WO2012176551A1 - Produit à base d'acier et son procédé de fabrication - Google Patents

Produit à base d'acier et son procédé de fabrication Download PDF

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Publication number
WO2012176551A1
WO2012176551A1 PCT/JP2012/061166 JP2012061166W WO2012176551A1 WO 2012176551 A1 WO2012176551 A1 WO 2012176551A1 JP 2012061166 W JP2012061166 W JP 2012061166W WO 2012176551 A1 WO2012176551 A1 WO 2012176551A1
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Prior art keywords
compound layer
layer
treatment
steel product
steel
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English (en)
Japanese (ja)
Inventor
晃司 西川
尚男 冨士川
渡辺　崇則
岩村　英明
守弘 藤田
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Air Water Inc
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Air Water Inc
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Priority to CN201280031158.4A priority Critical patent/CN103620081B/zh
Priority to US14/123,540 priority patent/US20140102592A1/en
Publication of WO2012176551A1 publication Critical patent/WO2012176551A1/fr
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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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/24—Nitriding
    • C23C8/26—Nitriding of ferrous surfaces
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02—Pretreatment of the material to be coated
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/80—After-treatment
    • 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/40—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for rings; for bearing races

Definitions

  • the present invention improves the corrosion resistance and adhesion by performing a surface treatment with nitriding treatment on a steel material, and improves its durability by applying to a back metal such as a brake pad, brake shoe, clutch plate, etc.
  • the present invention relates to a steel product that can be manufactured and a manufacturing method thereof.
  • Friction members such as brake pads, brake shoes, and clutch plates used in automobiles and the like are generally frequently used in which a friction material is bonded to a steel material as a back metal.
  • the adhesive strength between the friction material and the back metal is related to the performance and quality of the brake and is an extremely important factor from the safety aspect.
  • a method of roughening the surface by a technique such as shot peening has been adopted for the back metal for a long time.
  • a treatment for forming a chemical conversion coating such as zinc phosphate and a primer layer is performed in consideration of corrosion resistance (for example, Patent Document 1 below).
  • the above chemical conversion film has a problem with respect to heat resistance, and has a problem that corrosion resistance and adhesion are lowered by heat.
  • the characteristic that the corrosion resistance and adhesion deteriorate when large frictional heat is generated is extremely undesirable.
  • nitriding has been applied in a wide range of fields in order to improve the wear resistance and durability of mechanical parts and structural members made of various steel materials.
  • steel materials other than stainless steel can improve corrosion resistance by forming a nitride compound layer on the surface thereof.
  • One of the uses is, for example, application to a back pad of a brake pad.
  • a backing metal obtained by nitriding a steel material excluding stainless steel is more advantageous in terms of corrosion resistance than those obtained by forming the above-described chemical conversion film. Therefore, it has been studied to apply gas soft nitriding to the back metal of the brake pad (for example, Patent Document 2 below).
  • gas soft nitriding to the back metal of the brake pad (for example, Patent Document 2 below).
  • the back metal is formed by nitriding, it is not sufficient to simply improve the corrosion resistance by forming a nitride compound layer on the surface.
  • salt bath nitriding treatment is easy to form a relatively uneven surface, it is applied to a back metal (for example, Patent Document 3).
  • Patent Document 2 there is a description that irregularities such as humps and mesh-like protrusions are formed in order to improve adhesion to the friction material.
  • irregularities such as humps and mesh-like protrusions are formed in order to improve adhesion to the friction material.
  • the Fe—C—N-based compound formed by gas soft nitriding is not sufficient for its use as a brake pad back metal in terms of its own corrosion resistance.
  • defects that reach from the surface to the diffusion layer are normally formed, which adversely affects corrosion resistance.
  • Patent Document 3 a salt bath nitriding treatment is used as a method of forming an Fe—C—N compound.
  • the salt bath nitriding treatment unlike the nitriding treatment using a normal gas, it is easy to form irregularities that ensure adhesion performance on the surface.
  • a reaction in which a base material component such as Fe dissolves into the salt bath also proceeds simultaneously. For this reason, penetrating defects that reach the diffusion layer are much easier to form than nitriding using gas.
  • a nitride compound layer formed by diffusing a halogen element to a depth of 1 ⁇ m or more from the surface and then performing nitriding in a gas atmosphere not containing a carbon source is, as shown in FIG.
  • the nitride compound layer containing the said 2 layer has high adhesiveness and corrosion resistance, and came to completion of this invention.
  • an oxide layer mainly composed of iron oxide is formed on the nitride compound layer, unnecessary nitriding, oxide, oxynitride, etc. on the surface are added by adding a peening treatment with fine grains. It was also found that when removed, the adhesion and corrosion resistance were further improved.
  • the steel product of the present invention is a steel product in which a nitride compound layer and a nitrogen diffusion layer are formed on the surface layer of a base material that is steel,
  • the nitride compound layer includes a first compound layer formed on the nitrogen diffusion layer side, and a second compound layer formed on the surface side of the first compound layer,
  • the first compound layer has an ⁇ structure mainly composed of Fe 3 N
  • the second compound layer has a higher nitrogen concentration than the first compound layer and has an uneven surface.
