CN109930191A - Antibacterial stainless steel and preparation method thereof - Google Patents
Antibacterial stainless steel and preparation method thereof Download PDFInfo
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- CN109930191A CN109930191A CN201910249534.0A CN201910249534A CN109930191A CN 109930191 A CN109930191 A CN 109930191A CN 201910249534 A CN201910249534 A CN 201910249534A CN 109930191 A CN109930191 A CN 109930191A
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Abstract
The invention provides an antibacterial stainless steel and a preparation method thereof, wherein the method comprises the following steps: the method comprises the steps of pretreating stainless steel, placing the pretreated stainless steel in an acid solution, carrying out oxidation and coloring treatment by adopting alternating current, and then carrying out hole sealing treatment to obtain the antibacterial stainless steel. According to the invention, the alternating current mode is adopted to realize the alternate oxidation and coloring of the stainless steel surface, the oxidation and coloring of the stainless steel can be carried out in the same solution, the stainless steel has excellent antibacterial, mildew-proof and corrosion-resistant properties through the synergistic effect of various antibacterial elements, the color of a stainless steel product is adjusted through the change of process parameters, and the wear resistance and the glossiness of the stainless steel surface can be improved through hole sealing treatment; the method is simple and convenient, green and environment-friendly, does not use chromium-containing solution, reduces environmental pollution and meets the requirements of WEES and ROHS instructions.
Description
Technical field
The invention belongs to technical field of metal material surface treatment, it is related to a kind of anti-bacteria stainless steel and preparation method thereof.
Background technique
Stainless steel is a kind of alloy material with excellent corrosion resistance, wearability and toughness, excellent in mechanical performance, chemistry
Stability is good, building trade, household goods, cooking apparatus, auto industry, in terms of have a wide range of applications.
With the improvement of living standards, people increasingly pay attention to environment and own health, if stainless steel material connects in use
Touching grease etc. can promote bacteria breed, bring adverse effect to health of people.However, common stainless steel does not have antibacterial generally
Ability is extremely limited it in the application in certain fields.Therefore, the research and development of anti-bacteria stainless steel come in recent years
Become the research hotspot of new type functional stainless steel, can not only keep the mechanical property and any surface finish of stainless steel base
Degree, and the antibacterial effect with spectrum-stable.
Anti-bacteria stainless steel presses the difference of its manufacturing method, can substantially be divided into: surface covering type anti-bacteria stainless steel, addition are anti-
Alloy-type anti-bacteria stainless steel, composite bactericidal stainless steel and the Vacuum Deposition membranous type anti-bacteria stainless steel of bacterium metallic element.Surface applies
The coating binding force of stratotype anti-bacteria stainless steel is unstable, cannot apply at high temperature, and surface covering is easy weathering and falls off, antibacterial
The Durability of antimicrobial effect of material is not strong；Alloy-type anti-bacteria stainless steel, silver and copper are easily precipitated in crystal boundary in fusion process, cause stainless
Steel cracking, is allowed to be difficult to shape, while the bactericidal effect of anti-biotic material usually occurs on the surface of the material, the antibacterial gold of intrinsic silicon
Category does not play antibacterial action；The production of composite bactericidal stainless steel is complicated, stringenter to the range request excessively of rolling, stainless steel layer
It is not strong with the binding force of layers of copper, it can be easily separated and fall off and antibacterial effect is bad；Vacuum Deposition membranous type anti-bacteria stainless steel higher cost, and
And the discoloration problem of its surface silver, it is also difficult to solve.
Based on defect existing for single method of modifying, researcher uses a variety of modification mode phases to the research of anti-bacteria stainless steel
In conjunction with improving its performance.CN 103276426A discloses a kind of manufacturing method of anti-corrosion antibacterial oxidation film stainless steel, the side
Method includes: one layer of passivating film of first Passivation Treatment formation on stainless steel base, then processing forms one layer of point crystalline substance in an acidic solution
Stone oxidation film, finally drying obtains the stainless steel after sealing pores.CN 108950498A discloses a kind of antibacterial not
Become rusty steel board preparation method, comprising the following steps: stainless steel materials be first processed by shot blasting with chemical solution impregnation, so
After carry out seeping molybdenum processing and hot rolling densified, then form one layer of passivation layer and one layer of antibiotic layer in outer surface, finally obtain
Anti-bacteria stainless steel.There is the requirement that Green Chemistry is not met using chromium-containing solution in the above method, the former plated film mode is single,
The latter's processing step is more, and a variety of effects are difficult to coordinate, and is unable to give full play effect.
In conclusion the preparation of anti-bacteria stainless steel also needs to seek reasonable, efficient method, make its both had antibacterial, it is anti-corrosion,
The performance of color multiplicity, and can satisfy the requirement of Green Chemistry.
