CN100434565C - Process for preparing anti-bacteria stainless steel by double-layer glowing method - Google Patents
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- CN100434565C CN100434565C CNB200510120596XA CN200510120596A CN100434565C CN 100434565 C CN100434565 C CN 100434565C CN B200510120596X A CNB200510120596X A CN B200510120596XA CN 200510120596 A CN200510120596 A CN 200510120596A CN 100434565 C CN100434565 C CN 100434565C
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Abstract
The present invention relates to a method for preparing antimicrobial stainless steel by a double-layer glowing metallic cementation method, which is characterized in that stainless steel base material to be treated is put in a double-layer glowing metallic cementation furnace to carry out the operation of antimicrobial element permeation, wherein the working condition of the antimicrobial element permeation comprises: the working air pressure in the double-layer glowing metallic cementation furnace is from 1.33 to 133 Pa, the source electrode voltage is from 0.7 to 1.4KV, the workpiece voltage is from 0.6 to 1.2KV, the temperature is from 800 to 1050 DEG C, the interelectrode distance is from 10 to 20mm, and the permeation time is from 2 to 4 hours. Antimicrobial elements are Cu elements or Ag elements, vacuum aging treatment is carried out after the permeation of the Cu elements, wherein the vacuum aging treatment time is from 1 to 10 hours, and the treatment temperature is from 450 to 900 DEG C. The present invention has the advantages of simple production process, maintenance of the original corrosion resistance of substrates and good bacteria resistance of the surface because the surface of the stainless steel has a diffusion layer which is rich in copper phases or silver phases.
Description
One, technical field
The present invention relates to a kind of method for preparing anti-bacteria stainless steel.Relate in particular to a kind of method for preparing anti-bacteria stainless steel with the double-deck glow metal cementation.
Two, technical background
At present, all generally adopt stainless material in a lot of fields, sanitary equipment, kitchen tools and the tableware etc. used as daily life not only require its light, attractive in appearance, and requirement can antibiotic and sterilizing, thereby the stainless steel with anti-microbial property just arises at the historic moment.Successively developed multiple anti-bacteria stainless steel in recent years with good antibacterial effect, as the Japanology personnel by with the stainless steel being research basis, obtaining integral body is anti-bacteria stainless steel, comprise NSS-AM series interpolation Cu anti-bacteria stainless steel, SUS304, R430AB, R430LN-AB add silver-colored anti-bacteria stainless steel and SUS340LX ferritic series and SUS30451 austenite anti-bacteria stainless steel.Domestic correlative study is as follows:
The stainless steel and the method for making thereof of anti-microbial property " improve " (CN 96114349.5) are through thermal treatments such as 500-900 ℃ of aging or annealing, not only on the top layer and this copper-rich phase precipitation from homogeneous solution inside and disperseing in the substrate.
" stainless steel of product having enhanced antibacterial action and manufacture method thereof " (CN99800249.6) make contain contain in the above stainless steel of Cr:10% (weight) among Ag, Sn, Zn, the Pt more than a kind or a kind, make being scattered in this stainless steel more than a kind or a kind in median size 500 μ m following silver particles, silver oxide and the silver-colored sulfide.In order to make silver particles, silver oxide and silver-colored sulfide homodisperse, the pouring speed of continuous casting should be at 0.8～1.6m/min.
" surperficial cupric anti-bacteria stainless steel and manufacturing process thereof " is that the cementation coating that contains ε-Cu, the copper content of cementation coating are arranged on the stainless steel substrate surface is 1.5～30wt% (CN02139264.1).Its technology is: stainless steel substrate is put into the penetration enhancer heating and kept carrying out in 2～10 hours solid solution aging again handle.
" a kind of method that adopts ion implantation to prepare anti-bacteria stainless steel " is to inject antibiotic ion Cu on stainless steel-based material surface or the Ag implantation dosage is 1 * 10 (CN1566397A)
16～1 * 10
18Cm
-2
The first two top technology all is by steel-making, continuous casting and rolling technology, in stainless steel integrated, add antibacterial metal ions Cu or Ag, because it is serious to add the Cu oxidation in the smelting process, recovery rate is low, and whole adding Cu or Ag have increased the cost of steel widely in the while stainless steel base.In addition, the red brittleness of Cu can cause operation of rolling cracking, rolling technology is required high." surperficial cupric anti-bacteria stainless steel and manufacturing process thereof " is though be that the technology that copper is equipped with anti-bacteria stainless steel is oozed on the surface, but when handling big part, the preparation of penetration enhancer, mixing and thermal treatment process subsequently all can increase labour intensity, " a kind of method that adopts ion implantation to prepare anti-bacteria stainless steel " employed ion implantation device involves great expense, and being difficult to handle abnormal member, range of application is restricted.
