CN113755830A - Production process of surface modified stainless steel and surface modified stainless steel - Google Patents
Production process of surface modified stainless steel and surface modified stainless steel Download PDFInfo
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- CN113755830A CN113755830A CN202111001666.5A CN202111001666A CN113755830A CN 113755830 A CN113755830 A CN 113755830A CN 202111001666 A CN202111001666 A CN 202111001666A CN 113755830 A CN113755830 A CN 113755830A
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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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/50—Treatment of iron or alloys based thereon
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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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/40—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates
- C23C22/42—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates containing also phosphates
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Abstract
The application relates to the technical field of stainless steel, and particularly discloses a production process of surface modified stainless steel and the surface modified stainless steel. The surface modified stainless steel is obtained by modifying a stainless steel substrate with a modifying solution, wherein the modifying solution comprises the following raw materials in parts by weight: 30-50 parts of silica sol, 8-12 parts of persulfate, 10-20 parts of passivator and 8-12 parts of montmorillonite, wherein the passivator has oxidability. The modification liquid disclosed by the application can be used for modifying the surface of the stainless steel substrate, is beneficial to reducing the possibility of stripping of a passive film, and improves the protection effect on the stainless steel substrate.
Description
Technical Field
The application relates to the technical field of stainless steel, in particular to a production process of surface modified stainless steel and the surface modified stainless steel.
Background
Stainless steel is short for stainless acid-resistant steel, has excellent corrosion resistance and can resist corrosion of various corrosive media such as air, steam, water and the like. In actual use, the worn area of the stainless steel surface can induce pitting corrosion, which affects the service life of the stainless steel. In order to reduce the influence of the pitting phenomenon on the service life of stainless steel, it is required to improve the wear resistance of stainless steel.
In the related art, a surface-modified stainless steel is prepared by the following method: (1) cleaning and decontaminating a stainless steel substrate; (2) soaking the cleaned and decontaminated stainless steel substrate in a passivating agent for 15-30min, and taking out, wherein the passivating agent is a nitric acid solution with the mass fraction of 30% -35%; (3) flushing the stainless steel substrate by using water flow, wherein the flushing time is 10-20 min; (4) soaking the stainless steel matrix in 75-95 deg.C water for 5-10min, taking out, and drying to obtain surface modified stainless steel. The surface of the stainless steel matrix treated by the passivating agent generates a passivating film, and the passivating film increases the density of the surface of the stainless steel matrix, so that the corrosion resistance of the stainless steel matrix is improved.
In view of the above-described related art, the inventors believe that, in the related art, although the passivation film improves the corrosion resistance of the stainless steel substrate, the thickness of the passivation film is limited because the stainless steel substrate hinders the penetration of the passivating agent. When the concentration of external corrosive substances is high, the passive film is easy to peel off, and the protection effect of the passive film on the stainless steel substrate is influenced.
Disclosure of Invention
In the related art, when the concentration of external corrosive substances is high, the passivation film is easy to peel off, and the protection effect on the stainless steel substrate is influenced. In order to improve the defect, the application provides a production process of the surface modified stainless steel and the surface modified stainless steel.
In a first aspect, the present application provides a process for producing a surface-modified stainless steel, which adopts the following technical scheme: a production process of surface modified stainless steel comprises the following steps:
(1) preparing a modification liquid, preheating the modification liquid to 40-80 ℃, wherein the formula of the modification liquid comprises the following raw materials in parts by weight: 30-50 parts of silica sol, 8-12 parts of persulfate, 10-20 parts of passivator and 8-12 parts of montmorillonite, wherein the passivator has oxidability;
(2) and (2) washing off stains on the surface of the stainless steel substrate, polishing the surface of the stainless steel substrate, soaking the stainless steel substrate in a modification solution for 30-50min, pulling and taking out, and curing at room temperature for 12-18h to obtain the surface modified stainless steel.