  • the steel product manufacturing method of the present invention includes a nitride compound layer on the surface of the base material by performing a gas nitriding treatment for diffusing nitrogen after performing a fluorination treatment for diffusing fluorine on the surface of the steel material.
  • the fluorination treatment includes a fluorination process in which fluorine reacts with the steel material while introducing the fluorine source gas into the treatment furnace, and fluorine that has been heated and held in a state where the supply of the fluorine source gas is stopped to penetrate the steel material surface.
  • a diffusion step of diffusing to a depth of at least 1 ⁇ m, The gist of the gas nitriding treatment is to reduce and vaporize the diffused fluorine component in a gas atmosphere not containing a carbon source, and to diffuse and infiltrate nitrogen to form a nitride compound layer and a nitrogen diffusion layer. .
  • the nitride compound layer includes a first compound layer formed on the nitrogen diffusion layer side and a second compound layer formed on the surface side of the first compound layer.
  • the first compound layer has an ⁇ structure mainly composed of Fe 3 N
  • the second compound layer has a higher nitrogen concentration than the first compound layer and has irregularities formed on the surface.
  • the second compound layer has surface irregularities having many intermittent grooves with a predetermined depth. Further, it is formed by growing an Fe—N-based nitride compound outward. Furthermore, it is made of nitride having a higher nitrogen concentration than the first compound layer.
  • the second compound layer that forms the Fe—N-based surface irregularities, and particularly the first compound layer formed on the nitrogen diffusion layer side has better corrosion resistance than the Fe—C—N-based compound. Furthermore, due to the effects of the fluorination treatment and the gas nitriding treatment, a denser nitride compound layer is formed, and there are very few defects that penetrate from the surface to the nitrogen diffusion layer. Therefore, it becomes a nitride compound layer with extremely excellent corrosion resistance.
  • the second compound layer has a surface nitrogen concentration of 12% by mass or more. Increasing the amount of N intrusion into the surface layer so that the surface nitrogen concentration of the second compound layer is 12% by mass or more, and forming a nitride compound with a high N concentration can promote the outward growth of the nitride compound. It becomes possible.
  • the thickness of the first compound layer is 5 ⁇ m or more
  • the entire nitride compound layer becomes denser and the presence of defects penetrating to the nitrogen diffusion layer is extremely reduced, so that the corrosion resistance is remarkably improved.
  • the actual surface area ratio per unit area of the surface exceeds 1.8
  • the true surface area with respect to the apparent surface area is sufficiently large, and the degree of unevenness of the surface unevenness is accordingly high, so that reliable and stable adhesion performance can be ensured.
  • an oxide layer mainly composed of iron oxide having a thickness of 3 ⁇ m or less is formed as the outermost layer on the second compound layer, Furthermore, corrosion resistance can be improved.
  • the nitride compound layer has a high concentration of invading N.
  • the nitride compound layer closer to the nitrogen diffusion layer becomes a denser compound layer.
  • the nitride compound layer according to the present invention has a) a higher corrosion resistance of the nitride compound layer itself than other nitriding methods, b) a relatively dense compound layer can be formed on the nitrogen diffusion layer, and c) a source of rust.
  • the volume of through defects in the nitride compound layer can be increased simply by forming an oxide layer with a thickness of 3 ⁇ m or less that does not impair adhesion.
  • the portion is sealed to form a surface layer with extremely high corrosion resistance. Therefore, for example, when applied to the back metal of a brake shoe, peeling of the friction material due to the occurrence of corrosion is effectively prevented.
  • the penetrating defects present in the second compound layer are sealed with an oxide mainly composed of iron oxide, Furthermore, corrosion resistance can be improved. That is, the nitride compound layer has a high concentration of invading N.
  • the nitride compound layer closer to the nitrogen diffusion layer becomes a denser compound layer.
  • the nitride compound layer according to the present invention has a) a higher corrosion resistance of the nitride compound layer itself than other nitriding methods, b) a relatively dense compound layer can be formed on the nitrogen diffusion layer, and c) a source of rust.
  • the volume of through defects in the nitride compound layer can be increased simply by forming an oxide layer with a thickness of 3 ⁇ m or less that does not impair adhesion.
  • the portion is sealed to form a surface layer with extremely high corrosion resistance. Therefore, for example, when applied to the back metal of a brake shoe, peeling of the friction material due to the occurrence of corrosion is effectively prevented.
  • a halogenation treatment is performed in which a halogen element is diffused and permeated to a depth of 1 ⁇ m or more prior to the gas nitriding treatment.
  • the halogen element is reacted with active hydrogen generated by the decomposition of NH 3 gas to cause a reduction reaction and vaporize.
  • nitriding is performed in an atmosphere mainly composed of NH 3 gas containing no carbon source.
  • a nitrided compound layer formed by a general nitriding treatment has a property that it is very easy to take in carbon present in the surroundings and carbon in the substrate.
