WO2019176073A1 - 拡散接合治具用ステンレス鋼材 - Google Patents
拡散接合治具用ステンレス鋼材 Download PDFInfo
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- WO2019176073A1 WO2019176073A1 PCT/JP2018/010335 JP2018010335W WO2019176073A1 WO 2019176073 A1 WO2019176073 A1 WO 2019176073A1 JP 2018010335 W JP2018010335 W JP 2018010335W WO 2019176073 A1 WO2019176073 A1 WO 2019176073A1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3053—Fe as the principal constituent
- B23K35/308—Fe as the principal constituent with Cr as next major constituent
- B23K35/3086—Fe as the principal constituent with Cr as next major constituent containing Ni or Mn
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/02—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by means of a press ; Diffusion bonding
- B23K20/023—Thermo-compression bonding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/02—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by means of a press ; Diffusion bonding
- B23K20/023—Thermo-compression bonding
- B23K20/025—Bonding tips therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/22—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating taking account of the properties of the materials to be welded
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K37/00—Auxiliary devices or processes, not specially adapted to a procedure covered by only one of the preceding main groups
- B23K37/04—Auxiliary devices or processes, not specially adapted to a procedure covered by only one of the preceding main groups for holding or positioning work
- B23K37/0408—Auxiliary devices or processes, not specially adapted to a procedure covered by only one of the preceding main groups for holding or positioning work for planar work
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K37/00—Auxiliary devices or processes, not specially adapted to a procedure covered by only one of the preceding main groups
- B23K37/04—Auxiliary devices or processes, not specially adapted to a procedure covered by only one of the preceding main groups for holding or positioning work
- B23K37/0426—Fixtures for other work
- B23K37/0435—Clamps
- B23K37/0443—Jigs
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/34—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/42—Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/46—Ferrous alloys, e.g. steel alloys containing chromium with nickel with vanadium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/54—Ferrous alloys, e.g. steel alloys containing chromium with nickel with boron
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K2101/00—Articles made by soldering, welding or cutting
- B23K2101/04—Tubular or hollow articles
- B23K2101/14—Heat exchangers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K2101/00—Articles made by soldering, welding or cutting
- B23K2101/18—Sheet panels
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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
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/001—Austenite
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
Definitions
- the present invention relates to a stainless steel material for a diffusion bonding jig that is excellent in deformation suppression and releasability.
- the present invention also relates to a release member suitable for a manufacturing method using diffusion bonding.
- the plate heat exchanger has a structure in which a plurality of thin metal plates (plates) are stacked, and a hot medium passage and a cold medium passage are alternately formed adjacent to each other between the stacked plates. A heat exchange action is performed between the high temperature medium and the low temperature medium through the plate.
- Patent Document 1 describes a joining method such as fastening with a gasket and a screw, welding, and brazing. Small and medium-sized heat exchangers are often joined by brazing in consideration of pressure resistance. However, if plates with corrugated shapes are stacked and joined by brazing, there may be cases where joining problems peculiar to brazing materials occur, such as melting damage at the time of joining, cracking of the brazing part, channel burying by molten brazing, etc. .
- Diffusion bonding is a method of bonding by utilizing mutual diffusion of base material atoms generated at a bonding interface under a high temperature pressure in a vacuum or an inert atmosphere.
- the joint part that has been diffusion-bonded has the same strength and corrosion resistance as the base material.
- the stacked members to be bonded are pressed by a pressing means, and the pressed state is held for a predetermined time.
- diffusion bonding is performed between a member to be bonded and a pressurizing unit with a release member such as a contact plate or a spacer interposed therebetween.
- a release member such as a contact plate or a spacer interposed therebetween.
- a carbon material is used because it is required to have heat resistance against the temperature during diffusion bonding and not to be damaged.
- Patent Document 2 describes diffusion bonding means using a carbon sheet having elasticity.
- a stainless steel plate having excellent corrosion resistance is used as a metal plate from the viewpoint of improving the durability of the heat exchanger.
- a carbon material is used as a release member adjacent to the plate material, so after completing the diffusion bonding process, the plate It becomes difficult to remove the release member from the material, and the release properties of both members are lowered. Further, due to the carburization of carbon permeating into the stainless steel, there is a problem that the corrosion resistance of the plate material is lowered, or the surface roughness of the plate material is increased and the surface properties are lowered.
- the plate material that forms the flow channel in the main body of the heat exchanger has a non-joint surface portion on the flow channel side, and therefore is less constrained from the surroundings than other plate materials ((( See A)). Therefore, for example, as shown in FIG. 3 (B), the heat of the diffusion bonding process may cause thermal deformation that causes the plate material to expand to the flow path side at the non-bonding surface portion, depending on the degree of the thermal expansion.
- the deformed portion was not restored.
- the present invention has been devised to solve the above problems.
- Stainless steel for diffusion bonding jigs that suppresses deformation of the material to be bonded while maintaining the diffusion bonding property of the material to be bonded, and has excellent releasability after the diffusion bonding process (peelability between the material to be bonded and the release member).
