CN116377378A - Preparation method of wear-resistant antibacterial stainless steel - Google Patents
Preparation method of wear-resistant antibacterial stainless steel Download PDFInfo
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- CN116377378A CN116377378A CN202310150514.4A CN202310150514A CN116377378A CN 116377378 A CN116377378 A CN 116377378A CN 202310150514 A CN202310150514 A CN 202310150514A CN 116377378 A CN116377378 A CN 116377378A
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- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 34
- 239000010935 stainless steel Substances 0.000 title claims abstract description 34
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000005121 nitriding Methods 0.000 claims abstract description 20
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 13
- 239000000956 alloy Substances 0.000 claims abstract description 13
- 238000009792 diffusion process Methods 0.000 claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 230000018199 S phase Effects 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 229910052786 argon Inorganic materials 0.000 claims description 11
- 230000001105 regulatory effect Effects 0.000 claims description 11
- 238000005498 polishing Methods 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 229910000963 austenitic stainless steel Inorganic materials 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000005275 alloying Methods 0.000 abstract description 11
- 238000005516 engineering process Methods 0.000 abstract description 7
- 239000011159 matrix material Substances 0.000 abstract description 6
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 229910000619 316 stainless steel Inorganic materials 0.000 description 16
- 239000010410 layer Substances 0.000 description 16
- 229910003460 diamond Inorganic materials 0.000 description 6
- 239000010432 diamond Substances 0.000 description 6
- 241000894006 Bacteria Species 0.000 description 5
- 230000001580 bacterial effect Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000003242 anti bacterial agent Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 241000588724 Escherichia coli Species 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000009977 dual effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000012136 culture method Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000007102 metabolic function Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000005180 public health Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C12/00—Solid state diffusion of at least one non-metal element other than silicon and at least one metal element or silicon into metallic material surfaces
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Abstract
The invention discloses a preparation method of wear-resistant and antibacterial stainless steel, which is characterized in that a 316L stainless steel matrix sample is subjected to composite modification of a double glow plasma alloying Ag permeation technology and a low temperature plasma nitriding technology, and an Ag-N composite alloy layer consisting of an Ag diffusion layer and an S-phase diffusion layer is formed on the surface of the stainless steel, so that the wear-resistant and antibacterial effects are achieved.
Description
Technical Field
The invention belongs to the technical field of metal surface modification, and particularly relates to a preparation method of wear-resistant antibacterial stainless steel.
Background
The 316L austenitic stainless steel is one of the metal materials inseparable in life because of good processability and comprehensive mechanical properties, especially corrosion resistance, and is particularly widely used in the fields of food processing, medical equipment, public health and the like. However, the alloy also has some defects, such as low hardness and wear resistance, and no antibacterial property, so that wider application is limited; with the development of society, the improvement of the living standard of people and the enhancement of health consciousness, people put higher demands on stainless steel products, and the stainless steel products can be endowed with good wear resistance and antibacterial performance on the premise of not reducing the corrosion resistance, so that the stainless steel products are problems to be solved.
The antibacterial property of the antibacterial stainless steel is generally achieved by adding a metal antibacterial element such as Ag or Cu. However, the integral addition of the antibacterial agent for preparing the antibacterial stainless steel has a plurality of defects, such as: (1) complex production process; the whole antibacterial stainless steel is added with excessive antibacterial agent, so that the problem of easy cracking in the rolling process exists, and the existing steelmaking process needs to be adjusted. (2) low resource utilization; the area of the antibacterial stainless steel which has the antibacterial effect is the surface contacted with bacteria, namely the surface layer of the stainless steel has antibacterial performance so as to meet the antibacterial requirement, and the integral addition of the antibacterial agent tends to cause the waste of expensive metals such as Ag, zn and the like.
Aiming at specific use characteristics of the antibacterial stainless steel, the preparation of the antibacterial stainless steel by a surface modification method can be considered, and the double glow alloying plasma surface modification technology can save cost, and is environment-friendly and energy-saving; the low-temperature plasma nitriding technology can form high-hardness expanded austenite, namely an S-phase layer, on the surface of the austenitic stainless steel; therefore, the invention is hopeful to form an Ag-N composite alloy layer comprising an Ag diffusion layer and an S phase diffusion layer on the surface of the stainless steel by carrying out composite modification of a double glow plasma alloying Ag permeation technology and a low temperature plasma nitriding technology on a 316L stainless steel substrate sample, thereby achieving the effects of wear resistance and bacteria resistance.