Summary of the invention
In view of the problems of the existing technology, the purpose of the present invention is to provide a kind of anti-bacteria stainless steel and its preparation sides
Method, the method are used Chrome-free acid solution, alternating oxidation and the coloring of stainless steel are realized in a manner of alternating current, is passed through
The synergistic effect of a variety of antiseptic elements is adjusted so that stainless steel has excellent antibacterial, corrosion resisting property, while color multiplicity,
Extend its application range.
To achieve this purpose, the present invention adopts the following technical scheme:
On the one hand, the present invention provides a kind of preparation methods of anti-bacteria stainless steel, which comprises
Stainless steel progress pre-treatment is placed in acid solution, is aoxidized using alternating current, coloring treatment, then
Sealing pores are carried out, anti-bacteria stainless steel is obtained.
In the present invention, stainless steel first carries out pre-treatment, so that its surfacing, cleaning, then lead in acidic electrolysis bath
Enter alternating current, stainless steel is respectively formed oxidation film and deposition film alternately as anode, cathode, surface, makes the oxygen of stainless steel
Change and coloring can be completed in same solution, and multiple element plays Synergistic antimicrobial mildew-proof function, finally by sealing pores, improve
The glossiness and planarization of stainless steel surface.The method is easy to operate, environmentally protective, gained stainless steel product antibacterial, resistance to
Erosion is had excellent performance, and color multiplicity can effectively meet the needs of market.
It is used as currently preferred technical solution below, but not as the limitation of technical solution provided by the invention, passes through
Following technical scheme can preferably reach and realize technical purpose and beneficial effect of the invention.
As currently preferred technical solution, the pre-treatment successively includes mechanical polishing, electrochemical deoiling and electrochemistry
Polishing.
Preferably, the mechanical polishing is using sand paper progress surface polishing.
Preferably, the electrochemical deoiling is carried out using degreasing fluid.
Preferably, the composition of the degreasing fluid includes the phosphate of caustic alkali, the carbonate of alkali metal and alkali metal, preferably
For sodium hydroxide, sodium carbonate and sodium phosphate.
In the present invention, degreasing fluid is typically chosen alkaline solution, is conducive to the grease stain for removing stainless steel surface, using degreasing fluid
When being handled, temperature is generally 40~60 DEG C, and the processing time is shorter, general 2~3min.
As currently preferred technical solution, the electrochemical polishing treatment carries out in polishing fluid, is with stainless steel
Anode, using graphite as cathode.
Preferably, the composition of the polishing fluid includes phosphoric acid, sulfuric acid and glycerine.
Preferably, the volume ratio of the phosphoric acid, sulfuric acid and glycerine is (11~14): (5~8): 1, such as 11:5:1,
11:8:1,12:7:1,13:6:1,14:5:1 or 14:8:1 etc., it is not limited to cited numerical value, in the numberical range its
His unlisted numerical value is equally applicable.
In the present invention, phosphoric acid used and sulfuric acid are concentrated acid, wherein phosphoric acid quality score selection 85%, the quality of sulfuric acid
Score is then 98%.
Preferably, the temperature of the electrochemical polishing treatment is 50~80 DEG C, such as 50 DEG C, 60 DEG C, 70 DEG C or 80 DEG C etc.,
It is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable；Time is 5~10min,
Such as 5min, 6min, 7min, 8min, 9min or 10min etc., it is not limited to cited numerical value, in the numberical range its
His unlisted numerical value is equally applicable.
Preferably, the current density of the electrochemical polishing treatment is 20~60A/dm2, such as 20A/dm2、30A/dm2、
40A/dm2、50A/dm2Or 60A/dm2Deng it is not limited to cited numerical value, other interior unlisted numbers of the numberical range
It is worth equally applicable, preferably 20A/dm2。
In the present invention, when electrochemical polishing treatment, stainless steel is flattened as anode through electrochemical polish rear surface, can
So that the film layer more dense uniform that stainless steel surface is formed, and improve the corrosion resistance and wearability of film layer.
As currently preferred technical solution, the acid solution is Chrome-free acid solution.
In the present invention, acidic electrolysis bath used is free of chromium, mainly since the use of chromium, especially Cr VI can be right
Environment, which is brought, to be seriously affected, and " is limited according to " waste electronic andelectrical equipment instruction " (WEES instruction) and in electronic electric equipment
System use certain Hazardous Substances Directives " (ROHS instruction) requirement, should also reduce the use of chromium.
Preferably, the composition of the acid solution includes sulfuric acid, molybdenum salt, silver nitrate and lanthanide metal salt.