Three, summary of the invention
The purpose of this invention is to provide a kind of stainless steel surface that can make has the copper-rich phase of containing or argentiferous phase diffusion layer, can keep having good anti-microbial property on the original solidity to corrosion of the matrix basis and production technique is simple, the unrestricted anti-bacteria stainless steel preparation method of workpiece shape.
For achieving the above object, the technical solution adopted in the present invention is: pending stainless steel substrate is put into the double-deck glow metal leakage furnace carry out the antiseptic elements infiltration, the working conditions that antiseptic elements is infiltrated is, air pressure in the double-deck glow metal leakage furnace is 20～80Pa, source voltage is 1.0～1.4KV, and workpiece voltage is 0.6～0.9KV, and temperature is 880～1050 ℃, interpole gap is 10～20mm, and the infiltration time is 2～4 hours.Antiseptic elements or be Cu element or for the Ag element; Must carry out vacuum aging after the Cu element infiltrates and handle, the time that vacuum aging is handled is 1～10 hour, and treatment temp is 450～900 ℃.
Wherein: pending stainless steel substrate or be martensite or for austenite or for ferrite; The antiseptic elements infiltration capacity is that the Cu element is that 0.2～5.0wt%, Ag amount of element are 0.001～0.2wt%; Working gas or be argon gas or for nitrogen or for hydrogen or be two or more mixed gas wherein.
Because adopt technique scheme, stainless steel surface has the copper-rich phase of containing or argentiferous phase diffusion layer, keeping having good anti-microbial property on the original solidity to corrosion of the matrix basis.Therefore the present invention has solidity to corrosion height, technology is simple, the workpiece shape is unrestricted and anti-microbial property is strong characteristics.The present invention compares with other whole method for making steel, also can avoid the high and easy rimose problem of the operation of rolling of stainless steel integrated copper content.
Four, embodiment
A kind of method that is equipped with martensite antimicrobial stainless steel with the double-deck glow legal system of embodiment ()
1, a kind of concrete processing step that adopts the preparation of double-deck glow method to contain the Cu martensite antimicrobial stainless steel is as follows:
(1) body material is a Martensite Stainless Steel, and its weight percentage is C:0.08～0.45wt%; Cr:12～14wt%; Si :≤0.6wt%; Mn :≤0.8wt%; Cu :≤0.1wt%; All the other are Fe.
(2) above-mentioned Martensite Stainless Steel base material is put into carried out the surface in the double-deck glow metal leakage furnace and ooze copper, the pressure of argon gas is 20～80Pa, and source voltage is 1.2～1.4kV, workpiece voltage is 0.7～0.9kV, temperature is 900～1050 ℃, and interpole gap is 10～20mm, and the treatment time is 2～4 hours.Cu element infiltration capacity is 2.5～3.5wt%.
(3) carry out vacuum aging and handle, the treatment time is 2～10 hours, and treatment temp is 500～800 ℃.
2, a kind of concrete processing step that adopts the preparation of double-deck glow method to contain the Ag martensite antimicrobial stainless steel is as follows:
(1) body material is a Martensite Stainless Steel, and its weight percentage is C:0.08～0.45wt%; Cr:12～14wt%; Si :≤0.6wt%; Mn :≤0.8wt%; Cu :≤0.1wt%; All the other are Fe.
(2) above-mentioned Martensite Stainless Steel base material is put into carried out the surface in the double-deck glow metal leakage furnace and ooze silver, the pressure of argon gas is 20～80Pa, source voltage 1.0～1.2kV, workpiece voltage 0.6～0.8kV, 880～950 ℃ of temperature, interpole gap 10～20mm, 2～4 hours treatment times; The infiltration capacity of Ag element is 0.03～0.1wt%.
A kind of method that is equipped with austenite antimicrobial stainless steel with the double-deck glow legal system of embodiment (two)
1, a kind of concrete processing step that adopts the preparation of double-deck glow method to contain the Cu austenite antimicrobial stainless steel is as follows:
(1) body material is an austenitic stainless steel, and its weight percentage is C:0.01～0.15wt%; Cr:16～20wt%; Ni:8～10wt%; Si :≤1.00wt%; Mn :≤2.00wt%; Cu :≤0.10wt%; All the other are Fe.