Disclosure of Invention
The invention aims to provide a preparation method of wear-resistant antibacterial stainless steel, wherein an Ag-N composite alloy layer consisting of an Ag diffusion layer and an S-phase diffusion layer is formed on the surface of the stainless steel, so that the wear-resistant antibacterial effect is achieved.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a preparation method of wear-resistant antibacterial stainless steel comprises the following steps:
s1, firstly cutting a 316L austenitic stainless steel plate into cuboid small samples with 15 multiplied by 5mm by linear cutting, then sequentially grinding the surfaces of the samples by using 240# water abrasive paper, 400# water abrasive paper, 800# water abrasive paper, 1200# water abrasive paper and 2000# water abrasive paper, and then respectively using 1μm and 0.5μm, polishing the diamond polishing paste, finally cleaning the diamond polishing paste in an ultrasonic cleaner by using acetone and deionized water, drying the diamond polishing paste, and sealing the diamond polishing paste in absolute ethyl alcohol for later use;
s2, placing an Ag plate at a source position, placing a matrix sample on a cathode disc, adjusting the polar distance to be 15mm, vacuumizing, and filling a large amount of argon into a furnace to bombard the sample and the Ag plate for 30min so as to achieve the purposes of cleaning and activating the surface of the sample; the source voltage is regulated to 600-1000V, the cathode voltage is regulated to 650-750V, the furnace pressure is regulated to 30-200 Pa, and the temperature is controlled to be about 890-920 ℃;
s3, ag-N co-permeation can be divided into two steps, wherein argon gas is introduced in the first step, and the Ag plate is bombarded to enable ions to be sputtered and deposited on the surface of a sample for 3 hours, 4 hours and 5 hours respectively; after the heat preservation is finished, the source voltage is turned off, then the cathode voltage is turned off, and argon is turned off when the temperature is cooled to room temperature; secondly, taking out the sample, putting the sample into a plasma low-temperature nitriding furnace, vacuumizing, and introducing gas to clean the sample for 20 min, wherein the gas is hydrogen for cleaning; then H2 and N2 are introduced, the H2: N2 = 3:1, the furnace pressure is regulated to be 300-350 Pa, the nitriding temperature is controlled to be about 350-400 ℃, the working vacuum degree is 300Pa, the pulse voltage is 650V, the current is 20A, the nitriding heat preservation time is 6-15H, and finally the Ag-N composite alloy layer consisting of the Ag diffusion layer and the S-phase diffusion layer is formed.
Preferably, in S2, the furnace temperature of the infiltrated Ag is 900 ℃.
Preferably, in S4, the nitriding temperature is 380 ℃.
Preferably, in S4, the nitriding incubation time is 12 hours.
The invention has the beneficial effects that: according to the invention, an environment-friendly and energy-saving double glow plasma alloying technology is adopted to perform surface Ag-N co-permeation on 316L stainless steel to prepare the antibacterial stainless steel, and an Ag-N co-permeation alloy layer is formed on the surface of the stainless steel to achieve the effects of wear resistance and bacteria resistance.
Drawings
FIG. 1 is an XRD pattern reflecting the Ag-infiltrated treatment and double glow Ag-N co-infiltration treatment of 316L stainless steel according to an embodiment of the present invention.
FIG. 2 is a diagram showing the gold phase of a 316L stainless steel treated by low temperature nitriding and double glow alloying Ag-N co-cementation according to an embodiment of the present invention.
FIG. 3 is an EDS diagram reflecting a dual glow alloying Ag-N co-diffusion treatment of 316L stainless steel in accordance with an embodiment of the present invention.
FIG. 4 is a graph showing the surface hardness and cross-sectional hardness of a sample of 316 stainless steel substrate subjected to low temperature nitriding treatment and Ag-N co-cementation treatment according to an embodiment of the present invention.