In the present invention, in the composition of the acid solution, boric acid is also can be used in addition to sulfuric acid in the acids；Molybdenum salt and chromium
Salt has similar chemical property, is to replace one of being preferably selected for chromium, while molybdenum can also improve stainless steel film layer table
The gloss in face；Silver has excellent antibacterial and mouldproof performance, and silver ion can activate the oxygen in air or water, generates hydroxyl free
Base and active oxygen ion have stronger oxidability, can destroy the proliferative capacity of bacterium in a short time, inhibit or kill thin
Bacterium；Lanthanide element can play catalytic action, improve the antibacterial action of silver, while improve corrosion resisting property.
Preferably, the composition of the acid solution further includes nickel salt and/or manganese salt.
In the present invention, nickel, manganese are also two kinds of usually used elements, itself also has stronger antibacterial, fungicidal properties.
Preferably, in the acid solution each component concentration be 300~500g/L of sulfuric acid, such as 300g/L, 350g/L,
400g/L, 450g/L or 500g/L etc.；Molybdenum 40~60g/L of salt, such as 40g/L, 45g/L, 50g/L, 55g/L or 60g/L etc.；Nitre
1~3g/L of sour silver, such as 1g/L, 1.5g/L, 2g/L, 2.5g/L or 3g/L etc.；5~10g/L of lanthanide metal salt, such as 5g/L,
6g/L, 7g/L, 8g/L, 9g/L or 10g/L etc.；5~20g/L of nickel salt, for example, 5g/L, 8g/L, 10g/L, 12g/L, 16g/L or
20g/L etc.；5~20g/L of manganese salt, such as 5g/L, 8g/L, 10g/L, 12g/L, 16g/L or 20g/L etc.；Above data is respective
It is not limited in cited numerical value in range, other unlisted numerical value are equally applicable in respective numberical range.
Preferably, the molybdenum salt includes ammonium molybdate and/or sodium molybdate.
Preferably, the lanthanide metal salt includes cerium salt, preferably cerous nitrate and/or cerous sulfate.
Preferably, the nickel salt and/or manganese salt include any one in nickel sulfate, manganese sulfate, nickel nitrate or manganese nitrate or
At least two combination, the combination is typical but non-limiting example has: the combination of nickel sulfate and manganese sulfate, nickel sulfate and nitric acid
The combination of the combination of nickel, nickel nitrate and manganese nitrate, nickel sulfate, manganese sulfate and combination of nickel nitrate etc..
As currently preferred technical solution, the alternating current is positive the electric current of negative direction checker.
Preferably, the time of the electric current checker is 3~10s of positive direction, such as 3s, 4s, 5s, 6s, 7s, 8s, 9s
Or 10s etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable；Negative direction 3
~10s, such as 3s, 4s, 5s, 6s, 7s, 8s, 9s or 10s etc., it is not limited to cited numerical value, in the numberical range its
His unlisted numerical value is equally applicable.
In the present invention, due to the effect of alternating current, stainless steel is alternately as anode and cathode, when electric current is positive,
Stainless steel is as anode, and under the oxidation of free radical, the metal simple-substance etc. in stainless steel is oxidized to form oxidation film, works as electricity
When stream is negative sense, for stainless steel as cathode, the functional metal ion in electrolyte can be deposited on the oxidation film formed when oxidation
The hole or cracks of layer, oxidation and deposition reaction alternately make functional ion have preferable hide in oxide layer
Property, so that anti-microbial property is more longlasting；Since the elements such as molybdenum, silver, nickel, manganese develop the color, by adjusting current density, oxidation or coloring
The technological parameters such as time can effectively adjust the color of final stainless steel, it is made to meet the market demand.
Preferably, the current density of the alternating current is 20~120mA/dm2, such as 20mA/dm2、40mA/dm2、
60mA/dm2、80mA/dm2、100mA/dm2Or 120mA/dm2Deng it is not limited to cited numerical value, in the numberical range
Other unlisted numerical value are equally applicable.
Preferably, the oxidation, coloring treatment temperature be 20~60 DEG C, such as 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C or 60
DEG C etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable；Time be 5~
30min, such as 5min, 10min, 15min, 20min, 25min or 30min etc., it is not limited to cited numerical value, the number
It is equally applicable to be worth other unlisted numerical value in range.
As currently preferred technical solution, the stainless steel is aoxidized, after coloring treatment, is first washed, in advance
Heat, then carry out sealing pores.
Preferably, the cleaning solution used that washs is deionized water.
Preferably, the preheating is that stainless steel is preheated to 50~70 DEG C, such as 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C or 70 DEG C
Deng it is not limited to cited numerical value, other unlisted numerical value are equally applicable in the numberical range.
As currently preferred technical solution, the sealing pores are that stainless steel is soaked in silicon sol solution, excellent
It is selected as vertically being soaked in silicon sol solution.
