US20220349062A1 - Hydrophilic stainless steel and method for manufacturing same - Google Patents

Hydrophilic stainless steel and method for manufacturing same Download PDF

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US20220349062A1
US20220349062A1 US17/868,622 US202217868622A US2022349062A1 US 20220349062 A1 US20220349062 A1 US 20220349062A1 US 202217868622 A US202217868622 A US 202217868622A US 2022349062 A1 US2022349062 A1 US 2022349062A1
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Prior art keywords
stainless steel
present disclosure
temperature
hydrophilic
sized
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English (en)
Inventor
Dong Rip Kim
Jae Hyeon JEON
Jung Bin YANG
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Industry University Cooperation Foundation IUCF HYU
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Industry University Cooperation Foundation IUCF HYU
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Assigned to IUCF-HYU(INDUSTRY-UNIVERSITY COOPERATION FOUNDATION HANYANG UNIVERSITY) reassignment IUCF-HYU(INDUSTRY-UNIVERSITY COOPERATION FOUNDATION HANYANG UNIVERSITY) ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: JEON, JAE HYEON, KIM, DONG RIP, YANG, Jung Bin
Publication of US20220349062A1 publication Critical patent/US20220349062A1/en
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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0278—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips involving a particular surface treatment
    • 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
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26—Methods of annealing
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/68—Temporary coatings or embedding materials applied before or during heat treatment
    • C21D1/72—Temporary coatings or embedding materials applied before or during heat treatment during chemical change of surfaces
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • 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
    • C23C22/24—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 hexavalent chromium compounds
    • C23C22/30—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 hexavalent chromium compounds containing also trivalent chromium
    • 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
    • C23C22/78—Pretreatment of the material to be coated