(2) above-mentioned austenite stainless steel substrate is put into carried out the surface in the double-deck glow metal leakage furnace and ooze copper, the pressure of argon gas is 20～80Pa, source voltage 1.2～1.4kV, workpiece voltage 0.7～0.9kV, 900～1050 ℃ of temperature, interpole gap 10～20mm, 2～4 hours treatment times.The infiltration capacity of Cu element is 3.0～5.0wt%.
(3) carry out vacuum aging and handle, the treatment time is 2～10 hours, and treatment temp is 500～800 ℃.
2, a kind of concrete processing step that adopts the preparation of double-deck glow method to contain the Ag austenite antimicrobial stainless steel is as follows:
(1) body material is an austenitic stainless steel, and its weight percentage is C:0.01～0.15wt%; Cr:16～20wt%; Ni:8～10wt%; Si :≤1.00wt%; Mn :≤2.00wt%; Cu :≤0.10wt%; All the other are Fe.
(2) above-mentioned austenite stainless steel substrate is put into carried out the surface in the double-deck glow metal leakage furnace and ooze silver, the pressure of argon gas is 20～80Pa, source voltage 1.0～1.2kV, workpiece voltage 0.6～0.8kV, 880～950 ℃ of temperature, interpole gap 10～20mm, 2～4 hours treatment times.The infiltration capacity of Ag element is 0.01～0.06wt%.
A kind of method that is equipped with ferrite antibacterial stainless steel with the double-deck glow legal system of embodiment (three)
1, a kind of concrete processing step that adopts the preparation of double-deck glow method to contain the Cu ferrite antibacterial stainless steel is as follows:
(1) body material is a ferritic stainless steel, and its weight percentage is: C:0.08～0.15wt%; Cr:10～18wt%; Si :≤1.00wt%; Mn :≤0.8wt%; Cu :≤0.10wt%; All the other are Fe.
(2) above-mentioned ferrite stainless steel substrate is put into carried out the surface in the double-deck glow metal leakage furnace and ooze copper, the pressure of argon gas is 20～80Pa, and source voltage is 1.2～1.4kV, workpiece voltage is 0.7～0.9kV, temperature is 900～1050 ℃, and interpole gap is 10～20mm, and the treatment time is 2～4 hours.The infiltration capacity of Cu element is 1.0～2.0wt%.
(3) vacuum aging is handled, and the treatment time is 2～10 hours, and temperature is 500～800 ℃.
2, a kind of concrete processing step that adopts the preparation of double-deck glow method to contain the Ag ferrite antibacterial stainless steel is as follows:
(1) body material is a ferritic stainless steel, and its weight percentage is: C:0.08～0.15wt%; Cr:10～18wt%; Si :≤1.00wt%; Mn :≤0.8wt%; Cu :≤0.10wt%; All the other are Fe.
(2) stainless steel substrate is carried out the surface in the double-deck glow metal leakage furnace and ooze silver, the pressure of argon gas is 20～80Pa, source voltage 1.0～1.2kV, workpiece voltage 0.6～0.8kV, 880～950 ℃ of temperature, interpole gap 10～20mm, 2～4 hours treatment times.The infiltration capacity of Ag element is 0.01～0.05wt%.
The germ resistance experiment: it is agar plate method that the present invention adopts antibacterial experiment, and the bacterial classification that uses is staphylococcus aureus and intestinal bacteria.
Experimental arrangement is as follows:
1,99.95% alcoholic acid absorbent cotton is clean with sample, degreasing with containing.
2, intestinal bacteria or staphylococcus aureus are scattered in the 1/500NB solution.
3, bacterium liquid is inoculated on the sample.
4, on the test surface, cover the lining film.
5, keep this test body to reach the scheduled time (24h) in temperature (35 ± 1.0 ℃), the condition of RH (relative humidity) more than 90%.
6, with the agar culture method (35 ± 1.0 ℃ ,≤24h) measure the viable bacteria rate.
The sterilization rate of anti-microbial property after with experiment estimated, the sterilization rate branch " ,+, ++, +++" four grades,
The no antibiotic effect of "-" expression, "+" represents sterilization rate about 50%, ' ++ " represent sterilization rate about 80%, " +++" represent that sterilization rate is more than 99%.
