WO2018216514A1 - 高温部品及びその製造方法 - Google Patents
高温部品及びその製造方法 Download PDFInfo
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- WO2018216514A1 WO2018216514A1 PCT/JP2018/018416 JP2018018416W WO2018216514A1 WO 2018216514 A1 WO2018216514 A1 WO 2018216514A1 JP 2018018416 W JP2018018416 W JP 2018018416W WO 2018216514 A1 WO2018216514 A1 WO 2018216514A1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/007—Alloys based on nickel or cobalt with a light metal (alkali metal Li, Na, K, Rb, Cs; earth alkali metal Be, Mg, Ca, Sr, Ba, Al Ga, Ge, Ti) or B, Si, Zr, Hf, Sc, Y, lanthanides, actinides, as the next major constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
- B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0433—Nickel- or cobalt-based alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/055—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 20% but less than 30%
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
- B33Y40/20—Post-treatment, e.g. curing, coating or polishing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Definitions
- the present invention relates to a high-temperature component made of a ⁇ ′ (gamma prime) precipitation-strengthened Ni-base alloy and a method for manufacturing the same.
- high-temperature parts such as a turbine part of a gas turbine engine are made of a superalloy material that exhibits predetermined mechanical properties in a high-temperature environment.
- a superalloy material a ⁇ ′ precipitation strengthened Ni-based alloy is known in which an intermetallic compound called a ⁇ ′ phase is finely precipitated to improve high temperature strength.
- the ⁇ 'precipitation strengthened Ni-base alloy is, for example, Cr (chromium), W (tungsten), Mo (molybdenum), Re (rhenium) It contains at least one of Co (cobalt) and combines with Ni (nickel) to form a ⁇ ′ phase (mainly Ni 3 (Al, Ti)) as a main element such as Al (aluminum), Ti ( It contains at least one of titanium), Ta (tantalum), Nb (niobium) and V (vanadium).
- Patent Documents 1 and 2 disclose this kind of ⁇ ′ precipitation strengthened nickel-base alloy and parts made thereof.
- the manufacturing process of a part made of a ⁇ ′ precipitation strengthened nickel-base alloy described in Patent Document 1 obtains a billet in which the alloy powder is consolidated by hot isostatic pressing (HIP) and / or extrusion consolidation.
- the crystal grain structure of the intermediate product is recrystallized at a temperature higher than the alloy's ⁇ 'solvus temperature and lower than the initial melting temperature, and the ⁇ ' precipitates are dissolved (solidified) in the alloy, and then the matrix. It undergoes age hardening treatment for reprecipitation of the ⁇ 'phase inside or at the grain boundary.
- the total content of Al, Ti, and Nb is 10.5% or more and 13% in atomic percent in order to set the volume ratio of the ⁇ ′ phase to 40 to 50%. It is as follows. A part made of this alloy is obtained by solidifying an alloy powder by hot isostatic pressing and / or drawing, forming the part by isothermal forging, and subjecting the formed part to a recrystallization heat treatment. Is obtained by cooling. In the recrystallization heat treatment, by processing at a temperature higher than the solvus temperature of the ⁇ ′ phase of the alloy and lower than the melting start temperature of the alloy, a part having a coarse grain microstructure exceeding 15 ⁇ m is obtained.
- MIM metal injection molding
- the MIM manufacturing process generally includes a step of obtaining a compound by uniformly kneading metal powder and a binder (plastic + wax), a step of obtaining an intermediate molded body by injecting the compound into a mold and releasing the mold, and heating. , Removing the binder from the intermediate molded body with a catalyst or a solvent (degreasing), and sintering the degreased intermediate molded body to obtain a molded body (powder molded body).
- MIM can form three-dimensional shapes with near net shape, has high material yield, can reduce material costs and post-processing costs, and has relatively short production running time and high productivity. There are excellent points. Therefore, if MIM is applied to a manufacturing method for high-temperature parts, there are many advantages such as providing high-temperature parts at low cost.
- the inventors of the present application employ an alloy having a typical composition of IN713C (hereinafter referred to as “IN713C-MIM”) as an example of a ⁇ ′ precipitation-strengthened Ni-based alloy constituting a high-temperature part manufactured by MIM. -The high temperature characteristics of MIM were examined.
- IN713C is one of ⁇ ′ precipitation-strengthened Ni-based alloys having excellent creep resistance.
- IN713C-MIM has low creep resistance compared to parts manufactured by casting, and has reached a high temperature characteristic that can be adopted as high temperature parts such as turbine parts. The current situation is not.
- Patent Documents 1 and 2 disclose a powder forging method in which a sintered body of alloy powder is forged. As disclosed in Patent Documents 1 and 2, it is known that a crystal grain can be coarsened by causing recrystallization and grain growth by heat treatment after applying strain by isothermal forging or cold forging to a part before heat treatment. Yes. This is because, when the free energy of the material is increased due to the dislocation accumulated in the crystal grains due to the applied plastic strain, the recrystallized grains generated using this free energy as the driving force become fine, This is because the grain boundary energy, which is the driving force for grain growth, is higher as the crystal grains are finer.
- both MIM and forging are raw material technologies, and forging a powder compact formed by MIM is not usually performed, and MIM and forging are incompatible.