  • the nitride compound layer formed in the present invention has an extremely low carbon content.
  • the Fe-N-based nitride compound layer is formed instead of the Fe-CN-based.
  • the present invention in which the Fe—N-based nitride compound layer is formed is much more excellent in corrosion resistance than the formation of the Fe—C—N-based nitride compound layer. Since it is easy to form irregularities on the surface, salt bath nitriding is often used as a surface treatment method for the back metal at present. However, in the salt bath nitriding treatment, since a nitriding treatment is performed using a cyan compound, carbon is inevitably diffused together with nitrogen. For this reason, it has been found that the surface nitride compound layer inevitably contains a high concentration of carbon, which adversely affects the corrosion resistance.
  • nitriding is performed using a nitriding gas that does not contain a carbon source.
  • a nitriding gas that does not contain a carbon source.
  • the carbon component contained in the base material is inevitably contained in the nitride compound layer.
  • the surface is activated by the diffusion of fluorine in the fluorination treatment and the subsequent reduction of the fluorine component to facilitate the invasion of N. On the activated surface, the reaction between active hydrogen generated by the decomposition of ammonia gas and carbon existing in the nitride compound layer is promoted.
  • the fluorination treatment is repeated when the fluorination step and the diffusion step are repeated twice or more. Fluorine can be diffused and penetrated deeper into the surface layer of steel, and the effect of subsequent reduction and vaporization of the fluorine component can be deeply formed to form a thick nitride compound layer with low carbon concentration and high corrosion resistance. Can do.
  • after performing the gas nitriding treatment In the case of sealing penetration defects existing in the nitride compound layer by forming an oxide layer mainly composed of iron oxide having a thickness of 3 ⁇ m or less on the surface, Furthermore, corrosion resistance can be improved.
  • the nitride compound layer has a high concentration of invading N.
  • the nitride compound layer closer to the nitrogen diffusion layer becomes a denser compound layer.
  • the nitride compound layer according to the present invention has a) a higher corrosion resistance of the nitride compound layer itself than other nitriding methods, b) a relatively dense compound layer can be formed on the nitrogen diffusion layer, and c) a source of rust.
  • the volume of through defects in the nitride compound layer can be increased simply by forming an oxide layer with a thickness of 3 ⁇ m or less that does not impair adhesion.
  • the portion is sealed to form a surface layer with extremely high corrosion resistance. Therefore, for example, when applied to the back metal of a brake shoe, peeling of the friction material due to the occurrence of corrosion is effectively prevented.
  • the method for producing a steel product of the present invention after performing the gas nitriding treatment, By carrying out fine particle peening treatment with an average particle size of 100 ⁇ m or less and removing unnecessary nitrides, oxides, oxynitrides, etc.
  • the adhesive strength of the surface irregularities can be further improved. That is, when the nitride particles formed by nitriding are not sufficiently bonded to the nitride compound layer, or when the surface irregularities are covered with nitride, oxide, or oxynitride, the adhesion performance of that portion is reduced. It can be damaged. Therefore, by performing the peening process under weak conditions, the surface irregularities can be exposed and the adhesive force can be further stabilized.
  • the peening treatment is for adjusting the surface state in order to further improve the adhesion, and does not remove the portion where the through defects are sealed by the oxidation treatment.
  • the steel product of the present invention and the manufacturing method thereof have high adhesion when a friction material is adhered, for example, by using a surface treatment method mainly including a relatively inexpensive gas nitriding treatment.
  • a surface treatment method mainly including a relatively inexpensive gas nitriding treatment it is possible to form a surface layer that is extremely difficult to generate rust. For this reason, for example, when applied to a brake shoe back metal, the friction material does not peel off over a long period of time, resulting in a product with excellent durability.
  • FIG. 1 It is a schematic diagram which shows the layer structure of the nitride compound layer and nitrogen diffusion layer of the steel product of this invention. It is a figure which shows the result of having measured N density
  • FIG. It is a figure which shows the SEM observation result of the surface of an Example and Comparative Examples 1 and 2, and a cross section. It is a measurement result which measured a surface shape about an example and comparative example 2. It is a figure which shows the SEM observation result of the surface of C2-2 which is an Example, and C2-3.
  • the steel product of this embodiment is a steel product in which a nitride compound layer and a nitrogen diffusion layer are formed on the surface layer of a base material that is steel.
  • the nitride compound layer includes a first compound layer formed on the nitrogen diffusion layer side and a second compound layer formed on the surface side of the first compound layer.
  • the first compound layer has an ⁇ structure mainly composed of Fe 3 N, and the second compound layer has a higher nitrogen concentration than the first compound layer and has irregularities formed on the surface.
  • the steel product manufacturing method performs a nitriding treatment for diffusing fluorine on the surface of the steel material, and then performing a gas nitriding treatment for diffusing nitrogen, thereby forming a nitride compound layer and nitrogen on the surface layer of the base material.