- the purpose is to provide steel.
- the present inventors paid attention to the material and characteristics of the release member that is in direct contact with the material to be joined (plate material).
- the present invention is completed. It came.
- the present invention provides the following.
- the present invention is a stainless steel material containing 1.5 mass% or more of Si, and the high temperature strength (Fr) of the stainless steel material at 1000 ° C. and the high temperature at 1000 ° C. of the materials to be joined by diffusion bonding. It is a stainless steel material for a diffusion bonding jig having a ratio (Fr / Fp) to strength (Fp) of 0.9 or more and excellent deformation control and releasability.
- the stainless steel material is: C: 0.1 mass% or less, Si: 1.5 to 5.0 mass%, Mn: 2.5 mass% or less, P: 0.06 mass% or less S: 0.02% by mass or less, Ni: 8.0-15.0% by mass, Cr: 13.0-23.0% by mass, N: 0.2% by mass or less It is a stainless steel material for a diffusion bonding jig excellent in the described deformation suppression and releasability.
- the stainless steel material includes Mo: 3.0% by mass or less, Cu: 4.0% by mass or less, Nb: 0.8% by mass or less, Ti: 0.5% by mass or less, V: 1.0% by mass or less and B: for a diffusion bonding jig excellent in deformation suppression and releasability as described in (2) above, comprising at least one selected from the group consisting of 0.02% by mass or less Stainless steel material.
- the stainless steel material includes Al: 0.2% by mass or less, REM: 0.2% by mass or less, Y: 0.2% by mass or less, Ca: 0.1% by mass or less, and Mg :
- the present invention is a release member composed of the stainless steel material according to any one of (1) to (4) above.
- the present invention suppresses the deformation of the material to be bonded while maintaining the diffusion bonding property of the material to be bonded.
- a stainless steel material for a diffusion bonding jig that is excellent in releasability after being applied.
- FIG. 1 It is a schematic diagram for demonstrating embodiment of the to-be-joined material in a hot press apparatus. It is a figure which shows the pattern of the heating and cooling of the diffusion bonding process in an Example. It is a schematic diagram for demonstrating the measuring method of the deformation amount in an Example.
- (A) is a figure which shows the state which set the test assembly before diffusion joining
- (B) is a figure which shows the state which the plate material after diffusion joining deform
- This embodiment relates to a diffusion bonding jig used in a method of manufacturing a heat exchanger in which a plurality of materials to be bonded made of stainless steel are stacked, heated and pressurized, and diffusion bonded to the materials to be bonded.
- a release member is disposed on both surfaces of the material to be bonded
- a press jig is disposed so as to sandwich the material to be bonded via the release member, and then the press jig is interposed.
- the plate material which is the material to be joined, is diffused and joined to produce a heat exchanger.
- the release member of the diffusion bonding jig is disposed between the plate material and the holding jig.
- FIG. 1 shows an outline of a material to be joined to be subjected to diffusion bonding processing.
- a hot press apparatus that can perform pressurization and heating in a predetermined atmosphere is used.
- a material to be bonded (plate material) to be diffusion-bonded is prepared as a stacked body in which a plurality of plate materials are stacked and loaded into a pressure heating apparatus. And a mold release member is arrange
- FIG. 1 shows an example using a plate laminate 2 in which four plate materials 1 are stacked.
- the holding jig 4 is arranged so as to be in contact with each of the two release members 3 arranged outside the plate laminate 2.
- the pressing jig 4 is connected to the pressing shaft 5 of the pressing device.
- a pressurizing mechanism (not shown) is operated, the presser jig 4 presses the plate stack 2 through the pressurizing shaft 5, a predetermined pressure is applied to the plate material 1, and the pressurization state is maintained for a predetermined time. Retained.
- a pressurizing and heating apparatus that maintains a vacuum or an inert atmosphere, the plate laminate 2 of the material to be joined is pressurized and heated under predetermined conditions, and the plate material 1 is diffusion bonded.
- the plate material is not limited to four.
- the pressurizing device may be any device provided with a pressurizing mechanism such as a servo, a spring, or a weight.
- a release agent may be applied to the surface of the release member before diffusion bonding so that the material to be joined and the release member can be easily removed after diffusion bonding.
- the fluid passes through a narrow flow path formed by the plate materials, and heat exchange is performed between the high temperature side fluid and the low temperature side fluid via each plate material. It is. Therefore, the plate material is required to have good mechanical strength (high temperature strength) and corrosion resistance in a high temperature range. From this point of view, this embodiment uses stainless steel having excellent heat resistance and durability for the plate material. Moreover, it is desirable to use a thin plate shape in order to improve the heat exchange performance.
- release member made of a steel material containing 1.5% by mass or more of Si. Since the release member is placed under high temperature and high pressure in contact with the material to be bonded at the time of diffusion bonding, it is required that there is little damage or corrosion at high temperature and that it does not react with the material to be bonded.