Definitions

  • the present disclosure relates to hydrophilic stainless steel and a method of manufacturing the same.
  • Stainless steel is a rich resource and has strong corrosion resistance, thereby being used in various living and industrial fields such as tableware, medical appliances, power generation, aviation, construction materials, and storage tanks.
  • stainless steel is widely used as a material for heat exchangers in fields where polluted water, chemicals, groundwater, etc. are used because it is inexpensive among metal materials and has high corrosion resistance.
  • corrosion resistance can be secured by using stainless steel, but when used for a long time, scale is deposited on the surface of the heat exchanger.
  • the deposited scale has low thermal conductivity, which causes thermal insulation problems in the heat exchanger, thereby reducing the heat transfer efficiency of the heat exchanger.
  • a hydrophilic surface refers to a surface where a contact angle when a droplet contacts the surface is significantly lower than those of other surfaces, and water spreads.
  • the present disclosure has been made in view of the above problems, and it is one object of the present disclosure to provide hydrophilic stainless steel whose surface has unidirectionality by physically polishing the surface in one direction, thereby having hydrophilicity; and a method of manufacturing the same.
  • the above and other objects can be accomplished by the provision of a method of manufacturing hydrophilic stainless steel, the method including: polishing the surface of the stainless steel in one direction; and immersing the polished stainless steel in an acidic solution to form an oxide film.
  • the polished stainless steel may have a micro-sized surface structure.
  • the method may include, after the immersing of the polished stainless steel, raising the temperature of the stainless steel on which the oxide film has been formed, and then thermally treating the stainless steel; and cooling the thermally treated stainless steel.
  • the thermally treated stainless steel may have a nano-sized surface structure.
  • the thermally treating may be performed at 850° C. to 1150° C.
  • a temperature of from 550° C. to 850° C. may be achieved by raising at a temperature raising rate of 200° C./sec to 300° C./sec.
  • cooling from 850° C. to 550° C. may be performed at a cooling rate of 200° C./sec to 300° C./sec.
  • hydrophilic stainless steel manufactured according to the method of manufacturing hydrophilic stainless steel of the present disclosure.
  • the hydrophilic stainless steel may have a contact angle of 0° to 30°.
  • the surface of stainless steel can be imparted with hydrophilicity by physically polishing the stainless steel surface in one direction to form a micro-sized surface structure having unidirectionality thereon.
  • the surface of stainless steel can be imparted with hydrophilicity by physically polishing the stainless steel surface, and then thermally treating the surface at high temperature to form a micro-sized surface structure and nano-sized surface structure thereof.
  • manufacturing costs can be reduced, compared to an existing method of making the surface of stainless steel hydrophilic in a coating manner, by using a method of physically polishing stainless steel, and then thermally treating the stainless steel at high temperature.
  • the durability of stainless steel can be improved by physically polishing the surface of stainless steel, and then thermally treating the surface at high temperature.
  • the surface of stainless steel can be imparted with hydrophilic properties only through physical polishing and high-temperature heat treatment, which allows a large-area process.
  • FIG. 1 illustrates a flowchart of a method of manufacturing hydrophilic stainless steel according to an embodiment of the present disclosure.
  • FIG. 2 illustrates a scanning electron microscopy (SEM) image of the stainless steel surface of Example 1.
  • FIG. 3 illustrates an SEM image of the stainless steel surface of Example 2.
  • FIG. 4 is an image illustrating a measurement result of a contact angle with respect to the stainless steel of Example 1 using a contact angle measuring instrument.
  • FIG. 5 is an image illustrating a result of measuring a contact angle with respect to the stainless steel of Example 2 using a contact angle measuring instrument.
  • FIG. 6 illustrates a scanning electron microscopy (SEM) image of the stainless steel surface of Comparative Example 1.
  • FIG. 7 illustrates a result of measuring a contact angle with respect to the stainless steel of Comparative Example 1 using a contact angle measuring instrument.
  • FIG. 1 illustrates a flowchart of a method of manufacturing hydrophilic stainless steel according to an embodiment of the present disclosure.
  • the method of manufacturing hydrophilic stainless steel according to an embodiment of the present disclosure includes the step (S 110 ) of polishing the surface of the stainless steel in one direction and a step (S 120 ) of immersing the polished stainless steel in an acidic solution to form an oxide film.
  • the surface of the stainless steel may be physically polished in one direction using a grinding stone.
  • the grinding stone may be a grinding stone of 40 to 200 grit.
  • the surface of the stainless steel may be physically polished using a grinding stone of preferably 40 to 100 grit.
  • the physically polishing is a basic operation for making the surface of the stainless steel hydrophilic.
  • the physically polished stainless steel may have a micro-sized surface structure, specifically a micro-sized concave-convex structure having unidirectionality.
  • the surface of the stainless steel may be washed with water before or after S 110 to remove residues present on the stainless steel surface.
  • an oxide film may be formed the surface of the physically polished stainless steel by immersing the physically polished stainless steel in an acidic solution.
  • an oxide film is formed on the surface of the stainless steel because the surface is exposed to air, but the oxide film may be removed by physical polishing.
  • an oxide film may be formed again on the stainless steel surface whose oxide film has been removed by physical polishing.
  • the acidic solution may excessively supply oxygen to the physically polished stainless steel, thereby forming an oxide film including chromium (Cr) on the physically polished stainless steel surface.
  • the acidic solution may be, for example, a nitric acid (HNO 3 ) solution, but is not limited thereto.
  • an oxide film may be formed on the polished stainless steel surface by immersing the polished stainless steel in a 30% nitric acid solution at 50° C. for 100 minutes.
  • a step (S 130 ) of raising the temperature of the stainless steel on which the oxide film is formed, and then thermally treating the stainless steel; and a step (S 140 ) of cooling the thermally treated stainless steel may be included.
  • the temperature of the stainless steel on which the oxide film is formed by S 120 may be rapidly raised to a heat treatment process temperature under a general atmosphere or oxygen atmosphere, and then may be thermally treated during a heat treatment process time to further improve the hydrophilicity of the stainless steel surface.
  • the heat treatment process temperature means a target temperature to be reached by raising the temperature of the stainless steel having the oxide film formed thereon
  • time (hereinafter referred to as “heat treatment process time”) during which the heat treatment process is performed means a time during which the heat treatment process temperature is maintained after the stainless steel having the oxide film formed thereon reaches the heat treatment process temperature.
  • chromium (Cr) included in the stainless steel on which the oxide film is formed through the heat treatment may be formed into nano-sized crystals.
  • the stainless steel thermally treated through S 130 may have a nano-sized surface structure.
  • the thermally treated stainless steel surface may have nano-sized chromium oxide crystals.