Preferably, the soaking time is 5~20s, such as 5s, 6s, 8s, 10s, 12s, 14s, 15s, 16s, 18s or 20s
Deng it is not limited to cited numerical value, other unlisted numerical value are equally applicable in the numberical range.
As currently preferred technical solution, after the sealing pores, stainless steel is dried.
Preferably, the drying temperature is 110~130 DEG C, such as 110 DEG C, 115 DEG C, 120 DEG C, 125 DEG C or 130 DEG C etc.,
It is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable.
Preferably, the drying temperature is 1~2h, such as 1h, 1.2h, 1.5h, 1.8h or 2h etc., it is not limited to institute
The numerical value enumerated, other interior unlisted numerical value of the numberical range are equally applicable.
As currently preferred technical solution, the described method comprises the following steps:
(1) stainless steel is successively mechanically polished, the pre-treatment of electrochemical deoiling and electrochemical polish, the electrochemistry is thrown
The temperature of light is 50~80 DEG C, and the time is 5~10min, and current density is 20~60A/dm2；
(2) stainless steel after step (1) pre-treatment is placed in Chrome-free acid solution, using positive negative direction checker
Alternating current aoxidized, coloring treatment, and the time of electric current checker is 3~10s of positive direction, 3~10s of negative direction, electric current
Density is 20~120mA/dm2, oxidation, coloring treatment temperature be 20~60 DEG C, the time be 5~30min；
(3) by step (2) oxidation, stainless steel washing, preheating after coloring treatment, be then soaked in silicon sol solution into
Row sealing pores, soaking time are 5~20s, obtain anti-bacteria stainless steel after dry.
Second aspect, the present invention provides a kind of anti-bacteria stainless steels obtained using above-mentioned preparation method.
Compared with prior art, the present invention at least has the advantages that
(1) present invention realizes alternating oxidation and the coloring of stainless steel surface by the way of alternating current, by a variety of
The synergistic effect of antiseptic elements, so that stainless steel has excellent antibacterial, mould proof, corrosion resisting property, sealing pores can be improved stainless
The wearability and glossiness of steel surface；
(2) the color multiplicity of present invention gained stainless steel product, and can be adjusted by changes in process parameters, can effectively it expire
The sufficient market demand, expanded application range；
(3) the method for the invention is easy, environmentally protective, and oxidation and the coloring of stainless steel carry out in same solution, raw
It is higher to produce efficiency, does not use chromium-containing solution, mitigates environmental pollution, meets the requirement of WEES and ROHS instruction.
Detailed description of the invention
Fig. 1 is the anti-bacteria stainless steel product of the offer of the embodiment of the present invention 1 and resisting for the stainless steel product without any processing
Bacterium property test result comparison diagram；
Wherein, 8739 bacterium colony of 1- Escherichia coli ATCC, 2- culture medium.
Specific embodiment
In order to better illustrate the present invention, be easy to understand technical solution, below the present invention is described in more detail.But it is following
Embodiment be only simple example of the invention, represent or limit the scope of the present invention, the present invention protect model
It encloses and is subject to claims.
Specific embodiment of the invention part provides a kind of preparation method of anti-bacteria stainless steel, which comprises
Stainless steel progress pre-treatment is placed in acid solution, is aoxidized using alternating current, coloring treatment, then
Sealing pores are carried out, anti-bacteria stainless steel is obtained.
The following are typical but non-limiting embodiments of the invention:
Embodiment 1:
The preparation method for present embodiments providing a kind of anti-bacteria stainless steel, the described method comprises the following steps:
(1) stainless steel is successively mechanically polished, the pre-treatment of electrochemical deoiling and electrochemical polish, uses sand paper first
Stainless steel surface is polished, then uses degreasing fluid oil removing, the degreasing fluid component includes sodium hydroxide 60g/L, carbonic acid
Sodium 30g/L and sodium phosphate 20g/L, treatment temperature are 50 DEG C, handle time 2min, and later using stainless steel as anode, graphite is yin
Pole, carries out electrochemical polish in polishing fluid, and polishing fluid component used includes: the sulphur of phosphoric acid 650mL/L, 98wt% of 85wt%
Sour 300mL/L, glycerine 50mL/L, the current density of electrochemical polish are 20A/dm2, temperature is 80 DEG C, time 5min；
(2) stainless steel after step (1) pre-treatment is placed in Chrome-free acid solution, the component of Chrome-free acid solution used
It include: sulfuric acid 400g/L, sodium molybdate 50g/L, silver nitrate 1.5g/L, cerous nitrate 5g/L, manganese sulfate 5g/L, nickel sulfate 8g/L,
Under the conditions of 50 DEG C, aoxidized using the alternating current of positive negative direction checker, coloring treatment, the time of electric current checker
For positive direction 5s, negative direction 5s, current density 50mA/dm2, the processing time is 10min；
(3) by stainless steel washing, the preheating after step (2) oxidation, coloring treatment, then vertically it is soaked in silicon sol solution
Middle carry out sealing pores, soaking time 5s, dry 1h under the conditions of 120 DEG C, obtains anti-bacteria stainless steel later.