- the release member according to the present embodiment is preferably configured using a steel material having a high Si content from the viewpoint of suppressing the reaction with the material to be joined.
- the release member according to the present embodiment includes a steel material containing 1.5 mass% or more of Si.
- Si is an easily oxidizable element and forms a strong oxide film on the surface of the release member. Since the base material of the release member and the material to be joined are in contact with each other via the Si oxide film, the reaction at the interface between the release member and the material to be joined is inhibited. By forming this Si oxide film, adhesion and interface reaction between both members are suppressed, so that after the diffusion bonding process is completed, the release member can be easily removed from the material to be bonded with a small pulling force. .
- the release member includes a steel material containing 1.5% by mass or more of Si.
- the constituent material of the release member according to this embodiment is preferably an austenitic stainless steel material having excellent heat resistance, durability, formability, etc.
- a steel material having the following composition can be used.
- C 0.1 mass% or less
- Si 1.5 to 5.0 mass%
- Mn 2.5 mass% or less
- P 0.06 mass% or less
- S 0.02 mass% or less
- Ni 8.0 to 15.0% by mass
- Cr 13.0 to 23.0% by mass
- N 0.2% by mass or less.
- Al 0.2% by mass or less
- REM 0.2% by mass or less
- Y 0.2% by mass or less
- Ca 0.1% by mass or less
- Mg a stainless steel material containing at least one selected from the group consisting of 0.1% by mass or less.
- the C improves the strength and hardness of steel by solid solution strengthening.
- the C content is preferably 0.1% by mass or less.
- Si is blended in order to form a strong oxide film on the surface of the release member, and is preferably contained in an amount of 1.5% by mass or more. Since the reaction at the interface between the release member and the material to be joined is inhibited by the formed Si oxide film, the release member can be easily removed from the material to be joined with a small pulling force after diffusion bonding. In addition, the Si oxide film prevents the components contained in the release member from penetrating into the material to be joined, so that the good heat resistance and corrosion resistance of the material to be joined are maintained, and smooth surface properties are maintained. Is maintained. When the Si content is less than 1.5% by mass, the above-described effect due to the formation of the oxide film cannot be sufficiently obtained. In addition, even if it adds exceeding 5.0 mass%, while said effect will be substantially saturated, moderate workability will not be acquired by hardening, Therefore It should just contain 5.0 mass% or less.
- Mn is an element that improves high-temperature oxidation characteristics. If contained in excess, the Mn content is preferably 2.5% by mass or less in order to reduce workability by work hardening.
- Cr is an element that forms a passive film and imparts corrosion resistance, and improves corrosion resistance. If it is less than 13.0% by mass, the effect is not sufficient. When it exceeds 23.0 mass%, workability will fall. Therefore, the Cr content is preferably 13.0 to 23.0% by mass.
- Ni is an essential element for stabilizing the austenite phase and maintaining corrosion resistance, and is also effective for workability. If the amount is less than 8.0% by mass, these effects are not sufficient. If the amount exceeds 15.0% by mass, the effect is saturated and the cost is high, so the Ni content is 8.0 to 15. 0% by mass is preferred.
- P P and S are mixed as inevitable impurities.
- N is effective as an austenite stable element and improves the high temperature strength and corrosion resistance of stainless steel together with Cr and Ni.
- the productivity is lowered, so the N content is preferably 0.2% by mass or less.
- Mo and Cu are elements that contribute to improving high-temperature strength and corrosion resistance. Both the Mo content and the Cu content are preferably 0.02% by mass or more. On the other hand, if Mo is excessively contained, there is a possibility that the ferrite phase is formed and the workability is lowered. Therefore, the Mo content is preferably 3.0% by mass or less. If Cu is excessively contained, it causes a decrease in hot workability, so the Cu content is preferably 4.0% by mass or less.
- Nb, Ti and V are effective in improving the high temperature strength.
- the Nb content is preferably 0.01% by mass or more
- the Ti content is preferably 0.01% by mass or more
- the V content is preferably 0.01% by mass or more.
- the Nb content is preferably 0.8% by mass or less
- the Ti content is preferably 0.5% by mass or less
- the V content is preferably 1.0% by mass or less.
- the B is an element that improves hot workability.
- the B content is preferably 0.0002% by mass or more.
- the B content is preferably 0.02% by mass or less.
- One or more selected from the group consisting of Mo, Cu, Nb, Ti, V and B may be added.
- Al, REM (rare earth elements), Y, Ca, and Mg are effective in improving high-temperature oxidation resistance, and one or more selected from these elements may be added.
- the Al content is preferably 0.001% by mass or more
- the REM content is preferably 0.001% by mass or more
- the Y content is preferably 0.0002% by mass or more
- the Ca content is 0.0002%.
- the mass content is preferably at least
- the Mg content is preferably at least 0.0002 mass%. However, if each element is excessively contained, the workability is lowered.
- the Al content is preferably 0.2% by mass or less
- the REM content is preferably 0.2% by mass or less
- the Y content is 0.2 mass% or less is preferable
- Ca content is preferably 0.1 mass% or less
- Mg content is preferably 0.1 mass% or less.