  • This is a method for producing a steel product in which a diffusion layer is formed.
  • the fluorination treatment includes a fluorination process in which fluorine reacts with the steel material while introducing the fluorine source gas into the treatment furnace, and fluorine that has been heated and held in a state where the supply of the fluorine source gas is stopped to penetrate the steel material surface.
  • a diffusion step of diffusing to a depth of at least 1 ⁇ m In the gas nitriding treatment, the diffused fluorine component is reduced and vaporized in a gas atmosphere containing no carbon source, and nitrogen is diffused and penetrated to form a nitride compound layer and a nitrogen diffusion layer.
  • a fluorination treatment that performs a fluorination step and a fluorine diffusion step is applied to the steel material surface to form a deep fluorinated layer without excessively increasing the surface fluorine concentration.
  • a nitride compound layer is formed by gas nitriding treatment mainly containing NH 3 not containing a carbon source.
  • an Fe—N-based first compound layer with few penetration defects is formed on the nitrogen diffusion layer side, and a second compound layer having surface irregularities formed on the surface side is formed.
  • the steel material which has the surface layer excellent in both adhesiveness and corrosion resistance.
  • it can be suitably used as a back pad for brake pads, brake shoes, clutch plates and the like having excellent durability.
  • This embodiment is carbon steel, low alloy steel, high alloy steel, rolled steel for structure, high tensile steel, steel for machine structure, carbon tool steel, alloy tool steel, high speed tool steel, bearing steel, spring steel, skin
  • the present invention can be applied to various steel materials that can form a nitride compound layer, such as burned steel, nitrided steel, stainless steel, heat-resistant steel, and cast forged steel.
  • a nitride compound layer such as burned steel, nitrided steel, stainless steel, heat-resistant steel, and cast forged steel.
  • the back metal for brake pads, brake shoes, clutch plates, etc. structural rolled steel, high-tensile steel, and the like can be suitably used.
  • halogenation treatment is performed on these steel materials. By this halogenation treatment, the oxide film on the surface of the workpiece is removed and a halogenated layer is formed.
  • a dehalogenation element treatment for reducing the halogen component in the halogenated layer and a nitriding treatment nitrogen is diffused and penetrated from the surface of the object to be treated, thereby forming a nitride compound layer and a nitrogen diffusion layer.
  • the halogenation treatment include a fluorination treatment, a chlorination treatment, a bromination treatment, an iodination treatment, and the like, but a fluorination treatment that is easy to handle and easily used industrially can be suitably performed.
  • the fluorination treatment is performed by heating and holding at a temperature of 200 to 600 ° C.
  • a fluoride layer is formed.
  • a fluoride layer having a thickness slightly exceeding the thickness of the oxide film formed on the steel surface may be formed. That is, it is sufficient to replace the oxide film with fluoride, specifically, a fluoride layer less than 1 ⁇ m, and in many cases, a thinner fluoride layer may be formed.
  • a fluoride and fluorine permeation layer having a thickness of 1 ⁇ m or more, more preferably about 1.5 to 4.5 ⁇ m is formed.
  • a nitriding treatment layer composed of a nitride compound layer and a nitrogen diffusion layer is formed.
  • the nitride compound layer includes the first compound layer and the second compound layer described above.
  • the surface roughness of the second compound layer is preferably such that recesses having a depth of 0.5 ⁇ m or more have a high density, and more preferably 1 ⁇ m or more and 5 ⁇ m or less. This is because if the depth of the surface irregularities is too shallow, desired adhesive performance cannot be obtained. On the other hand, if the depth of the surface irregularities is too deep, the bonding force with the first compound layer becomes weak, and there is a risk of causing peeling and the like, resulting in a decrease in adhesion performance.
  • the concentration of the fluorine source gas used for the fluorination treatment is adjusted to an appropriate concentration according to the material of the object to be treated.
  • the fluorine concentration on the surface of the object to be processed becomes too high, there are too many portions to be vaporized during the nitriding treatment, and the surface portion of the nitride compound layer is pulverized and the adhesiveness tends to deteriorate.
  • the fluorine concentration on the surface of the object to be processed before the nitriding treatment step is preferably 60% by mass or less, and more preferably about 50% by mass or less. Therefore, in the surface treatment method of the present invention, a fluorine diffusion step is provided in order to deeply penetrate the fluorine without extremely increasing the fluorine concentration on the surface of the object to be treated. That is, during the fluorination treatment, a fluorine source gas is allowed to flow in the treatment furnace for a certain period of time to react the object to be treated with fluorine, and the supply of the fluorine source gas is stopped and the fluorine is maintained by heating for a certain period of time. A diffusion step for promoting diffusion and adjusting the fluorine concentration on the surface portion is provided.
  • the fluorination treatment preferably repeats the fluorination step and the diffusion step twice or more. This is because the diffusion rate of fluorine in the steel material is very slow. Therefore, if the fluorine concentration on the surface is excessively increased, it takes a long time to decrease the concentration by diffusion, resulting in poor efficiency.