Through adopting above-mentioned technical scheme, this application compares with relevant technique, uses the passivating agent of modified liquid replacement to combine mechanical polishing and modified liquid processing two kinds of modes, with the degree of depth that deepens the passivating agent infiltration. In the step (2), when the passivating agent passivates the stainless steel substrate, the persulfate in the modification liquid is ionized in the silica sol and decomposed to generate sulfate radicals. The sulfate radical causes a part of metal particles on the surface of the stainless steel matrix to fall off, and simultaneously, the sulfate radical also causes silicon-oxygen bonds in the montmorillonite to break and destroys the silicon-oxygen tetrahedral structure of the montmorillonite. When the metal particles are separated from the stainless steel matrix, the iron in the metal particles is oxidized into ferric iron by the passivating agent. The montmorillonite adsorbs metal particles, broken silicon-oxygen bonds in the montmorillonite are combined with ferric iron to form a ferrite tetrahedron structure, and broken parts of the silicon-oxygen bonds are repaired. After the silica sol is solidified, the metal particles, the montmorillonite and the silica sol are combined to form a ceramic membrane, and the ceramic membrane covers the surface of the passive film, so that the possibility of peeling of the passive film is reduced, and the protection effect on a stainless steel matrix is improved.
Preferably, the formula of the modifying solution comprises the following raw materials in parts by weight: 35-45 parts of silica sol, 9-11 parts of persulfate, 13-17 parts of passivator and 9-11 parts of montmorillonite.
By adopting the technical scheme, the proportion of the modified liquid is optimized, the possibility of stripping of the passive film is reduced, and the protection effect on the stainless steel matrix is improved.
Preferably, the passivating agent is a nitric acid solution or a phosphomolybdic acid solution.
By adopting the technical scheme, the nitric acid and the phosphomolybdic acid can convert the metal simple substance on the surface of the stainless steel substrate into the passive film. The phosphomolybdic acid can be decomposed in the passivation process, is converted into insoluble molybdenum salt, is compounded with the passivation film, is favorable for reducing the possibility of peeling of the passivation film, and improves the protection effect on the stainless steel matrix.
Preferably, the formula of the modifying solution also comprises 4-8 parts by weight of silane coupling agent.
By adopting the technical scheme, in the process of curing the silica sol, the silane coupling agent migrates to the liquid level of the silica sol along with the evaporation of water in the silica sol. And after the silica sol is cured, the silane coupling agent is grafted on the surface of the ceramic membrane and forms a hydrophobic membrane. The silane coupling agent enhances the hydrophobicity of the ceramic membrane, reduces the damage of water-soluble corrosive substances in the external environment to the ceramic membrane, is beneficial to reducing the possibility of stripping of a passive membrane, and improves the protection effect on a stainless steel matrix.
Preferably, the silane coupling agent is vinyltriethoxysilane or tetraethoxysilane.
By adopting the technical scheme, the vinyltriethoxysilane and the tetraethoxysilane can generate a plurality of silanol groups during hydrolysis. After the silanol groups are dehydrated, the vinyltriethoxysilane and the tetraethoxysilane can form intermolecular crosslinking through the dehydration of the silanol groups, so that the density and the thickness of the hydrophobic film are improved, the possibility of peeling of a passive film is reduced, and the protection effect on a stainless steel matrix is improved. Compared with tetraethoxysilane, the carbon-carbon double bond in the vinyltriethoxysilane can be oxidized by the passivating agent to generate hydroxyl, so that the reaction sites of silanol groups are increased, and the crosslinking among silane coupling agents is promoted.
Preferably, the formula of the modifying solution also comprises 4-8 parts by weight of hydrogen peroxide.
By adopting the technical scheme, the hydrogen peroxide can activate the sodium persulfate, the decomposition of the sodium persulfate is accelerated, and meanwhile, the hydrogen peroxide can also be cracked to generate hydroxyl radicals, so that the content of the radicals in the modified liquid is improved, the falling speed of metal particles on the surface of the stainless steel substrate is accelerated, the thickness of a passivation film is increased, the possibility of falling of the passivation film is reduced, and the protection effect on the stainless steel substrate is improved.
Preferably, the water content of the silica sol is 58-66%.
By adopting the technical scheme, when the water content of the silica sol is too high, the thickness of the ceramic membrane is small, and the protection effect on the stainless steel matrix is insufficient. When the water content of the silica sol is too low, the silica sol is cured too fast, so that residual water exists in the passivation film easily, and the combination of the ceramic film and the passivation film is easily influenced. When the water content of the silica sol is 58-66%, the possibility of stripping of a passive film is reduced, and the protection effect on a stainless steel substrate is improved.