- the shape of the release member is appropriately selected according to the shape of the material to be joined. Since the plate material of the plate heat exchanger is generally plate-shaped, a release member disposed in contact with the plate material is used as a release plate.
- the plate thickness is preferably 2 to 10 mm, and more preferably 3 to 8 mm.
- the ratio (Fr / Fp) of the high temperature strength (Fr) at 1000 ° C. of the release member to the high temperature strength (Fp) at 1000 ° C. of the material to be joined is 0.9 or more. It is preferable to perform diffusion bonding using a combination of a material and a release member.
- the release member Since the release member is sandwiched between the material to be joined and the pressing jig during diffusion bonding and exposed to high pressure and high temperature, deformation may occur if the release member has low high temperature strength. If the release member is deformed, the uniformity of the pressure applied to the material to be joined with the release member may be impaired, which may lead to a defective joint. Therefore, in the present embodiment, the high temperature characteristics of the release member were examined based on the high temperature strength at 1000 ° C. used as a standard processing temperature during diffusion bonding.
- the release member is preferably a steel material having a high temperature strength ratio (Fr / Fp) at 1000 ° C. of 0.9 or more. If the high-temperature strength of the release member is less than 0.9 compared to the high-temperature strength of the material to be joined, the release member may be excessively deformed due to pressurization by the holding jig. Due to the deformation of the release member, the pressure applied to the material to be bonded becomes non-uniform, and the material to be bonded may be deformed. Therefore, from the viewpoint of suppressing deformation, it is preferable to use a combination of a release member having a high temperature strength ratio of 0.9 or more and a material to be joined, and more preferably 1.0 or more.
- the ratio (Tr / Tp) of the thermal expansion coefficient (Tr) of the release member and the thermal expansion coefficient (Tp) of the material to be joined at 30 ° C. to 1000 ° C. is 0.90 to 1. It is preferred to use a combination that is .60. If the material to be joined and the release member are both thermally expanded during heating, elastic deformation occurs. If there is a difference in thermal expansion between both members, the two members restrain each other's deformation to accumulate strain, which may lead to plastic deformation depending on the degree of strain.
- the material to be joined that forms the heat medium flow path (hollow part) in the heat exchanger has a portion that can be a non-joint surface on the opposite surface side even if it is in contact with the release member on one surface side.
- the joining surfaces of the materials to be joined are constrained from the surroundings, the hollow part as described above is not restrained from the surroundings, and therefore elastic deformation due to thermal expansion occurs ((( See B)). If the degree of this elastic deformation is excessive, it may become difficult to restore the shape due to plastic deformation.
- both the thermal expansion coefficients of the material to be joined and the release member may be approximately the same. preferable.
- this thermal characteristic can be evaluated based on the ratio (Tr / Tp) between the thermal expansion coefficient (Tr) of the release member and the thermal expansion coefficient (Tp) of the material to be joined.
- the thermal expansion coefficient ratio (Tp / Tr) is in the range of ⁇ 5% centering on 1.0, that is, 0.95 to 1.05. Good.
- the average cooling rate after heating in diffusion bonding is preferably less than 1.2 ° C./min. While the material to be joined and the release member are thermally expanded at the time of diffusion bonding, they are thermally contracted in the cooling process after diffusion bonding and restored to their original shapes. If there is a difference in thermal expansion between the material to be joined and the release member, both members constrain the shrinkage change during cooling, so that distortion is accumulated. If this shrinkage change becomes excessively large, plastic deformation may occur. Therefore, this embodiment focuses on the average cooling rate after the diffusion bonding is completed. When the treatment is performed at an average cooling rate of less than 1.2 ° C./min, the amount of deformation remaining after cooling can be suppressed. If the cooling rate is higher than that, the heat shrinkage change becomes large, and the amount of deformation remaining after cooling becomes large, which is not preferable.
- the average cooling rate may be controlled within a temperature range from the holding temperature during diffusion bonding to about 400 ° C.
- the holding jig is a member that is connected to the pressurizing mechanism of the pressurizing device and transmits the pressing force to the material to be joined. Since it is required to have heat resistance at the temperature at the time of diffusion bonding and not to be damaged, it is preferable to use a carbon material for the holding jig.
- release agent In the present invention, it is preferable to apply a release agent on both surfaces of the release member.
- boron night (boron nitride) spray such as hexagonal boron nitride powder (h-BN) can be used.
- the application thickness of the release agent may be three times or more (about 10 ⁇ m) of the average particle size (for example, about 3 ⁇ m) of the release agent powder.
- the final finished sheet thickness is 3 mm, and the surface finish treatment is 2B finish or 2D finish
- the cold-rolled annealed sheet was obtained.
- a plate was cut out with a size of 210 mm ⁇ 160 mm to prepare a test material. These test materials were subjected to a test relating to a material to be joined or a release member. In the component composition shown in Table 1, the balance is Fe and inevitable impurities.