Sterilization rate is pressed the following formula definition:
In the formula: contrast bacterium number is the viable count carry out antibacterial experiment in the sterilization agar plate after;
Bacterium number after the experiment is the viable count that the experiment back is measured.
Antibacterial experiment result (seeing Table 1) shows, does not infiltrate sample and does not have any antibacterial effect, and embodiment shows good antibacterial effect to intestinal bacteria and staphylococcus aureus.
Table 1 antibacterial experiment result
Claims (4)
1, a kind of method that adopts the double-deck glow legal system to be equipped with anti-bacteria stainless steel, it is characterized in that pending stainless steel substrate is put into the double-deck glow metal leakage furnace carries out the antiseptic elements infiltration, the working conditions that antiseptic elements is infiltrated is, air pressure in the double-deck glow metal leakage furnace is 20～80Pa, source voltage is 1.0～1.4KV, and workpiece voltage is 0.6～0.9KV, and temperature is 880～1050 ℃, interpole gap is 10～20mm, and the infiltration time is 2～4 hours; Antiseptic elements or be Cu element or for the Ag element must be carried out vacuum aging after the Cu element infiltrates and be handled, and the vacuum aging treatment time is 1～10 hour, and treatment temp is 450～900 ℃.
2, employing double-deck glow legal system according to claim 1 is equipped with the method for anti-bacteria stainless steel, it is characterized in that described antiseptic elements infiltration capacity is: the Cu element is that 0.2～5.0wt%, Ag amount of element are 0.001～0.2wt%.
3, employing double-deck glow legal system according to claim 1 is equipped with the method for anti-bacteria stainless steel, it is characterized in that described pending stainless steel substrate or for martensite or for austenite or for ferrite.
4, employing double-deck glow legal system according to claim 1 is equipped with the method for anti-bacteria stainless steel, it is characterized in that described working gas or for argon gas or for nitrogen or for hydrogen or be two or more mixed gas wherein.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101880860B (en) * | 2010-05-29 | 2012-04-11 | 太原理工大学 | Preparation method of stainless steel surface copper-silver diffusion coating layer |
| CN102181822B (en) * | 2011-03-24 | 2013-11-06 | 桂林电子科技大学 | Antibacterial stainless steel with copper-cerium-containing surface, and application and preparation process thereof |
| CN102676986B (en) * | 2012-05-03 | 2014-03-19 | 太原理工大学 | Method for preparing silver leaching layer on surface of titanium dental implant |
| CN103088285B (en) * | 2013-01-15 | 2016-02-17 | 太原理工大学 | A kind of preparation method of corronel cementation coating |
| CN103991250B (en) * | 2014-04-30 | 2016-05-04 | 华南理工大学 | Anti-bacteria stainless steel of a kind of surperficial argentiferous and preparation method thereof |
| CN109338324A (en) * | 2018-11-27 | 2019-02-15 | 南京航空航天大学 | A kind of resistance to marime fouling of Q235 steel surface seeps layers of copper and the preparation method and application thereof |
| CN114717508A (en) * | 2020-12-22 | 2022-07-08 | 武汉苏泊尔炊具有限公司 | Antibacterial cutter and manufacturing method thereof |
| CN114369808B (en) * | 2021-12-20 | 2024-02-06 | 中国兵器科学研究院宁波分院 | Method for preparing antibacterial coating on surface of magnesium and magnesium alloy |
Citations (3)
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| CN1214374A (en) * | 1998-10-14 | 1999-04-21 | 太原理工大学 | Surface metallurgical technology to precipitate hardened stainless steel |
| JPH11277104A (en) * | 1998-03-25 | 1999-10-12 | Nisshin Steel Co Ltd | Manufacture of copper-containing austenitic stainless steel strip |
| CN1566397A (en) * | 2003-07-04 | 2005-01-19 | 武汉科技大学 | Process for preparing antibacterial stainless steel using ion-implantation method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11277104A (en) * | 1998-03-25 | 1999-10-12 | Nisshin Steel Co Ltd | Manufacture of copper-containing austenitic stainless steel strip |
| CN1214374A (en) * | 1998-10-14 | 1999-04-21 | 太原理工大学 | Surface metallurgical technology to precipitate hardened stainless steel |
| CN1566397A (en) * | 2003-07-04 | 2005-01-19 | 武汉科技大学 | Process for preparing antibacterial stainless steel using ion-implantation method |
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