Preferably, the montmorillonite has an average particle size of 80 μm to 160 μm.
By adopting the technical scheme, when the average particle size of the montmorillonite is too small, the montmorillonite is easy to agglomerate, and the molding of the ceramic membrane is influenced. When the average particle size of the montmorillonite is too large, the reactivity of the montmorillonite is poor, and the metal particles are not easily combined with the montmorillonite, so that the molding of the ceramic membrane is influenced. When the average grain diameter of the montmorillonite is 80-160 μm, the montmorillonite has better forming effect, is beneficial to reducing the possibility of stripping of a passive film and improving the protection effect on a stainless steel matrix.
Preferably, the stainless steel substrate is 304 stainless steel or 254SMO stainless steel.
By adopting the technical scheme, both 304 stainless steel and 254SMO stainless steel can be used as the stainless steel substrate. Because the corrosion resistance of the 254SMO stainless steel is better than that of the 304 stainless steel, and the ceramic film contains metal particles from a stainless steel substrate, when the 254SMO stainless steel is used as the stainless steel substrate, the ceramic film has better resistance effect on external corrosion, thereby being beneficial to reducing the possibility of stripping of a passive film and improving the protection effect on the stainless steel substrate.
In a second aspect, the present application provides a surface modified stainless steel, which adopts the following technical scheme:
the surface modified stainless steel is prepared by adopting the production process of the surface modified stainless steel.
By adopting the technical scheme, the surface modified stainless steel is obtained by treating the stainless steel substrate with the modifying liquid.
In summary, the present application has the following beneficial effects:
1. according to the method, firstly, a stainless steel substrate is polished, surface modification is carried out on the stainless steel substrate by using a modification liquid, metal particles on the surface of the stainless steel substrate fall off by persulfate in the modification liquid, and a passivation film is generated on the surface of the stainless steel substrate by using a passivator. The fallen metal particles are combined with montmorillonite under the action of persulfate, and are solidified together with silica sol, and finally a ceramic film is generated on the surface of the passive film, so that the possibility of peeling of the passive film is reduced, and the protection effect on a stainless steel substrate is improved.
2. Preferably, vinyltriethoxysilane or tetraethoxysilane are used for the hydrophobic treatment of the ceramic membrane. The vinyltriethoxysilane and the tetraethoxysilane can both generate intermolecular crosslinking, thereby being beneficial to improving the thickness and the density of the hydrophobic film. The carbon-carbon double bond of the vinyltriethoxysilane can be oxidized into hydroxyl by a passivating agent, so that the increase of the dehydration reaction site of silanol is facilitated, the increase of the thickness and the density of a hydrophobic film are facilitated, the protection effect on a stainless steel substrate is improved 3, and the surface modified stainless steel is obtained by treating the stainless steel substrate with the modifying liquid.
Detailed Description
The present application will be described in further detail with reference to examples.
Examples
The raw materials used in the examples of the present application are commercially available, wherein the silica sol is selected from HS-230 silica sol sold by Shandong Hao Shunhui chemical company, the sodium persulfate is selected from industrial-grade sodium persulfate produced by Shandong Zhuui chemical company, the nitric acid is purchased from Texas gold and chemical trade company, the montmorillonite is purchased from processing plant of mineral products of Capacity in Lingshu county, the phosphomolybdic acid (CAS number 1429-74-4) is purchased from Jianchu biomedical company, the ethyl orthosilicate is purchased from Jinnan Laihua chemical company, the vinyltriethoxysilane is purchased from Jinnan Chuan chemical company, the hydrogen peroxide is purchased from Jiangxi City chemical company, the 304 stainless steel and the 254SMO stainless steel are purchased from Wubei Babboda Steel company.
Examples 1 to 5
The following description will be given by taking example 1 as an example.
