, and ultrasonic time is 8 minutes;
(2) pickling, the stainless steel after ultrasonic oil removing in hydrochloric acid 2 minutes, carry out pickling;
(3) plating adds titanium fluoric acid ammonium and boric acid and deionized water to be mixed with plating solution in container, then keeps solution temperature at 40 ℃, and the stainless steel after pickling is placed in to plating solution plating 48 hours;
(4) rinse drying, plating completes the post-flush surface, then dry, obtains.
Fig. 2 is the SEM figure (being scanning electron microscope (SEM) photograph) of the anti-bacteria stainless steel for preparing, as can be seen from Figure 2, contains a large amount of titania in stainless steel surface coating, be point-like or spindle shape, and it is uniformly distributed in the stainless steel sample surfaces;
Fig. 3 be prepared anti-bacteria stainless steel surface the titanium dioxide antibiotic layer XRD spectra (being the X-ray diffraction spectrogram), the spectrum peak from Fig. 3 can find out, the main component of antibiotic layer is anatase titanium dioxide.
The outward appearance photo that Fig. 4 is the prepared anti-bacteria stainless steel sample of the present embodiment.
Embodiment 2
A kind of preparation method of anti-bacteria stainless steel comprises the following steps:
(1) get stainless steel, with 1000 purpose sand papering stainless steel surface, making its surperficial roughness is Ra0.045;
(2) adopt ethyl acetate and remove the greasy dirt of stainless steel surface under ultrasonic environment, the amount of ethyl acetate is for just covering the stainless steel sample, and ultrasonic time is 15 minutes;
(3) with NaOH, NaCO
3, Na
3pO
4and NaSiO
4prepare chemical degreasing fluid, wherein NaOH concentration is 50g/L, NaCO
3concentration is 35g/L, Na
3pO
4concentration is 30g/L, NaSiO
4concentration is 6g/L, and the temperature of electrochemical deoiling liquid remains 50 ℃, and the sample after step (2) is processed is placed in to electrochemical deoiling liquid 20 minutes;
(4) pickling, the pickling 1 minute in hydrochloric acid soln of the sample after step (3) is processed, then be positioned in sulphuric acid soln activation 30 seconds, and wherein the volumetric concentration of hydrochloric acid soln is 20%, the volumetric concentration of sulphuric acid soln concentration is 5%.
(5) plating, in container, add titanium fluoric acid ammonium, boric acid and deionized water to be mixed with plating solution, then keep solution temperature at 40 ℃, stainless steel after pickling is placed in to plating solution plating 60 hours, the composition of described plating liquid and ratio are, by percentage to the quality, titanium fluoric acid ammonium: boric acid: deionized water=3.3:3.1:100;
(6) then use the deionized water rinsing surface, then natural air drying, obtain.
Fig. 5 is shown in by the outward appearance photo of the anti-bacteria stainless steel of gained.
Embodiment 3
A kind of preparation method of anti-bacteria stainless steel comprises the following steps:
(1) get stainless steel, first use 800 purpose sand paper, then use 1000 purpose sand papering stainless steel surface, making its surperficial roughness is Ra0.042;
(2) adopt acetone and remove the greasy dirt of stainless steel surface under ultrasonic environment, the amount of acetone is for just covering the stainless steel sample, and ultrasonic time is 12 minutes; After ultrasonic oil removing, then clean 6 minutes with dehydrated alcohol, then with drying up after washed with de-ionized water;
(3) with NaOH, NaCO
3, Na
3pO
4and NaSiO
4prepare chemical degreasing fluid, wherein NaOH concentration is 60g/L, NaCO
3concentration is 30g/L, Na
3pO
4concentration is 20g/L, NaSiO
4concentration is 8g/L, and the temperature of electrochemical deoiling liquid remains 60 ℃, and the sample after step (2) is processed is placed in to electrochemical deoiling liquid 30 minutes;
(4) pickling, the pickling 1 minute in hydrochloric acid soln of the sample after step (3) is processed, then be positioned in sulphuric acid soln activation 30 seconds, wherein the volumetric concentration of hydrochloric acid soln is 30%, the volumetric concentration of sulphuric acid soln concentration is for being 8%.
(5) plating, in container, add titanium fluoric acid ammonium and boric acid and deionized water to be mixed with plating solution, then keep solution temperature at 40 ℃, stainless steel after pickling is placed in to plating solution plating 50 hours, the composition of described plating liquid and ratio are, by percentage to the quality, titanium fluoric acid ammonium: boric acid: deionized water=3.3:3.1:100;
(6) then use the deionized water rinsing surface, then natural air drying, obtain.
Fig. 6 is shown in by the outward appearance photo of the anti-bacteria stainless steel of gained.