  • the fluorine source gas is supplied in several divided portions at a temperature of 200 ° C. or higher, preferably 300 ° C. or higher, more preferably 400 ° C. or higher.
  • the fluorination step and the diffusion step it is possible to form a relatively deep fluorine permeation layer without excessively increasing the fluorine concentration on the surface of the object to be processed.
  • the temperature of the fluorination treatment including the fluorination step and the diffusion step is less than 200 ° C.
  • the diffusion rate of fluorine is slow, and it takes a long time to form a fluoride layer of 1 ⁇ m or more, resulting in poor productivity.
  • the temperature of the fluorination treatment exceeds 600 ° C., the diffusion rate of fluorine increases, while the reaction rate between fluorine and steel material increases excessively, making it difficult to control the fluorine concentration on the material surface.
  • the temperature of the fluorination treatment is preferably 200 ° C. or more and 600 ° C. or less.
  • the depth of diffusion of fluorine is less than 1 ⁇ m, the height of the unevenness formed on the surface becomes insufficient, and the adhesive force with the friction material or the like cannot be sufficiently improved.
  • the penetration depth of the fluorine exceeds 5 ⁇ m, the amount of outgassing on the surface becomes too large and the surface becomes porous, and the irregular shape is easily broken, which tends to cause powdering. Therefore, it is preferable that the depth of diffusion of fluorine in the fluorination treatment is 1 ⁇ m or more and 5 ⁇ m or less.
  • the treatment time is preferably 1 minute or more and 120 minutes or less.
  • the fluorination treatment can be performed in a furnace that performs nitriding treatment, or the fluorination treatment and the nitriding treatment can be performed in separate furnaces.
  • the fluorination treatment chamber and the nitridation treatment chamber can be provided separately in the same furnace.
  • the fluorination treatment and the nitriding treatment are preferably performed separately in different furnaces or rooms. By doing so, it is easy to control the fluorine concentration on the surface of the material and the penetration depth of fluorine.
  • nitriding treatment is performed. The nitriding treatment is performed by heating and holding the fluorinated steel product in an atmosphere gas containing a nitriding source gas such as NH 3 .
  • a nitride compound layer including a first compound layer formed on the nitrogen diffusion layer side and a second compound layer formed on the surface side of the first compound layer is formed.
  • the first compound layer has an ⁇ structure mainly composed of Fe 3 N
  • the second compound layer has a higher nitrogen concentration than the first compound layer and has irregularities formed on the surface.
  • the second compound layer preferably has a high N concentration with a surface nitrogen concentration of 12% by mass or more.
  • the second compound layer has surface irregularities and exhibits adhesive performance.
  • Such a second compound layer with surface irregularities is formed by forming the irregularities by defluorinating the fluorinated layer, and growing nitrides outwardly on the convex portions formed thereby.
  • the second compound layer formed at this time is considered to be a compound layer containing a considerable amount of a nitride compound having a smaller mass than the first compound layer, and as a result, a compound layer having a complicated uneven shape with higher adhesion. It is. It is preferable that the surface unevenness of the second compound layer has a high density of recesses having a depth of 0.5 ⁇ m or more. This is because if the depth of surface irregularities is less than 0.5 ⁇ m, sufficient adhesion performance may not be obtained.
  • the nitriding conditions are preferably set so that the surface nitrogen concentration is 12% by mass or more.
  • the surface nitrogen concentration is preferably 20% by mass or less.
  • the thickness of the second compound layer is preferably 0.7 ⁇ m or more, and more preferably 1 ⁇ m or more. If the thickness of the second compound layer is less than 0.7 ⁇ m, it is difficult to significantly improve the adhesive strength.
  • the thickness of the second compound layer exceeds 5 ⁇ m, the layer having a high nitrogen concentration becomes thick and becomes brittle, so that the adhesive strength may be lowered. Therefore, the thickness of the second compound layer is desirably 0.7 ⁇ m or more and 5 ⁇ m or less.
  • the actual surface area ratio per unit area of the surface is preferably set to a value exceeding 1.8. This is because forming the surface irregularities increases the actual surface area per unit area, thereby increasing the adhesion area, thereby improving the adhesion.
  • the actual surface area ratio per unit area is a value obtained by dividing the actual surface area value by the apparent surface area value.
  • the actual surface area and the actual surface area ratio can be measured by, for example, an apparatus that analyzes a three-dimensional surface shape. Further, the actual surface area ratio may be calculated from the ratio to the linear distance by measuring the length of the uneven portion in a certain cross section. Alternatively, a 3D image may be captured and obtained from the captured image. If the actual surface area ratio is 1.8 or less, a significant improvement in surface adhesion cannot be expected. On the other hand, when the actual surface area ratio exceeds 5, there is a risk that the strength of bonding the second compound layer having the above-described surface irregularities with the first compound layer as the underlying layer is lowered, and the adhesiveness is lowered. For this reason, the actual surface area ratio is preferably more than 1.8 and not more than 5.
  • the value is more preferably 2 or more and 4.5 or less.