Embodiment 2:
The preparation method for present embodiments providing a kind of anti-bacteria stainless steel, the described method comprises the following steps:
(1) stainless steel is successively mechanically polished, the pre-treatment of electrochemical deoiling and electrochemical polish, uses sand paper first
Stainless steel surface is polished, then uses degreasing fluid oil removing, the degreasing fluid component includes sodium hydroxide 45g/L, carbonic acid
Sodium 30g/L and sodium phosphate 15g/L, treatment temperature are 40 DEG C, handle time 3min, and later using stainless steel as anode, graphite is yin
Pole, carries out electrochemical polish in polishing fluid, and polishing fluid component used includes: the sulphur of phosphoric acid 600mL/L, 98wt% of 85wt%
Sour 350mL/L, glycerine 50mL/L, the current density of electrochemical polish are 30A/dm2, temperature is 70 DEG C, time 6min；
(2) stainless steel after step (1) pre-treatment is placed in Chrome-free acid solution, the component of Chrome-free acid solution used
It include: sulfuric acid 300g/L, sodium molybdate 60g/L, silver nitrate 3g/L, cerous nitrate 8g/L, manganese nitrate 15g/L, nickel nitrate 5g/L, 20
It under the conditions of DEG C, is aoxidized using the alternating current of positive negative direction checker, coloring treatment, the time of electric current checker is
Positive direction 10s, negative direction 10s, current density 20mA/dm2, the processing time is 30min；
(3) by stainless steel washing, the preheating after step (2) oxidation, coloring treatment, then vertically it is soaked in silicon sol solution
Middle carry out sealing pores, soaking time 8s, dry 1.5h under the conditions of 130 DEG C, obtains anti-bacteria stainless steel later.
Embodiment 3:
The preparation method for present embodiments providing a kind of anti-bacteria stainless steel, the described method comprises the following steps:
(1) stainless steel is successively mechanically polished, the pre-treatment of electrochemical deoiling and electrochemical polish, uses sand paper first
Stainless steel surface is polished, then uses degreasing fluid oil removing, the degreasing fluid component includes potassium hydroxide 50g/L, carbonic acid
Potassium 35g/L and potassium phosphate 20g/L, treatment temperature are 60 DEG C, handle time 1.5min, later using stainless steel as anode, graphite is
Cathode, carries out electrochemical polish in polishing fluid, and polishing fluid component used includes: phosphoric acid 700mL/L, 98wt% of 85wt%
Sulfuric acid 250mL/L, glycerine 50mL/L, the current density of electrochemical polish are 40A/dm2, temperature is 70 DEG C, time 7min；
(2) stainless steel after step (1) pre-treatment is placed in Chrome-free acid solution, the component of Chrome-free acid solution used
It include: sulfuric acid 500g/L, ammonium molybdate 40g/L, silver nitrate 1g/L, cerous sulfate 10g/L, nickel sulfate 20g/L, under the conditions of 60 DEG C,
It being aoxidized using the alternating current of positive negative direction checker, coloring treatment, the time of electric current checker is positive direction 3s,
Negative direction 3s, current density 120mA/dm2, the processing time is 5min；
(3) by stainless steel washing, the preheating after step (2) oxidation, coloring treatment, then vertically it is soaked in silicon sol solution
Middle carry out sealing pores, soaking time 15s, dry 2h under the conditions of 110 DEG C, obtains anti-bacteria stainless steel later.
Embodiment 4:
The preparation method for present embodiments providing a kind of anti-bacteria stainless steel, the described method comprises the following steps:
(1) stainless steel is successively mechanically polished, the pre-treatment of electrochemical deoiling and electrochemical polish, uses sand paper first
Stainless steel surface is polished, then uses degreasing fluid oil removing, the degreasing fluid component includes potassium hydroxide 45g/L, carbonic acid
Potassium 30g/L and potassium phosphate 20g/L, treatment temperature are 50 DEG C, handle time 2min, and later using stainless steel as anode, graphite is yin
Pole, carries out electrochemical polish in polishing fluid, and polishing fluid component used includes: the sulphur of phosphoric acid 550mL/L, 98wt% of 85wt%
Sour 400mL/L, glycerine 50mL/L, the current density of electrochemical polish are 60A/dm2, temperature is 50 DEG C, time 10min；
(2) stainless steel after step (1) pre-treatment is placed in Chrome-free acid solution, the component of Chrome-free acid solution used
Include: sulfuric acid 450g/L, sodium molybdate 45g/L, silver nitrate 2g/L, cerous nitrate 7g/L, under the conditions of 40 DEG C, is handed over using positive negative direction
For transformation alternating current aoxidized, coloring treatment, time of electric current checker is positive direction 4s, negative direction 8s, electric current
Density is 80mA/dm2, the processing time is 20min；
(3) by stainless steel washing, the preheating after step (2) oxidation, coloring treatment, then vertically it is soaked in silicon sol solution
Middle carry out sealing pores, soaking time 20s, dry 1h under the conditions of 125 DEG C, obtains anti-bacteria stainless steel later.