FIG. 5 is a graph of friction coefficient versus time reflecting abrasion of samples S1, S2, S3 under a load of 10N after a high temperature double glow alloying Ag-N co-diffusion treatment of 316L stainless steel according to an embodiment of the present invention,
FIG. 6 is a graph showing a 12h plate incubation at 37℃for a 316 stainless steel substrate sample, a low temperature nitriding sample, and a high temperature alloying Ag-N co-cementation sample, respectively, according to an embodiment of the present invention.
FIG. 7 is an XRD pattern reflecting samples Ag3SS, ag4SS, and Ag5SS after treatment with high temperature dual glow alloying Ag according to an embodiment of the present invention.
FIG. 8 is a graph of friction coefficient versus time reflecting wear of samples Ag3SS, ag4SS, ag5SS under a load of 10N after treatment with high temperature double glow alloying Ag for 316L stainless steel according to an embodiment of the present invention.
Description of the embodiments
For a better description of the present invention, the technical solution of the present invention will be easily understood, and the present invention will be further described in detail with reference to the accompanying drawings and the specific embodiments. It is to be understood that the following examples are provided for illustration only and are not intended to represent or limit the scope of the invention as claimed.
The reagents or apparatus used in the examples below are conventional products available commercially without the manufacturer's knowledge.
Examples
The test material is 316L austenitic stainless steel, and the standard mark is 0Cr17Ni12Mo2. Firstly, according to the size requirement of a test block required by a subsequent experiment, cutting a 316L austenitic stainless steel plate into a cuboid small sample with the size of 15 multiplied by 5mm by wire cutting, sequentially grinding the surfaces of the sample by using 240# water abrasive paper, 400# water abrasive paper, 800# water abrasive paper, 1200# water abrasive paper and 2000# water abrasive paper, polishing by using diamond polishing paste with the size of 1 mu m and 0.5 mu m respectively, finally cleaning by using acetone and deionized water in an ultrasonic cleaner, drying, and sealing in absolute ethyl alcohol for standby.
Placing a silver plate at a source electrode position, placing a matrix sample on a cathode disc, adjusting the polar distance to be 15mm, vacuumizing, and charging a large amount of argon into a furnace to bombard the sample and the Ag plate for 30min so as to achieve the purposes of cleaning and activating the surface of the sample; regulating the source voltage to 1000V, the cathode voltage to 650V-750V, the furnace pressure to 30-200 Pa, and controlling the temperature to about 900 ℃; ag-N co-permeation can be divided into two steps, wherein argon is introduced into the first step, and the Ag plate is bombarded to enable ions to be sputtered and deposited on the surface of a sample for 3h,4h and 5h respectively; after the heat preservation is finished, the source voltage is turned off, then the cathode voltage is turned off, and argon is turned off when the temperature is cooled to room temperature; and secondly, performing plasma low-temperature nitriding process on the sample subjected to Ag permeation, wherein the temperature is 380 ℃, the ratio of H2 to N2=3:1, the nitriding heat preservation time is 12 hours, and finally, an Ag-N composite alloy layer consisting of an Ag deposition layer and an S-phase diffusion layer is formed on the surface of the sample. The samples are marked by the alloy ionization Ag permeation time, and the corresponding samples are marked as S1, S2 and S3 according to the Ag permeation time.
According to the method, the antibacterial detection of the 316L stainless steel matrix, the plasma low-temperature nitriding sample and the plasma alloying Ag-N co-permeation samples acting on the escherichia coli for 1h, 6h and 12h is analyzed by a plate culture method, and as can be seen from fig. 4, the matrix sample SS and the plasma low-temperature nitriding sample NSS do not have antibacterial effects, and after three Ag-N co-permeation process samples are contacted with the escherichia coli for different time, the three Ag-N co-permeation process samples all show different antibacterial performances, and in general, the antibacterial rate of the sample S3 is best, the antibacterial rate reaches 93% after the sample acts on bacterial colonies for 6h, and the longer the acting time is, the more obvious the antibacterial rate is; from the aspect of antibacterial mechanism, the Ag-containing alloy layer of the sample S3 is thickest, and more Ag ions in the surface alloy layer are separated out under the action of longer time, so that the concentration of the alloy ions in bacterial liquid is continuously increased along with the increase of time, and finally the Ag ions penetrate the bacterial cell wall, so that bacterial enzymes and proteins are inactivated, and the metabolism function of bacteria is destroyed to cause death of the bacteria.