Example 1
The surface modified stainless steel of example 1 was prepared according to the following procedure:
(1) mixing the raw materials to prepare a modified solution, preheating the modified solution to 60 ℃, wherein the formula of the modified solution comprises the following raw materials: 30kg of silica sol, 8kg of persulfate, 10kg of passivating agent and 8kg of montmorillonite, wherein the water content of the silica sol is 54%, the persulfate is sodium persulfate, the passivating agent is a nitric acid solution, the mass fraction of nitric acid in the nitric acid solution is 35%, and the average particle size of the montmorillonite is 40 mu m;
(2) washing off stains on the surface of the stainless steel substrate, polishing the surface of the stainless steel substrate, soaking the stainless steel substrate in a modification solution for 40min, then pulling out the stainless steel substrate, and curing at room temperature for 12-18h to obtain surface modified stainless steel; wherein the stainless steel substrate is 304 stainless steel, and the stainless steel substrate is a cubic sample with the side length of 100 mm.
As shown in Table 1, examples 1 to 5 are different mainly in the raw material ratio of the modifying solution.
TABLE 1
Example 6
This example differs from example 3 in that a 15 mass percent phosphomolybdic acid solution was used instead of the nitric acid solution in the raw material of the modification solution.
Example 7
The difference between this example and example 6 is that the raw materials for preparing the modifying solution further include 4kg of silane coupling agent, and the silane coupling agent is tetraethoxysilane. As shown in Table 2, examples 7 to 11 differ mainly in the amount of ethyl orthosilicate used.
TABLE 2
Example 12
This example differs from example 9 in that the same weight of vinyltriethoxysilane was used in place of ethyl orthosilicate.
Example 13
This example is different from example 12 in that 4kg of hydrogen peroxide was further included in the raw materials for preparing the modifying solution. As shown in Table 3, examples 12 to 16 differ mainly in the amount of hydrogen peroxide used.
TABLE 3
| Sample(s) | Example 13 | Example 14 | Example 15 | Example 16 | Example 17 |
| Hydrogen peroxide/kg | 4 | 5 | 6 | 7 | 8 |
As shown in Table 4, examples 18 to 21 are different from example 15 mainly in the water content of the silica sol.
TABLE 4
As shown in Table 5, examples 22 to 25 differ from example 19 mainly in the average particle size of montmorillonite.
TABLE 5
Example 26
The present example is different from example 25 in that the material of the stainless steel substrate is 254SMO stainless steel.
Comparative example
Comparative example 1
A surface modified stainless steel is prepared by the following method:
(1) cleaning and decontaminating a stainless steel substrate;
(2) soaking the cleaned and decontaminated stainless steel substrate in a nitric acid solution with the mass fraction of 32% for 25min, and taking out;
(3) washing the stainless steel substrate by using deionized water, wherein the washing time is 15 min;
(4) and soaking the stainless steel substrate in water at the temperature of 80 ℃ for 8min, taking out and drying to obtain the surface modified stainless steel.
Comparative example 2
This comparative example differs from example 3 in that a persulfate is not included.
Comparative example 3
This comparative example differs from example 3 in that no montmorillonite is included.
Performance detection test method
A salt spray test is carried out by using a Q-FOG circulating corrosion salt spray box produced by American Q-LAB company, and a solution used in the salt spray test is a sodium chloride solution with the mass fraction of 5% and hydrochloric acid with the mass fraction of 5% which are mixed according to the ratio of 1: 1. During testing, the prepared surface modified stainless steel sample is placed in a salt spray box, the time from the beginning of testing to the stripping of the sample surface is tested, and the test results are shown in table 6. The detection method refers to GB/T10125-2012 salt fog test for artificial atmosphere corrosion test.
TABLE 6
It can be seen from the combination of examples 1 to 5 and comparative example 1 and table 6 that the time for the first peeling of the surface of the test piece in examples 1 to 5 is longer than that in comparative example 1, which shows that the surface modified stainless steel of the present application reduces the possibility of peeling of the passive film and contributes to the improvement of the protective effect on the stainless steel substrate. In examples 1 to 5, the time at which the surface of the sample of example 3 peeled off was the latest.
It can be seen from the combination of example 3 and comparative examples 2 to 3 and from Table 6 that the time for the initial occurrence of exfoliation on the surface of the test piece in example 3 is longer than that in comparative example 2 and comparative example 3, indicating that the passivation layer has a better effect of protecting the stainless steel substrate when persulfate is used in combination with montmorillonite.
Combining example 3 and example 6 with table 6, it can be seen that the time for the first occurrence of peeling of the sample surface measured in example 6 is longer than that in example 3, indicating that phosphomolybdic acid is more helpful to improve the protective effect of the passivation layer on the stainless steel substrate than nitric acid.