- Steel No. 1 to Steel No. 5 is austenitic stainless steel.
- Steel No. 6 to Steel No. 9 is ferritic stainless steel.
- the obtained test material was subjected to a high-temperature tensile test at a strain rate of 0.3% / min at a temperature of 1000 ° C. in accordance with JIS G 0567, and 0.2% yield strength was measured. In the present specification, this measured value is the high temperature strength at 1000 ° C.
- the measurement results are shown in Table 1 (unit: MPa). And based on the measured numerical value, ratio (Fr / Fp) of the high temperature strength (Fr) of a mold release member and the high temperature strength (Fp) of a to-be-joined material was computed. The results are shown in Table 2.
- test assembly was prepared by combining four test materials for the material to be joined (plate material) and one test material for the release member (release plate). As shown in Table 2, in this test, the steel material No. Four test materials consisting of 5 were used. Two plate materials (thickness: 1.0 mm / sheet) having an opening to be a flow path were used, and a steel material No. 1-No. Two plate materials (thickness 0.4 mm / sheet) as heat transfer plates not having the above-mentioned openings are stacked so that a test material having a thickness of 3.0 mm consisting of 5 is stacked and the two plate materials are sandwiched. Arranged. A carbon jig was used as the holding jig.
- Hexagonal boron nitride powder (boron spray manufactured by YK Inoas Co., Ltd.) was applied to both surfaces of the release member as a release agent.
- the above-mentioned test assembly was subjected to diffusion bonding treatment under the following pressure and heating conditions.
- ⁇ Atmosphere Initial vacuum is 1 ⁇ 10 ⁇ 2 Pa or less ⁇ Junction temperature: 1080 ° C.
- -Temperature rising time About 2 hours from normal temperature to bonding temperature-Soaking (bonding) time: 3 hours-Average cooling rate: 3.2 ° C / min (pattern A) from 1080 ° C to 400 ° C, or 1. 1 ° C / min (B pattern)
- Pressure Surface pressure 2MPa
- FIG. 2 shows a heating and cooling pattern applied to the diffusion bonding process.
- the A pattern and B pattern in FIG. 2 show the above two patterns in which the average cooling rate is changed. After cooling to room temperature, the test assembly was taken out of the hot press apparatus and subjected to the following evaluation tests on deformation suppression and mold release.
- FIG. 3 is a schematic view showing a cross section of the test assembly.
- FIG. 3A shows a state before diffusion bonding, and a test assembly 14 in which four plate members 11a to 11d and two release plates 13 are combined with a carbon holding jig 15. A form in which pressure is applied while sandwiched is shown.
- FIG. 3B shows the state of the test assembly 14 after diffusion bonding. Since the plate materials 11a and 11d facing the cavity 16 side in the test assembly 14 after diffusion bonding are constrained by the release plate 3 and the other plate materials 11b and 11c except for the cavity portion side, they expand when heated.
- the height 17 of the highest portion deformed with reference to the surfaces of the plate materials 11a and 11d in contact with the release plate 3 was measured, and the maximum value was obtained. In the present specification, this numerical value is referred to as a deformation amount of the plate material. Based on this deformation amount, the deformation state after diffusion bonding was evaluated. The height 17 was measured using a high-speed three-dimensional shape system manufactured by Combs. From the viewpoint of suppressing deformation, the deformation was evaluated as good ( ⁇ ) when it was less than 30 ⁇ m, appropriate ( ⁇ ) when it was 30 ⁇ m to 50 ⁇ m, and inappropriate ( ⁇ ) when it was above 50 ⁇ m.
- the release plates are each steel No. 1-No. 3 is an example in which diffusion bonding is performed by the test assembly configured by No. 3;
- the amount of deformation after diffusion bonding was good ( ⁇ ) or appropriate ( ⁇ ) and was in the range of 50 ⁇ m or less, and a diffusion bonded product in which deformation was suppressed was obtained.
- the plate material and the release plate were peeled off with a small tensile force.
- the release plate could be easily detached from the material to be joined after diffusion bonding. It is presumed that the Si oxide film formed on the surface of the release plate hinders the interfacial reaction between the material to be joined and the release plate, suppresses the adhesion between both members, and improves the release property.
- Comparative Examples 1 to 12 are steel Nos. 4 to No. A release plate composed of 9 is used.
- the Si content of the steel material of the release plate is less than 1.5% by mass, which is outside the scope of the present invention. In either case, the releasability was slightly insufficient ( ⁇ ) or unsuitable ( ⁇ ), and removal after diffusion bonding was difficult.
- Comparative Examples 3 to 6, 10, and 12 had a high-temperature strength ratio of less than 0.9, the deformation after diffusion bonding was large, and the deformation suppression after diffusion bonding was inappropriate ( ⁇ ).
- the stainless steel material having the specified composition of the present invention can suppress the deformation of the material to be bonded while maintaining the diffusion bonding property of the material to be bonded. It was confirmed that an excellent diffusion bonding jig could be provided, and particularly suitable for a release member.