The anti-bacteria stainless steel product that embodiment 1-4 is prepared carries out following performance test respectively:
1. appearance and adhesive force test:
The stainless steel product appearance test method are as follows: under ordinary ray, range estimation inspection is carried out to product from different perspectives
It looks into, the adhesion test method of the stainless steel is carried out referring to GB/T 1720-1989 standard, and test result is as shown in table 1.
The appearance and adhesive force test result of anti-bacteria stainless steel product in 1 embodiment 1-4 of table
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Appearance | True qualities | It is pale yellow | It is deep yellow | It is pale yellow |
| Adhesive force | 1 grade | 1 grade | 1 grade | 1 grade |
2. corrosion resistance is tested:
The corrosion resistance test method are as follows: product is placed in the FeCl that mass concentration is 10%3In solution, soaking temperature
It is 30 DEG C, the rate of corrosion of test product after soaking time 1h, 1h.The calculation of rate of corrosion is rate of corrosion (%)=(corrosion
Weight after preceding weight-corrosion)/(weight before corroding) × 100%, test result is as shown in table 2.
The corrosion resistance test result of anti-bacteria stainless steel product in 2 embodiment 1-4 of table
As shown in Table 2, the rate of corrosion of gained anti-bacteria stainless steel product is no more than 0.4% in embodiment, corrosion resistance
It is excellent.
3. rub resistance is tested:
The rub resistance test method are as follows: moved horizontally, remembered along product surface using the erasing rubber that load is 500g
Times of exercise when film layer disappears is recorded, test result is as shown in table 3.
The rub resistance test result of anti-bacteria stainless steel product in 3 embodiment 1-4 of table
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Wearability (number) | 632 | 674 | 713 | 647 |
As shown in Table 3, in embodiment gained anti-bacteria stainless steel product the rubber friction for being amenable to 600 times or more, it is resistance to
Frictional behaviour is excellent.
4. antibiotic property is tested:
The antibiotic property test method are as follows: detected in strict accordance with ISO 22196-2011 professional standard, using large intestine
Bacillus ATCC 8739 and gold-coloured staphylococci ATCC 6538 investigates the bacteriostasis property of stainless steel product, test as test strain
The results are shown in Table 4.Wherein the anti-bacteria stainless steel product (left side) in embodiment 1 and the stainless steel product without any processing
(right side) is as shown in Figure 1 for the antibiotic property test result comparison diagram of test strain with Escherichia coli ATCC 8739.
The antibiotic property test result of anti-bacteria stainless steel product in 4 embodiment 1-4 of table
As shown in Table 4, in embodiment gained anti-bacteria stainless steel product to Escherichia coli ATCC 8739 and gold-coloured staphylococci
The antibiotic rate of ATCC 6538 has reached 99% or more, excellent antibacterial performance, and untreated stainless steel produces in blank test
Clump count increases instead after product terminate test, does not have antibiotic property.
5. fungus resistance is tested:
The fungus resistance test method are as follows: using aspergillus niger, thermophilic loose mould, ball hair shell, G virens and Aureobasidium pullulans
Stainless steel product is detected, observes 28 days, observes its mildew degree, grade scale is as shown in table 5.
The grade scale of mildew degree in the test of 5 fungus resistance of table
| It does not grow | 0 grade |
| Trace grows (< 10%) | 1 grade |
| Slight growth (>=10%~< 30%) | 2 grades |
| Moderate grows (>=30%~< 60%) | 3 grades |
| Severe growth (>=60%~covering comprehensively) | 4 grades |
According to grade scale in table 5, the present invention in embodiment 1-4 fungus resistance test in embodiment 2,3 and 4 length
Mould degree is 1 grade, and the mildew degree of embodiment 1 is 2 grades, and anti-fungi performance is excellent.
Comparative example 1:
This comparative example provides a kind of preparation method of anti-bacteria stainless steel, and the method is referring to the method in embodiment 1, area
Be not only that: step (2) uses unidirectional direct-current, and stainless steel makees cathode.