As can be seen by combining example 6 with examples 7 to 11 and by combining Table 6, the time for the first occurrence of flaking on the surface of the test piece measured in examples 7 to 11 was longer than that in example 3, indicating that the silane coupling agent contributes to the improvement of the protective effect on the stainless steel substrate. In examples 7 to 11, the passivation layer of example 9 was more effective in protecting the stainless steel substrate.
It can be seen from the combination of example 9 and example 12 and table 6 that the time for the first occurrence of flaking on the surface of the test piece measured in example 12 is longer than that of example 9, indicating that vinyltriethoxysilane contributes more to the improvement of the protective effect of the passivation layer on the stainless steel substrate than tetraethoxysilane.
It can be seen from the combination of example 12, examples 13 to 17 and table 6 that the time for the first peeling of the sample surface was longer in examples 13 to 17 than in example 12, indicating that hydrogen peroxide helps to reduce the peeling of the passivation film and improve the protection effect of the passivation film on the stainless steel substrate. In examples 13 to 17, the passivation layer of example 15 is more effective in protecting the stainless steel substrate.
It can be seen from the combination of example 15, examples 18 to 21 and table 6 that the passivation layer has better protection effect on the stainless steel substrate when the water content of the silica sol is 58% to 66%. Within the range of 58-66%, when the water content of the silica sol is 62%, the passivation layer has better protection effect on the stainless steel matrix.
When the average particle size of montmorillonite is 80 μm to 160 μm, the passivation layer has better protection effect on the stainless steel substrate, as can be seen by combining example 19, examples 22 to 25 and table 6. In the range of 80-160 μm, when the average grain size of montmorillonite is 120 μm, the passivation layer has better protection effect on the stainless steel matrix.
When the stainless steel substrate of 254SMO stainless steel is used in place of 304 stainless steel, the time delay for the initial peeling of the surface of the test piece is shown to be improved by the passivation layer when the stainless steel substrate is used in combination with example 23 and example 26.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. A production process of surface modified stainless steel is characterized by comprising the following steps:
(1) preparing a modification liquid, preheating the modification liquid to 40-80 ℃, wherein the formula of the modification liquid comprises the following raw materials in parts by weight: 30-50 parts of silica sol, 8-12 parts of persulfate, 10-20 parts of passivator and 8-12 parts of montmorillonite, wherein the passivator has oxidability;
(2) and (2) washing off stains on the surface of the stainless steel substrate, polishing the surface of the stainless steel substrate, soaking the stainless steel substrate in a modification solution for 30-50min, pulling and taking out, and curing at room temperature for 12-18h to obtain the surface modified stainless steel.
2. The production process of the surface modified stainless steel according to claim 1, wherein the formula of the modifying solution comprises the following raw materials in parts by weight: 35-45 parts of silica sol, 9-11 parts of persulfate, 13-17 parts of passivator and 9-11 parts of montmorillonite.
3. The process for producing a surface-modified stainless steel as claimed in claim 1, wherein the passivating agent is a nitric acid solution or a phosphomolybdic acid solution.
4. The process for producing surface-modified stainless steel according to claim 1, wherein the formulation of the modifying solution further comprises 4 to 8 parts by weight of a silane coupling agent.
5. The process for producing surface-modified stainless steel according to claim 4, wherein the silane coupling agent is prepared from vinyltriethoxysilane and tetraethoxysilane in a ratio of (2-4): 1 by weight ratio.
6. The process for producing a surface-modified stainless steel according to claim 1, wherein the formulation of the modifying solution further comprises 4 to 8 parts by weight of hydrogen peroxide.
7. The process for producing surface-modified stainless steel according to claim 1, wherein the silica sol has a water content of 58% to 66%.
8. The process for producing a surface-modified stainless steel according to claim 1, wherein the montmorillonite has an average particle size of 80 μm to 160 μm.
9. The process for producing a surface-modified stainless steel as claimed in claim 1, wherein the stainless steel substrate is 304 stainless steel or 254SMO stainless steel.
10. A surface-modified stainless steel produced by the production process of the surface-modified stainless steel according to any one of claims 1 to 9.
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