  • the nitriding temperature is less than 450 ° C.
  • the reaction between the permeated fluorine and the hydrogen entering from the steel material surface becomes slow, and the formation rate of the second compound layer is also slowed, resulting in poor productivity.
  • the temperature exceeds 650 ° C.
  • the growth of the second compound layer is too fast, and particularly the surface layer portion of the second compound layer becomes extremely porous, and the strength of the formed nitride compound is lowered and can be practically used. There may be no case. Therefore, the nitriding temperature is set to 450 ° C.
  • nitriding temperature is 500 ° C. or higher and 600 ° C. or lower.
  • surface irregularities which are surface shapes peculiar to the present invention appear. That is, the infiltrated fluorine and hydrogen are reacted to vaporize, and the second compound layer is grown inward and outward.
  • the time is 10 minutes or more and 3 hours or less.
  • the thickness of the first compound layer is preferably about 5 ⁇ m. This is because a relatively dense compound layer is formed on the base material side of the first compound layer formed on the surface.
  • the nitride compound layer including the first compound layer and the second compound layer preferably has a thickness of 7 ⁇ m or more, and more preferably 8 ⁇ m or more in consideration of corrosion resistance.
  • the thickness of the nitride compound layer is preferably 7 ⁇ m or more and 25 ⁇ m or less.
  • the upper limit of the thickness is more preferably 20 ⁇ m or less.
  • the nitriding gas used in the nitriding process does not include a carburizing gas.
  • a nitride compound layer having higher corrosion resistance is formed.
  • a method of supplying only NH 3 gas, NH 3 gas and nitrogen gas, NH 3 gas and hydrogen gas, NH 3 gas, nitrogen gas and hydrogen gas can be exemplified.
  • a surface oxidation step can be performed as necessary.
  • an oxide layer mainly composed of iron oxide having a thickness of 3 ⁇ m or less is formed as the outermost layer.
  • the purpose of this oxidation treatment step is to seal the penetrating defect portion leading to the nitrogen diffusion layer existing under the nitride compound layer with the oxide.
  • the method is not particularly limited, and for example, a method of oxidizing in an atmosphere containing an oxidation source gas such as oxygen or water vapor while being heated and held following the nitriding treatment can be employed. Moreover, the method of oxidizing during a cooling process may be sufficient, and the method of oxidizing by carrying out heating maintenance again once after cooling can also be performed.
  • the steel material nitrided by the method of the present invention has a complex shape with irregularities on the order of microns on the outermost surface, but the first compound layer formed on the nitrogen diffusion layer side has relatively few penetration defects. Therefore, the sealing can be easily performed without performing a strong oxidation treatment. Therefore, the corrosion resistance can be sufficiently improved even by a short-time oxidation treatment using a cooling process.
  • the oxide layer mainly composed of Fe 3 O 4 of 3 ⁇ m or less is preferably exposed to an atmosphere containing 3% by volume or less, more preferably 1% by volume or less of the oxidation source gas at a temperature of 450 ° C. or higher. It is preferable to form.
  • the thickness of the oxide layer to be formed is preferably 3 ⁇ m or less, and more preferably 1.5 ⁇ m or less. This method is excellent in productivity because a desired oxide layer can be formed within the time for cooling the object to be processed. Moreover, when forming the said oxide layer, in order to exhibit the effect, it is desirable that the thickness shall be 0.2 micrometer or more. In this embodiment, after the gas nitriding treatment, a fine particle peening treatment can be performed as necessary.
  • the fine particle peening treatment is a peening treatment with fine particles having an average particle diameter of 100 ⁇ m or less, and may be performed following the gas nitriding treatment or may be performed following the oxidizing treatment after the gas nitriding treatment.
  • This removes unnecessary nitrides, oxides, oxynitrides and the like covering the outermost surface, and exposes surface irregularities having a depth of 0.5 ⁇ m or more. That is, since the purpose of the oxidation treatment is to seal through defects as described above, after the oxidation treatment, a fine uneven shape is further given to the surface, and unnecessary particles, nitrides, oxidations are added.
  • an object, oxynitride or the like there may be a portion where an object, oxynitride or the like is formed so as to cover the uneven surface.
  • a peening treatment at a pressure of about 0.1 to 0.4 MPa using fine particles such as glass beads and ceramic particles having an average particle diameter of 100 ⁇ m or less, preferably 70 ⁇ m or less is added.
  • fine particles such as glass beads and ceramic particles having an average particle diameter of 100 ⁇ m or less, preferably 70 ⁇ m or less
  • a surface state with higher adhesion can be obtained.
  • the second compound layer having surface irregularities and excellent adhesion to the first compound layer is formed on the surface of the steel product, and a surface layer having high adhesiveness is formed.