In this comparative example, using unidirectional direct-current, cathode is made with stainless steel, surface only carries out electrolyte intermediate ion
Deposition and coloring, and non-oxidation process, at this point, it is poor with the binding ability of stainless steel surface after functional ion deposition, it is easy
It falls off, the anti-microbial property of products obtained therefrom is not lasting.
Can be seen that the present invention with comparative example based on the above embodiments can realize stainless steel watch by the way of alternating current
The alternating oxidation in face and coloring, and the oxidation of stainless steel can be carried out with coloring in same solution, pass through a variety of antiseptic elements
Synergistic effect, so that stainless steel has excellent antibacterial, mould proof, corrosion resisting property, adjusts stainless steel by changes in process parameters
The color of product, then the wearability and glossiness of stainless steel surface can be improved by sealing pores；The method is easy, green ring
It protects, does not use chromium-containing solution, mitigate environmental pollution, meet the requirement of WEES and ROHS instruction.
The Applicant declares that the present invention is explained by the above embodiments method detailed of the invention, but the present invention not office
Be limited to above-mentioned method detailed, that is, do not mean that the invention must rely on the above detailed methods to implement.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., all of which fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. a kind of preparation method of anti-bacteria stainless steel, which is characterized in that the described method includes:
Stainless steel progress pre-treatment is placed in acid solution, is aoxidized using alternating current, coloring treatment, is then carried out
Sealing pores obtain anti-bacteria stainless steel.
2. preparation method according to claim 1, which is characterized in that the pre-treatment successively includes mechanical polishing, chemistry
Oil removing and electrochemical polish；
Preferably, the mechanical polishing is using sand paper progress surface polishing；
Preferably, the electrochemical deoiling is carried out using degreasing fluid；
Preferably, the composition of the degreasing fluid includes the phosphate of caustic alkali, the carbonate of alkali metal and alkali metal, preferably hydrogen
Sodium oxide molybdena, sodium carbonate and sodium phosphate.
3. preparation method according to claim 2, which is characterized in that the electrochemical polishing treatment in polishing fluid into
Row, using stainless steel as anode, using graphite as cathode；
Preferably, the composition of the polishing fluid includes phosphoric acid, sulfuric acid and glycerine；
Preferably, the volume ratio of the phosphoric acid, sulfuric acid and glycerine is (11~14): (5~8): 1；
Preferably, the temperature of the electrochemical polishing treatment is 50~80 DEG C, and the time is 5~10min；
Preferably, the current density of the electrochemical polishing treatment is 20~60A/dm2, preferably 20A/dm2。
4. preparation method according to claim 1-3, which is characterized in that the acid solution is that Chrome-free acidity is molten
Liquid；
Preferably, the composition of the acid solution includes sulfuric acid, molybdenum salt, silver nitrate and lanthanide metal salt；
Preferably, the composition of the acid solution further includes nickel salt and/or manganese salt；
Preferably, the concentration of each component is 300~500g/L of sulfuric acid, 40~60g/L of molybdenum salt, silver nitrate 1 in the acid solution
~3g/L, 5~10g/L of lanthanide metal salt, 5~20g/L of nickel salt, 5~20g/L of manganese salt；
Preferably, the molybdenum salt includes ammonium molybdate and/or sodium molybdate；
Preferably, the lanthanide metal salt includes cerium salt, preferably cerous nitrate and/or cerous sulfate；
Preferably, the nickel salt and/or manganese salt include any one in nickel sulfate, manganese sulfate, nickel nitrate or manganese nitrate or at least
Two kinds of combination.
5. preparation method according to claim 1-4, which is characterized in that the alternating current be positive negative direction friendship
For the electric current of transformation；
Preferably, the time of the electric current checker is 3~10s of positive direction, 3~10s of negative direction；
Preferably, the current density of the alternating current is 20~120mA/dm2；
Preferably, it is described oxidation, coloring treatment temperature be 20~60 DEG C, the time be 5~30min.
6. preparation method according to claim 1-5, which is characterized in that the stainless steel is aoxidized, coloured
It after processing, first washed, preheated, then carry out sealing pores；
Preferably, the cleaning solution used that washs is deionized water；
Preferably, the preheating is that stainless steel is preheated to 50~70 DEG C.
7. preparation method according to claim 1-6, which is characterized in that the sealing pores are to soak stainless steel
It steeps in silicon sol solution, is preferably vertically soaked in silicon sol solution；
Preferably, the soaking time is 5~20s.
8. preparation method according to claim 1-7, which is characterized in that after the sealing pores, by stainless steel
It is dried；
Preferably, the drying temperature is 110~130 DEG C；
Preferably, the drying temperature is 1~2h.