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Abstract
Description
図1に拡散接合の処理に供される被接合材に関する概要を示す。拡散接合を行う装置としては、所定の雰囲気内で加圧及び加熱を行うことができるホットプレス装置等が用いられる。拡散接合される被接合材(プレート材)は、複数枚のプレート材を重ねて積層された積層体として用意され、加圧加熱装置内に装填される。そして、当該積層体の両面に接するように離型部材が配置される。図1は、4枚のプレート材1を重ねたプレート積層体2を用いた例である。加圧加熱装置内では、プレート積層体2の外側に配置した2枚の離型部材3のそれぞれと接するように押え治具4が配置される。当該押え治具4は、加圧装置の加圧軸5に連結されている。加圧機構(図示なし)を作動すると、加圧軸5を通じて押え治具4がプレート積層体2を挟み込むように押圧し、プレート材1に対して所定の圧力が加わり、加圧状態が所定時間保持される。真空または不活性雰囲気を保持する加圧加熱装置内では、被接合材の上記プレート積層体2に所定条件で加圧と加熱が施されて、プレート材1は拡散接合される。なお、プレート材は、4枚に限られない。複数個のプレート積層体を用いて、各プレート積層体の間に離型部材を挿入した組立体を接合してもよい。また、図1に示したプレート材1は、内側の2枚に流路(図示しない)を設けているため、外側の2枚よりも厚みが大きくなっている。流路の組み合わせについても図1に示した構造に限られない。
本実施形態は、Siを1.5質量%以上含有する鋼材で構成された離型部材を使用することが好ましい。離型部材は、拡散接合時の被接合材と接して高温高圧下に置かれているから、高温での破損や腐食が少ないこと、被接合材と反応しないこと等が求められる。本実施形態に係る離型部材は、被接合材との反応を抑制する観点から、Si含有量の多い鋼材を用いて構成することが好ましい。
本実施形態に係る離型部材は、Siを1.5質量%以上含有する鋼材を含むものである。Siは、易酸化元素であり、離型部材の表面に強固な酸化膜を形成する。このSi酸化膜を介して離型部材の母材と被接合材とが接触するので、離型部材と被接合材との界面における反応が阻害される。このSi酸化膜の形成により、両方の部材間での接着や界面反応が抑制されるので、拡散接合処理が終了した後に、被接合材から離型部材を小さな引き離し力で容易に取り除くことができる。また、離型部材の含有成分が被接合材の内部に浸透することも上記のSi酸化膜によって阻害されるため、被接合材のステンレス鋼が有する良好な耐熱性や耐食性を維持されるとともに、平滑な表面性状が維持される。このような観点から、離型部材は、Siを1.5質量%以上含有する鋼材を含むことが好ましい。
さらに、本実施形態は、離型部材の1000℃における高温強度(Fr)と被接合材の1000℃における高温強度(Fp)との比(Fr/Fp)が0.9以上である、被接合材と離型部材との組み合わせを用いて拡散接合を行うことが好ましい。
被接合材と離型部材は、30℃~1000℃における離型部材の熱膨張係数(Tr)と被接合材の熱膨張係数(Tp)との比(Tr/Tp)が0.90~1.60である組み合わせを用いることが好ましい。被接合材と離型部材は、いずれも加熱時に熱膨張すると弾性変形が生じる。双方の部材に熱膨張差が存在すると、双方が互いの変形を拘束し合うことで歪みが蓄積されて、歪み量の程度によっては塑性変形に至る可能性がある。
拡散接合における加熱後の平均冷却速度は、1.2℃/min未満であることが好ましい。被接合材と離型部材は、拡散接合時には熱膨張する一方で、拡散接合後の冷却過程において熱収縮して元の形状に復元される。被接合材と離型部材との間に熱膨張差が存在すると、冷却時の収縮変化を双方部材が拘束し合うため、歪みが蓄積される。この収縮変化が過度の大きさになると、塑性変形を招く可能性がある。そこで、本実施形態は、拡散接合が終了した後の平均冷却速度に着目した。1.2℃/min未満の平均冷却速度で処理すると、冷却後に残存する変形量を抑制することができる。それ以上の冷却速度であると、熱収縮変化が大きくなり、冷却後に残存する変形量が大きくなり好ましくない。上記の平均冷却速度は、拡散接合時の保持温度から400℃程度までの温度範囲で制御すればよい。
押え治具は、加圧装置の加圧機構に連結されて、被接合材に対して押圧力を伝える部材である。拡散接合時の温度において耐熱性があって破損しないことが求められるので、押え治具にはカーボン材を用いることが好ましい。
本発明は、離型部材の両面には離型剤を塗布することが好ましい。例えば、六方晶窒化ホウ素粉末(h-BN)等のボロンナイト(窒化ホウ素)系スプレーを使用できる。離型剤の塗布厚みは、離型剤粉末の平均粒度(例えば約3μm程度)の3倍以上(約10μm程度)であればよい。