  • an Fe—N-based first compound layer with few penetration defects and high corrosion resistance is formed on the base material side, and the corrosion resistance is also improved. Furthermore, when an oxidation treatment process that forms a thin oxide layer that does not impair adhesion to friction materials, etc., or a peening treatment process to adjust the surface condition, penetration that exists slightly in the nitride compound layer Defects are sealed, and a surface treatment layer with higher corrosion resistance can be formed. Therefore, the formed surface treatment layer is a treatment layer which has high adhesion in terms of surface shape and excellent corrosion resistance in which deterioration of the adhesion is suppressed.
  • the steel product surface-treated by the treatment method of the present invention has excellent durability by being applied to a back metal or the like that adheres friction members such as brake pads, brake shoes, and clutch plates used in automobiles, for example. It becomes a structural member. Next, examples will be described.
  • SS400 which is a general structural rolled steel plate
  • SAPH440 which is a hot rolled steel plate for automobile structures
  • SPFH590 which is a workable hot rolled high tensile steel plate for automobiles
  • the mixture was heated to 500 ° C., and the fluorination treatment layer was reduced (that is, defluorination treatment) for 20 minutes while supplying 70 volume% NH 3 gas and 30 volume% H 2 gas into the furnace. Thereafter, the temperature was raised to 550 ° C., 60 minutes, 70 volume% NH 3 gas and 30 volume% N 2 gas were supplied into the furnace to perform nitriding treatment, and cooled to room temperature in a nitrogen atmosphere. Note that the thickness of the fluorinated layer was investigated for those cooled in a nitrogen atmosphere simply by performing the above fluorination step and diffusion step, and a 1.5 to 2.0 ⁇ m fluorination layer was formed on any specimen. Confirmed that.
  • Comparative Example 1 (it is a nitriding product using a conventional fluorination treatment): The above three steel type test pieces were heated to 400 ° C. in a furnace in a nitrogen atmosphere and then diluted with nitrogen gas to 2.5% by volume. A fluorination treatment was carried out for 20 minutes while supplying NF 3 gas in the furnace. Thereafter, the temperature was raised to 550 ° C., 60 minutes, 70 volume% NH 3 gas and 30 volume% N 2 gas were supplied into the furnace to perform nitriding treatment, and cooled to room temperature in a nitrogen atmosphere.
  • the specific surface area in the table means that the actual surface area increased due to the formation of surface irregularities with respect to the measurement area, but the actual surface area was measured three-dimensionally (for example, omnifocal plus manufactured by Zeta Instruments)
  • the value of the ratio of the actual surface area / measured area when an optical 3D fine surface shape measuring device can be used) is calculated. From Table 1, in the Examples, a nitride compound layer having a low carbon concentration is formed on the surface of any steel type. Moreover, it turns out that it has a very high surface nitrogen concentration with respect to Comparative Examples 1 and 2.
  • FIG. 2 the result of having measured the density
  • the first compound layer nitrogen concentration to be considered 8% before and after ⁇ (Fe 3 N) phase, on the surface side, a 11 wt% A second compound layer is formed that appears to contain a ⁇ (Fe 2 N) phase with a higher surface nitrogen concentration.
  • the N concentration in each layer has a so-called gradient composition in which the N concentration gradually decreases from the surface, and the second compound layer has a high bonding force with the first compound layer under it even though it is a surface uneven layer, and is loaded.
  • FIG. 3 shows the results of SEM observation of the surfaces and cross sections of the example, comparative example 1, and comparative example 2. From this surface SEM photograph, it can be seen that many groove-like surface irregularities are formed on the order of microns in the example.
  • fluorine was simply concentrated on the surface, but after the appropriate diffusion treatment was applied, the fluoride was reduced and the nitridation treatment was performed. Is formed. That is, by performing a fluorination treatment including a diffusion step, the fluorine is deeply penetrated, and the penetrated fluorine component is reduced and vaporized to form a recess.
  • the formed second compound layer has a clear color difference from the first compound layer, and since the color is dark, it contains a considerable amount of light elements. You can see that it is a layer. This indicates that N has penetrated from the surrounding area due to the increase in surface area, resulting in a high N concentration, and a nitride having a different composition from that of the nitride in the first compound layer is formed and grown. Thereby, the surface unevenness becomes a more complicated shape.
  • corrugation in which the value of a specific surface area is significantly large compared with the comparative examples 1 and 2 is formed.
  • the surface layer structure of the embodiment in which the actual surface area is greatly increased has a surface shape with extremely excellent adhesiveness due to the effect of increasing the bonding area.
  • the surface layer structure of this Example does not show a large difference among the three steel types used in the test, and other steel types are similar by forming, reducing, and vaporizing a deep fluoride layer by the same method. It means that a surface shape can be formed. In the outermost surface portion of the cross-sectional SEM photograph of the example of FIG.
  • Comparative Example 2 is a salt bath nitriding product that has a large specific surface area and is generally used as a nitriding treatment for brake shoes and the like. Whereas Comparative Example 2 has a comparatively smooth surface uneven shape, the Example has a groove portion (concave portion) having a depth of 0.5 ⁇ m or more at a high density of at least 2 to 3 places per nominal length of 50 ⁇ m.
  • An adhesion evaluation test was performed using SPFH590 material.