  • the thermally treated stainless steel surface may have a nano-sized surface structure formed through the thermal treatment together with a micro-sized surface structure formed through the physical polishing.
  • the nano-sized surface structure formed on the thermally treated stainless steel surface may improve the hydrophilic properties of the stainless steel surface.
  • Cr 2 O 3 is a ceramic material with high surface energy, and even a simple Cr 2 O 3 layer with no structure has a low contact angle (CA).
  • CA contact angle
  • when a nanostructure is formed on the stainless steel surface hydrophilicity is improved as a hydrophilic area is widened. Therefore, when a nano-sized Cr 2 O 3 structure is formed on the surface, super-hydrophilic properties may be expressed and improved.
  • the present disclosure may improve the hydrophilic properties of the stainless steel surface rather by utilizing defects (i.e., a micro-sized surface structure and a nano-sized surface structure) formed on the stainless steel surface.
  • the present disclosure may improve the hydrophilic properties of the stainless steel surface by forming a nano-sized surface structure on the stainless steel surface through heat treatment at a lower temperature than in the existing technology.
  • the heat treatment process temperature may be 850° C. to 1150° C.
  • the heat treatment process temperature is less than 850° C., a nano-sized surface structure may not formed on the stainless steel surface on which the oxide film has been formed.
  • an austenite phase used in the present disclosure may be deformed, which may cause a problem in that physical and chemical properties of the material are changed.
  • the heat treatment process time may be 10 to 60 minutes. When the heat treatment process time is less than 10 minutes, a nano-sized surface structure may not formed on the stainless steel surface through the heat treatment.
  • the temperature raising process of S 130 may include a first temperature raising process; and a second temperature raising process whose temperature raising rate is faster than that of the first temperature raising process.
  • the temperature of the stainless steel on which the oxide film has been formed is raised at temperature raising rate of 100° C./min through the first temperature raising process, and then 550° C. may reach the heat treatment process temperature, i.e., 850° C., by raising temperature at a temperature raising rate of 200° C./sec or more through the second temperature raising process. That is, the temperature of the second temperature raising process should be rapidly raised at a rate of 200° C. or more per second.
  • the temperature of the stainless steel on which the oxide film has been formed may be rapidly raised at a temperature raising rate of 200° C./sec to 300° C./sec to prevent corrosion of the stainless steel during the temperature raising process.
  • carbide precipitation occurs at a metal grain boundary.
  • carbide since carbide is a highly corrosive material compared to stainless steel, corrosion easily occurs depending on a carbide precipitated at a grain boundary, and the metal grain boundary itself separates and falls off.
  • stainless steel having a hydrophilic surface may be manufactured by cooling the thermally treated stainless steel.
  • the thermally treated stainless steel may be cooled from 850° C. to 550° C. at a cooling rate of 200° C./sec to 300° C./sec. Since other phases may be formed and corroded on the surface of the stainless steel at 700° C. as in the second temperature raising step, cooling is rapidly performed from 850° C. to 550° C.
  • the hydrophilic stainless steel manufactured by the method of the present disclosure may have a surface contact angle of 0° to 30°.
  • the contact angle of the physically polished stainless steel may be 10° to 30°, and the contact angle of the stainless steel thermally treated after the physically polishing may be 0° to 10°.
  • the cooled stainless steel may be washed to remove residues remaining on the surface of the cooled stainless steel.
  • stainless steel having super-hydrophilic surface properties may be manufactured by thermally treating the stainless steel surface at a high temperature after physical polishing.
  • the present disclosure uses a method of thermally treating at a high temperature after physical polishing, so that the manufacturing cost may be reduced compared to a method for manufacturing a hydrophilic surface of stainless steel through a conventional coating method.
  • the stainless steel surface was polished in one direction using a 60# grinding stone to form a micro-sized surface structure.
  • the washed stainless steel was immersed in a 30% nitric acid solution at 70° C. for 60 minutes to re-form an oxide film removed from the stainless steel surface, thereby forming an oxide film.
  • the stainless steel surface was polished in one direction using a 60# grinding stone to form a micro-sized surface structure.
  • the washed stainless steel was immersed in a 30% nitric acid solution at 70° C. for 60 minutes to re-form an oxide film removed from the stainless steel surface, thereby forming an oxide film.
  • the temperature of the stainless steel was raised to 850° C. under a general atmosphere, and then thermally treated for 30 minutes.
  • the stainless steel was washed to remove residues remaining on the stainless steel surface.
  • the stainless steel surface was not polished in one direction, the temperature of the stainless steel was raised to 850° C. at 100° C/min, and heat treatment was not performed.
  • FIG. 2 illustrates a scanning electron microscopy (SEM) image of the stainless steel surface of Example 1.
  • Example 1 a micro-sized concave-convex structure formed in one direction is formed on the stainless steel surface of Example 1.
  • water on the stainless steel surface may be drained and spread along a direction in which the micro-surface structure is formed, so that the stainless steel surface have hydrophilicity.
  • FIG. 3 illustrates an SEM image of the stainless steel surface of Example 2. Referring to FIG. 3 , it can be seen that nano-sized chromium crystals are formed together with a micro-sized concave-convex structure having directionality on the stainless steel surface of Example 2.
  • nano-sized chromium crystals are formed through high-temperature heat treatment in addition to the micro-surface structure according to the present disclosure, so that hydrophilic properties are improved.
  • FIG. 4 is an image illustrating a measurement result of a contact angle with respect to the stainless steel of Example 1 using a contact angle measuring instrument.
  • Example 1 the contact angle of Example 1 is 16°. That is, it can be confirmed that the present disclosure has hydrophilicity by forming a micro-sized surface structure having unidirectionality on the stainless steel surface through physical polishing.
  • FIG. 5 is an image illustrating a result of measuring a contact angle with respect to the stainless steel of Example 2 using a contact angle measuring instrument.
  • Example 2 the contact angle of Example 2 is almost 0°. Through this, it can be confirmed that the nano-sized surface structure formed through high-temperature heat treatment is formed, together with the micro-sized surface structure formed by physical polishing, on the stainless steel surface according to the present disclosure, so that hydrophilic properties are further improved.
  • FIG. 6 illustrates a scanning electron microscopy (SEM) image of the stainless steel surface of Comparative Example 1.
  • FIG. 7 illustrates a result of measuring a contact angle with respect to the stainless steel of Comparative Example 1 using a contact angle measuring instrument.
  • Comparative Example 1 is very large as 34°.
  • the present disclosure forms a nano-sized surface structure formed through high-temperature heat treatment, together with the micro-sized surface structure formed by physical polishing, on the stainless steel surface, so that hydrophilic properties are further improved.