表1に示す成分組成を有する鋼材No.1~鋼材No.9を、30kgの真空溶解で溶製し、得られた鋼塊を厚み30mmの板に鍛造した。次いで、1200℃の熱間圧延を行い、厚み6mmの熱延板とした後、1100℃で60秒の均熱焼鈍を施して熱延焼鈍板を得た。当該熱延焼鈍板を厚み3.0mmまで冷間圧延を行った後、1100℃で均熱30秒の最終焼鈍を施し、最終仕上板厚を3mmとし、表面仕上げ処理を2B仕上または2D仕上で行い、冷延焼鈍板を得た。また、プレートに使用した鋼材No.5および鋼材No.6については、さらに、冷間圧延、焼鈍を施し、最終仕上板厚を0.4mmおよび1.0mmとし、表面仕上げ処理を2Bまたは2D仕上げで行い、冷延焼鈍材を得た。当該冷延焼鈍板から、210mm×160mmの寸法で板を切り出して試験材を作製した。これらの試験材を被接合材または離型部材に係る試験に供した。表1に示す成分組成は、残部がFeおよび不可避的不純物である。
得られた試験材を用いて、JIS G 0567に準拠し、1000℃の温度において歪速度:0.3%/minの高温引張試験を行い、0.2%耐力を測定した。本明細書では、この測定値を1000℃における高温強度とした。その測定結果を表1に示す(単位:MPa)。そして、測定された数値に基づき、離型部材の高温強度(Fr)と被接合材の高温強度(Fp)との比(Fr/Fp)を算出した。その結果を表2に示す。
得られた試験材を用いて、JIS Z 2285に準拠し、示差膨張分析装置(株式会社リガク製、赤外線加熱式熱膨張測定装置(TMA)、標準試料:石英)により昇温速度1℃/秒で30℃~1000℃に加熱した。その際の試験片の膨張量を測定し、30℃~1000℃での熱膨張係数(α30-1000℃)として算出した。その測定結果を表1に示す(単位:×10-6/℃)。
被接合材(プレート材)の試験材4枚と離型部材(離型板)の試験材1枚とを組み合わせた試験組立体を作製した。表2に示すように、本試験においては、プレート材として鋼材No.5からなる4枚の試験材を使用した。流路になる開口を有する2枚のプレート材(厚み1.0mm/枚)の試験材を使用し、離型部材には鋼材No.1~No.5からなる厚み3.0mmの試験材を重ねて、その2枚のプレート材を挟むように、上記の開口を有しない伝熱板としての2枚のプレート材(厚み0.4mm/枚)を配置した。押え治具にはカーボン製治具を用いた。離型剤として六方晶窒化ホウ素粉末(株式会社YKイノアス製ボロンスプレー)を離型部材の両面に塗布した。ホットプレス装置により、上記の試験組立体に対して以下の加圧条件および加熱条件で拡散接合処理を施した。
・接合温度: 1080℃
・昇温時間: 常温から接合温度まで約2時間
・均熱(接合)時間: 3時間
・平均冷却速度: 1080℃から400℃までを、3.2℃/min(Aパターン)、または1.1℃/min(Bパターン)
・加圧力: 面圧2MPa
変形抑制に関しては、拡散接合されたプレート材の変形量に基づいて評価した。当該変形量を測定する手法を説明する。図3は、試験組立体の断面を示した模式図である。図3の(A)は、拡散接合前の状態であり、4枚のプレート材11a~11dと2枚の離型板13とを組み合わせた試験組立体14を、カーボン製の押え治具15で挟んだ状態で加圧される形態を示している。図3の(B)は、拡散接合後の試験組立体14の状態を示している。拡散接合後の試験組立体14における空洞部16側に面したプレート材11a,11dは、空洞部側以外を離型板3、他のプレート材11b,11cで拘束されているので、加熱時に膨張すると空洞部側に屈曲するように変形する。冷却時の収縮変化によっても形状が復元しなければ、屈曲形状として残存する。離型板3に接したプレート材11a,11dの面を基準にして変形した最も高い箇所の高さ17を測定し、そのうち最大の数値を求めた。本明細書では、この数値をプレート材の変形量という。この変形量に基づいて、拡散接合後の変形状態を評価した。上記の高さ17は、コムズ製の高速3次元形状システムを用いて測定した。変形抑制の観点から、変形量が30μm未満であるときを良好(◎)、30μm~50μmであるときを適正(○)、50μm超であるときを不適(×)と評価した。
試験組立体を用いて、接合後の離型性に関して評価するため、プレート材と離型板との剥離試験を行った。その概要を図4に示す。引張装置(図示なし)と、ワイヤー26の先に吸盤25が取り付けられた治具を2つ用意した。拡散接合後の試験組立体24における2つの離型板23の表面に当該治具の吸盤25を取り付けた。一方の治具のワイヤー26に所定重量の錘27を連結した後、引張装置によって他方の治具のワイヤー26を引き上げた。試験組立体24の両面を錘27の重量で引っ張ることにより、プレート材21と離型板23とが剥離するか否かを目視で観察し、剥離の有無について確認した。錘27の重量を変化させて同様の手順で試験を繰り返した。評価基準に関しては、拡散接合後のプレート材と離型板とを小さい力で外せるのが望ましいことから、5kg以下の錘重量でプレート材と離型板とが剥離した場合は、離型性が良好(○)であり、20kg以下の錘重量でプレート材と離型板とが剥離した場合は、離型性がやや不足(△)であり、20kg超えの錘重量でプレート材と離型板とが剥離しない場合は、離型性が不良(×)であると判定した。
本試験では、鋼材No.5のオーステナイト系ステンレス鋼からなるプレート材、および鋼材No.6のフェライト系ステンレス鋼からなるプレート材に対して、それぞれ鋼材No.1~No.9の各ステンレス鋼からなる離型板を組み合わせた18種の試験組立体を用いて、高温強度、熱膨張係数、変形抑制、離型性に関する試験を行った。その試験結果を表2に示す。変形抑制と離型性については、2種の加熱冷却パターンに対して、それぞれ3個の試験組立体を用いて試験を行った。変形抑制については、3個の変形量の平均値で評価した。離型性については、3個の結果の平均で評価した。