Examples
The test material is 316L austenitic stainless steel, and the standard mark is 0Cr17Ni12Mo2. Firstly, according to the size requirement of a test block required by a subsequent experiment, cutting a 316L austenitic stainless steel plate into a cuboid small sample with the size of 15 multiplied by 5mm by wire cutting, sequentially grinding the surfaces of the sample by using 240# water abrasive paper, 400# water abrasive paper, 800# water abrasive paper, 1200# water abrasive paper and 2000# water abrasive paper, polishing by using diamond polishing paste with the size of 1 mu m and 0.5 mu m respectively, finally cleaning by using acetone and deionized water in an ultrasonic cleaner, drying, and sealing in absolute ethyl alcohol for standby.
Placing a silver plate at a source electrode position, placing a matrix sample on a cathode disc, adjusting the polar distance to be 15mm, vacuumizing, and charging a large amount of argon into a furnace to bombard the sample and the Ag plate for 30min so as to achieve the purposes of cleaning and activating the surface of the sample; regulating the source voltage to 1000V, the cathode voltage to 650-750V, the furnace pressure to 30-200 Pa, and controlling the temperature to about 900 ℃; and (3) carrying out Ag permeation, namely introducing argon, bombarding an Ag plate to enable ions to be sputtered and deposited on the surface of the sample for 3 hours, 4 hours and 5 hours respectively. And marking the samples by using the Ag permeation time of the alloy ionization, wherein the corresponding samples are respectively marked as Ag3SS, ag4SS and Ag5SS.
Claims (4)
1. The preparation method of the wear-resistant antibacterial stainless steel is characterized by comprising the following steps of:
s1, firstly cutting a 316L austenitic stainless steel plate into a sample, grinding the surface of the sample, polishing the sample, finally cleaning the sample in an ultrasonic cleaner by using acetone and deionized water, drying the sample, and sealing the sample in absolute ethyl alcohol for later use;
s2, placing the Ag plate at the source position, placing the sample on a cathode disc, adjusting the electrode distance to be 10-20mm, vacuumizing, and charging argon into the furnace to bombard the sample and the Ag plate for 20-40min so as to achieve the purposes of cleaning and activating the surface of the sample; the source voltage is regulated to 600-1000V, the cathode voltage is regulated to 650-750V, the furnace pressure is regulated to 30-200 Pa, and the temperature is controlled to 890-920 ℃;
s3, ag-N co-permeation can be divided into two steps, wherein argon is introduced into the first step, and the Ag plate is bombarded to enable ions to be sputtered and deposited on the surface of the sample for 3-5 hours; after the heat preservation is finished, the source voltage is turned off, then the cathode voltage is turned off, and argon is turned off when the temperature is cooled to room temperature; secondly, taking out the sample, putting the sample into a plasma low-temperature nitriding furnace, vacuumizing, and introducing gas to clean the sample for 10-30min; then H2 and N2 are introduced, the H2: N2 = 3:1, the furnace pressure is regulated to be 300-350 Pa, the nitriding temperature is regulated to be 350-400 ℃, the working vacuum degree is 250-300Pa, the pulse voltage is 550-650V, the current is 10-30A, the nitriding heat preservation time is 9-14H, and finally the Ag-N composite alloy layer consisting of the Ag diffusion layer and the S-phase diffusion layer is formed.
2. The method for producing a wear-resistant and antibacterial stainless steel according to claim 1, wherein in S2, the furnace temperature of Ag-infiltrated is 900 ℃.
3. The method for producing a wear-resistant and antibacterial stainless steel according to claim 1, wherein in S4, the nitriding temperature is 380 ℃.
4. The method for preparing wear-resistant and antibacterial stainless steel according to claim 1, wherein in the step S4, nitriding heat preservation time is 12 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202310150514.4A CN116377378A (en) | 2023-02-22 | 2023-02-22 | Preparation method of wear-resistant antibacterial stainless steel |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310150514.4A CN116377378A (en) | 2023-02-22 | 2023-02-22 | Preparation method of wear-resistant antibacterial stainless steel |
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| CN116377378A true CN116377378A (en) | 2023-07-04 |
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- 2023-02-22 CN CN202310150514.4A patent/CN116377378A/en active Pending
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