Embodiment 4
A kind of preparation method of anti-bacteria stainless steel comprises the following steps:
(1) get stainless steel, first use 800 purpose sand paper, then use 1000 purpose sand papering stainless steel surface, making its surperficial roughness is Ra0.046;
(2) adopt acetone and remove the greasy dirt of stainless steel surface under ultrasonic environment, the amount of acetone is for just covering the stainless steel sample, and ultrasonic time is 5 minutes; After ultrasonic oil removing, then clean 5 minutes with dehydrated alcohol, then with drying up after washed with de-ionized water;
(3) with NaOH, NaCO
3, Na
3pO
4and NaSiO
4prepare chemical degreasing fluid, wherein NaOH concentration is 55g/L, NaCO
3concentration is 40g/L, Na
3pO
4concentration is 15g/L, NaSiO
4concentration is 10g/L, and the temperature of electrochemical deoiling liquid remains 40 ℃, and the sample after step (2) is processed is placed in to electrochemical deoiling liquid 15 minutes;
(4) pickling, the pickling 1 minute in hydrochloric acid soln of the sample after step (3) is processed, then be positioned in sulphuric acid soln activation 30 seconds, wherein the volumetric concentration of hydrochloric acid soln is 36%, the volumetric concentration of sulphuric acid soln concentration is for being 12%.
(5) plating, in container, add titanium fluoric acid ammonium and boric acid and deionized water to be mixed with plating solution, then keep solution temperature at 40 ℃, stainless steel after pickling is placed in to plating solution plating 50 hours, the composition of described plating liquid and ratio are, by percentage to the quality, titanium fluoric acid ammonium: boric acid: deionized water=4.5:2.1:100;
(6) then use the deionized water rinsing surface, then natural air drying, obtain.
Fig. 7 is shown in by the outward appearance photo of the anti-bacteria stainless steel of gained.
The above, it is only preferred embodiment of the present invention, not technical scope of the present invention is imposed any restrictions, therefore any trickle modification, equivalent variations and modification that every foundation technical spirit of the present invention is done above embodiment all still belong in the scope of technical solution of the present invention.
Claims (10)
1. the preparation method of an anti-bacteria stainless steel, is characterized in that, comprises the following steps:
(1) ultrasonic oil removing, adopt organic reagent and remove the greasy dirt of stainless steel surface under ultrasonic environment;
(2) pickling, the stainless steel after ultrasonic oil removing carries out pickling in mineral acid;
(3) plating adds titanium fluoric acid ammonium, boric acid and deionized water to be mixed with plating solution in container, then keeps solution temperature at 40 ℃, and the stainless steel after pickling is placed in to the plating of plating solution;
(4) rinse drying, plating completes the post-flush surface, then dry, obtains.
2. the preparation method of a kind of anti-bacteria stainless steel according to claim 1, is characterized in that, in step (1) before, stainless steel surface polished.
3. the preparation method of a kind of anti-bacteria stainless steel according to claim 1, is characterized in that, in step (1) afterwards, step (2) before, also adopts NaOH, NaCO
3, Na
3pO
4and NaSiO
4prepare chemical degreasing fluid, the stainless steel after then step (1) being processed is placed in prepared electrochemical deoiling liquid and carries out electrochemical deoiling.
4. the preparation method of a kind of anti-bacteria stainless steel according to claim 1, is characterized in that, the organic reagent in step (1) is a kind of in acetone, ethyl acetate.
5. the preparation method of a kind of anti-bacteria stainless steel according to claim 1, is characterized in that, in step (1), the time of ultrasonic oil removing is 8～15 minutes.
6. the preparation method of a kind of anti-bacteria stainless steel according to claim 1, is characterized in that, in step (2), the process of pickling is: first pickling 1 minute in hydrochloric acid soln, then activation 30 seconds in sulphuric acid soln.
7. the preparation method of a kind of anti-bacteria stainless steel according to claim 2, is characterized in that, polishing to stainless surfaceness is less than Ra0.050.
8. the preparation method of a kind of anti-bacteria stainless steel according to claim 3, is characterized in that, described electrochemical deoiling liquid, and NaOH concentration is 60g/L, NaCO
3concentration is 30g/L, Na
3pO
4concentration is 20g/L, NaSiO
4concentration is 8g/L.
9. the preparation method of a kind of anti-bacteria stainless steel according to claim 1, is characterized in that, in step (3), the composition of described plating solution and ratio be, by percentage to the quality, and titanium fluoric acid ammonium: boric acid: deionized water=3.3:3.1:100.
10. according to the preparation-obtained anti-bacteria stainless steel of method of claim 1-9 any one.
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Cited By (3)
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| CN104141133A (en) * | 2014-07-31 | 2014-11-12 | 厦门大学 | Preparation method of ionic-liquid-modified anti-bacterial stainless steel material |
| 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 |
| CN109054486A (en) * | 2018-06-29 | 2018-12-21 | 安徽同益彩钢薄板科技有限公司 | The method of anti-bacteria stainless steel is prepared under a kind of room temperature |
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| 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 |
| CN109054486A (en) * | 2018-06-29 | 2018-12-21 | 安徽同益彩钢薄板科技有限公司 | The method of anti-bacteria stainless steel is prepared under a kind of room temperature |
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| CN103451631B (en) | 2016-06-15 |
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