2 プレート積層体
3 離型部材
4 押え治具
5 加圧軸
11a、11b、11c、11d プレート材
13 離型板
14 試験組立体
15 押え治具
16 空洞部
17 高さ(変形量)
21 プレート材
23 離型板
24 試験組立体
25 吸盤
26 ワイヤー
27 錘
Claims (5)
- Siを1.5質量%以上含有するステンレス鋼材であって、前記ステンレス鋼材の1000℃における高温強度(Fr)と拡散接合によって接合される被接合材の1000℃における高温強度(Fp)との比(Fr/Fp)が0.9以上である、変形抑制および離型性に優れた拡散接合治具用ステンレス鋼材。
- 前記ステンレス鋼材は、C:0.1質量%以下、Si:1.5~5.0質量%、Mn:2.5質量%以下、P:0.06質量%以下、S:0.02質量%以下、Ni:8.0~15.0質量%、Cr:13.0~23.0質量%、N:0.2質量%以下を含む、請求項1に記載の変形抑制および離型性に優れた拡散接合治具用ステンレス鋼材。
- 前記ステンレス鋼材は、Mo:3.0質量%以下、Cu:4.0質量%以下、Nb:0.8質量%以下、Ti:0.5質量%以下、V:1.0質量%以下、およびB:0.02質量%以下からなる群から選択される1種以上を含む、請求項2に記載の変形抑制および離型性に優れた拡散接合治具用ステンレス鋼材。
- 前記ステンレス鋼材は、Al:0.2質量%以下、REM:0.2質量%以下、Y:0.2質量%以下、Ca:0.1質量%以下、およびMg:0.1質量%以下からなる群から選択される1種以上を含む、請求項2または3に記載の変形抑制および離型性に優れた拡散接合治具用ステンレス鋼材。
- 請求項1~4のいずれかに記載のステンレス鋼材で構成された離型部材。
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PCT/JP2018/010335 WO2019176073A1 (ja) | 2018-03-15 | 2018-03-15 | 拡散接合治具用ステンレス鋼材 |
MYPI2019001258A MY194076A (en) | 2018-03-15 | 2018-03-15 | Release member |
EP18789305.2A EP3567127B8 (en) | 2018-03-15 | 2018-03-15 | Release member including stainless steel material for use in diffusion bonding jigs |
ES18789305T ES2835378T3 (es) | 2018-03-15 | 2018-03-15 | Elemento de liberación que incluye acero inoxidable para ser utilizado en plantillas de unión por difusión |
SG11201902184P SG11201902184PA (en) | 2018-03-15 | 2018-03-15 | Stainless Steel Material For Diffusion Bonding Jig |
KR1020187037301A KR102220875B1 (ko) | 2018-03-15 | 2018-03-15 | 변형 억제 및 이형성이 뛰어난 확산 접합 지그용 스테인리스강재로 구성된 이형 부재 |
CN201880001626.0A CN110494580A (zh) | 2018-03-15 | 2018-03-15 | 扩散接合夹具用不锈钢材 |
US16/219,039 US10695874B2 (en) | 2018-03-15 | 2018-12-13 | Stainless steel material for diffusion bonding jig |
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KR20190109225A (ko) | 2019-09-25 |
ES2835378T3 (es) | 2021-06-22 |
EP3567127A1 (en) | 2019-11-13 |
EP3567127B8 (en) | 2021-01-20 |
EP3567127A4 (en) | 2019-11-13 |
SG11201902184PA (en) | 2019-10-30 |
EP3567127B1 (en) | 2020-11-11 |
CN110494580A (zh) | 2019-11-22 |
MY194076A (en) | 2022-11-11 |
US20190283189A1 (en) | 2019-09-19 |
KR102220875B1 (ko) | 2021-02-25 |
US10695874B2 (en) | 2020-06-30 |
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