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  • Chemical Treatment Of Metals (AREA)
US17/868,622 2020-01-20 2022-07-19 Hydrophilic stainless steel and method for manufacturing same Pending US20220349062A1 (en)

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Application Number Priority Date Filing Date Title
KR1020200007363A KR102419291B1 (ko) 2020-01-20 2020-01-20 친수성 스테인리스강 및 이의 제조방법
KR10-2020-0007363 2020-01-20
PCT/KR2020/006522 WO2021149876A1 (ko) 2020-01-20 2020-05-19 친수성 스테인리스강 및 이의 제조방법

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JP3902254B2 (ja) * 1995-09-05 2007-04-04 大陽日酸株式会社 ステンレス鋼材の乾式耐食熱処理方法およびステンレス鋼材
JP4454776B2 (ja) 2000-03-29 2010-04-21 日新製鋼株式会社 親水性フェライト系ステンレス鋼材
JP4454777B2 (ja) * 2000-03-29 2010-04-21 日新製鋼株式会社 親水性オーステナイト系ステンレス鋼材
JP2005240062A (ja) * 2004-02-24 2005-09-08 Nisshin Steel Co Ltd 親水性ステンレス鋼板及びその製造方法
KR101085176B1 (ko) * 2009-02-27 2011-11-18 포항공과대학교 산학협력단 극친수성 표면 가공 방법
JP6694693B2 (ja) * 2015-10-22 2020-05-20 株式会社Ihi ステンレス鋼部品の処理方法
WO2018075779A1 (en) 2016-10-19 2018-04-26 Ak Steel Properties, Inc. Surface modification of stainless steels

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