9. preparation method according to claim 1-8, which is characterized in that the described method comprises the following steps:
(1) stainless steel is successively mechanically polished, the pre-treatment of electrochemical deoiling and electrochemical polish, the electrochemical polish
Temperature is 50~80 DEG C, and the time is 5~10min, and current density is 20~60A/dm2；
(2) stainless steel after step (1) pre-treatment is placed in Chrome-free acid solution, using the alternation of positive negative direction checker
Electric current aoxidized, coloring treatment, and the time of electric current checker is 3~10s of positive direction, 3~10s of negative direction, current density
For 20~120mA/dm2, oxidation, coloring treatment temperature be 20~60 DEG C, the time be 5~30min；
(3) it by stainless steel washing, the preheating after step (2) oxidation, coloring treatment, is then soaked in silicon sol solution and is sealed
Hole processing, soaking time are 5~20s, obtain anti-bacteria stainless steel after dry.
10. a kind of anti-bacteria stainless steel obtained using the described in any item preparation methods of claim 1-9.
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Cited By (8)
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| CN111534844A (en) * | 2020-05-14 | 2020-08-14 | 东南大学 | Antibacterial stainless steel surface treatment device and method |
| CN111647926A (en) * | 2020-05-14 | 2020-09-11 | 东南大学 | Preparation method of antibacterial aluminum alloy by anodic oxidation |
| CN111778538A (en) * | 2020-07-06 | 2020-10-16 | 上海脉诺金属表面处理技术有限公司 | Antibacterial electrochemical oxidation liquid and electrochemical oxidation process for stainless steel |
| CN112160001A (en) * | 2020-09-25 | 2021-01-01 | 同曦集团有限公司 | Antibacterial, mildewproof and antiviral oxidized stainless steel and preparation method thereof |
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| CN112522773A (en) * | 2020-11-04 | 2021-03-19 | 东南大学 | Preparation method of stainless steel with antibacterial surface |
| CN112575355A (en) * | 2019-09-30 | 2021-03-30 | 浙江绍兴苏泊尔生活电器有限公司 | Cooking utensil and surface treatment method thereof |
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| CN101748470A (en) * | 2009-12-28 | 2010-06-23 | 常州佳得顺抗菌材料科技有限公司 | Antibacterial stainless steel with electrochemical oxidation film |
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| CN101748470A (en) * | 2009-12-28 | 2010-06-23 | 常州佳得顺抗菌材料科技有限公司 | Antibacterial stainless steel with electrochemical oxidation film |
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| CN112575355B (en) * | 2019-09-30 | 2023-11-14 | 浙江绍兴苏泊尔生活电器有限公司 | Cooking appliance and surface treatment method thereof |
| CN111647926A (en) * | 2020-05-14 | 2020-09-11 | 东南大学 | Preparation method of antibacterial aluminum alloy by anodic oxidation |
| CN111534844A (en) * | 2020-05-14 | 2020-08-14 | 东南大学 | Antibacterial stainless steel surface treatment device and method |
| CN111778538A (en) * | 2020-07-06 | 2020-10-16 | 上海脉诺金属表面处理技术有限公司 | Antibacterial electrochemical oxidation liquid and electrochemical oxidation process for stainless steel |
| CN112160001A (en) * | 2020-09-25 | 2021-01-01 | 同曦集团有限公司 | Antibacterial, mildewproof and antiviral oxidized stainless steel and preparation method thereof |
| CN112160001B (en) * | 2020-09-25 | 2021-07-27 | 同曦集团有限公司 | Antibacterial, mildewproof and antiviral oxidized stainless steel and preparation method thereof |
| CN112160007B (en) * | 2020-09-25 | 2022-02-08 | 同曦集团有限公司 | Antibacterial, mildewproof and antiviral electrophoresis stainless steel and preparation method thereof |
| CN112160007A (en) * | 2020-09-25 | 2021-01-01 | 同曦集团有限公司 | Antibacterial, mildewproof and antiviral electrophoresis stainless steel and preparation method thereof |
| CN112522773A (en) * | 2020-11-04 | 2021-03-19 | 东南大学 | Preparation method of stainless steel with antibacterial surface |
| CN112522773B (en) * | 2020-11-04 | 2022-01-28 | 东南大学 | Preparation method of stainless steel with antibacterial surface |
| CN114107970A (en) * | 2021-11-29 | 2022-03-01 | 深圳市诚达科技股份有限公司 | Normal-temperature preparation method of corrosion-resistant film on stainless steel surface |
| CN114107970B (en) * | 2021-11-29 | 2024-04-12 | 深圳市诚达科技股份有限公司 | Normal-temperature preparation method of corrosion-resistant film on stainless steel surface |
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