  • the test piece was subjected to fluorination treatment under the conditions shown in Table 2. That is, after performing the specified time fluorination step with 10% by volume of NF 3 gas diluted with nitrogen gas, the supply of NF 3 gas was stopped and the specified time diffusion step was performed.
  • the fluorination step for 2.5 minutes and the diffusion step for 5 minutes were performed by the above method, and then the fluorination step for 2.5 minutes and the diffusion step for 10 minutes were further performed.
  • Example C2 is a 1 minute fluorination step and a 2 minute diffusion step followed by a 1 minute fluorination step and a 3 minute diffusion step, followed by a 1 minute fluorination step and a 5 minute diffusion step. Carried out. Thereafter, the test pieces were once soaked to 400 ° C., and increased at 3 ° C./min while reducing the fluoride layer to 580 ° C. in an atmosphere of 50 vol% NH 3 gas and 50 vol% N 2 gas. Warm up. Thereafter, 100 volume% NH 3 gas was supplied into the furnace at 580 ° C. for 30 minutes to perform nitriding treatment and cooling. Table 2 also shows the fluorinated layer thickness and surface fluorine concentration of each test piece after fluorination treatment.
  • Example C2-2 after completion of nitridation of C2, cooling was performed in a nitrogen atmosphere containing 0.1% by volume of oxygen to form an oxide layer having an average thickness of about 1.0 ⁇ m. did.
  • Example C2-3 a sample obtained by projecting the surface of the test piece after cooling C2-2 at a pressure of 0.2 to 0.3 MPa using ceramic fine particles having an average particle diameter of about 60 ⁇ m was also produced.
  • the thickness of the second compound layer is greatly influenced by the thickness of the fluoride layer and the fluorine concentration of the fluoride layer.
  • the thickness of the second compound layer is too small, the adhesiveness with the adhesive is low, so that rust easily develops, and as a result, the adhesive strength is low.
  • b of Comparative Example 1 in which the thickness of the second compound layer is excessive seems to be particularly deteriorated in adhesion between the convex portion and the underlying nitride compound layer.
  • FIG. 5 shows surface SEM photographs of Examples C2-2 and C2-3.
  • the steel material surface treatment method of the present invention is a surface treatment method mainly based on a relatively inexpensive gas nitriding treatment, but can form a highly adherent uneven layer on the steel surface and a nitrided compound having high corrosion resistance.
  • a layer can be formed. Accordingly, the steel material surface-treated by the surface treatment method of the present invention has a high adhesiveness when, for example, a friction material is adhered, and a surface layer that is extremely difficult to generate rust is formed. It is difficult to cause problems such as material peeling, that is, it can be used as a member having excellent durability.
  • the steel product obtained by the production method of the present invention has a surface layer excellent in both surface adhesion and corrosion resistance, and is suitably used as a backing metal for brake pads, brake shoes, clutch plates, etc., which are excellent in durability, for example. can do.
  • the scope of application of the present invention is not limited to this. If it is used in a place where the adhesion performance is required in an environment where corrosion resistance is required, it exhibits excellent performance in various applications.

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  • Engineering & Computer Science (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
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Abstract

L'invention concerne un produit à base d'acier qui combine une résistance à la corrosion et une adhésivité excellentes. Le produit à base d'acier est obtenu par formation d'une couche de composé de nitrure et d'une couche de diffusion d'azote sur la couche superficielle d'un matériau à base d'acier. La couche de composé de nitrure contient une première couche de composé qui est formée sur le côté couche de diffusion d'azote, et une deuxième couche de composé qui est formée sur la surface de la première couche de composé. La première couche de composé présente une structure ε composée principalement de Fe3N, et la deuxième couche de composé présente une concentration en azote supérieure à celle de la première couche de composé, et présente des saillies et des creux formés sur la surface. Cette configuration permet de former une couche de composé de nitrure dotée d'une excellente adhésivité, d'une teneur en carbone extrêmement basse et d'une haute résistance à la corrosion.
PCT/JP2012/061166 2011-06-24 2012-04-19 Produit à base d'acier et son procédé de fabrication Ceased WO2012176551A1 (fr)

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JP6308041B2 (ja) * 2014-06-17 2018-04-11 株式会社ジェイテクト 摩擦板、摩擦板の製造方法及び検査方法
JP6487276B2 (ja) * 2015-06-01 2019-03-20 株式会社ジェイテクト 摺動部材の製造方法およびクラッチプレートの製造方法
CN106868444A (zh) * 2017-03-29 2017-06-20 济南弘正科技有限公司 一种离合器外套组合表面氧化处理工艺
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JP7268983B2 (ja) * 2018-09-14 2023-05-08 三井化学株式会社 建築材料および建築材料の製造方法
JP7258598B2 (ja) * 2019-02-27 2023-04-17 三井化学株式会社 接合構造体および金属部材
JP6818207B1 (ja) * 2019-07-24 2021-01-20 Ｒｔｍ 株式会社 金型の冷却孔の表面処理方法
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