- the present invention has been made in view of the above circumstances, and its purpose is to use a powder forming method excluding a method including plastic working such as powder forging, from a metal powder, from a ⁇ ′ precipitation strengthened Ni-based alloy.
- a technique for coarsening the crystal grains of the structure of high-temperature parts is proposed.
- a typical composition of IN713C contains 0.08 to 0.20% by mass of C (carbon), and a powder compact obtained by molding an alloy powder of this composition by MIM further has a C content.
- carbides metal carbide
- the inventors of the present application presumed that carbides (metal carbide) existing at the crystal grain boundaries of the powder molded body hindered the grain boundary movement and inhibited the crystal grain growth, and the IN713C-MIM crystal grains were coarse. It came to the idea that one of the causes of the failure was the amount of carbon contained in the IN713C-MIM powder compact.
- the manufacturing method of the high temperature component which concerns on 1 aspect of this invention is the following.
- a crystal grain coarsening step of coarsening the crystal grain size of the powder compact by heat treatment The powder compact is characterized by containing 0.002% or more and 0.07% or less of C and 5.40% or more and 8.40% or less of Al + Ti by mass percentage.
- the content of C that is present in the grain boundaries of the powder compact and generates carbides that inhibit crystal grain growth is 0.002% by mass or more and 0.07% by mass in the powder compact. It was found that the crystal grain size of the resulting high-temperature part was grown from the particle size of the alloy powder by limiting to not more than%. A high temperature component having a crystal structure coarsened by such crystal grain growth is expected to have high creep resistance.
- a high-temperature part made of a reinforced Ni-base alloy, having an average crystal grain size of 150 ⁇ m or more, a crystal grain structure having an equiaxed structure in all three orthogonal cross sections and a non-dendritic structure is manufactured. be able to.
- a metal structure in which the average of the dimensional ratio (aspect ratio) between the major axis and the minor axis of each crystal grain is less than 2 is defined as “equiaxial structure”.
- the C content may be greater than 0.03% and 0.07% or less in terms of mass percentage.
- the ⁇ ′ precipitation strengthened Ni-based alloy has a mass percentage of Nb + Ta of not more than 4.60%, Cr of not less than 5.00% and not more than 22.80% in addition to C, Al, and Ti. 19.50% or less of Co, 1.80% or more and 13.75% or less of Mo + W, 0.10% or less of B, 1.0% or less of Zr, and 2.0% or less of Hf. It may be.
- the ⁇ ′ precipitation-strengthened Ni-based alloy has a mass percentage of C of 0.03% to 0.07%, Al + Ti of 6.00% to 7.50%, 50% to 3.00% Nb + Ta, 11.00% to 15.00% Cr, 3.80% to 5.20% Mo, 0.005% to 0.020% B And 0.05% or more and 0.20% or less of Zr, and the balance may be made of Ni and inevitable impurities.
- the method for producing a high-temperature component is isotropic to the powder compact using gas pressure, which is performed between the molding step and the crystal grain coarsening step or simultaneously with the crystal grain coarsening step.
- a porosity reduction step of reducing the porosity by applying pressure may be further included.
- the crystal grain coarsening step includes heating the powder compact at a predetermined coarsening treatment temperature in a vacuum atmosphere or an inert gas atmosphere, It is preferable that the heat treatment temperature is a temperature in a range of not less than the pinning effect disappearance temperature inherent to the powder compact and not more than the solidus temperature of the powder compact.
- the solidus temperature may be a value obtained by adding a predetermined ⁇ ° C. to the solidus temperature obtained by experiment.
- the C content may be greater than 0.03% and 0.07% or less in terms of mass percentage.
- the said powder molded object is 4.60% or less Nb + Ta, 5.00% or more and 22.80% or less Cr in addition to C, Al, and Ti. 19.50% or less of Co, 1.80% or more and 13.75% or less of Mo + W, 0.10% or less of B, 1.0% or less of Zr, and 2.0% or less of Hf. It may be.
- the powder compact is 0.03% to 0.07% C, 6.00% to 7.50% Al + Ti, 1.50% in mass percentage.
- Nb + Ta of 3.00% or less, 11.00% or more and 15.00% or less of Cr, 3.80% or more and 5.20% or less of Mo, 0.005% or more and 0.020% or less of B, and It may contain 0.05% or more and 0.20% or less of Zr, with the balance being made of Ni and inevitable impurities.
- the specific powder forming method may include a powder forging method, and the forming step may include collecting the alloy powder into the shape of the high-temperature part and baking it. .
- the forming step includes injecting a compound obtained by kneading the alloy powder and a resin binder into a mold to form an intermediate formed body, and degreasing the intermediate formed body. And sintering the degreased intermediate molded body to obtain the powder molded body.
- the MIM to obtain a powder molded body molded into the shape of a high-temperature part, a high-temperature part with high shape accuracy can be obtained. Furthermore, by using MIM, the yield of the material is high, the material cost and the post-processing cost can be reduced, the production running time is relatively short, and the improvement of productivity can be expected.
- an average particle diameter of the alloy powder is 20 ⁇ m or more and 60 ⁇ m or less.
- the alloy powder has the above average particle diameter, it is expected that the resin binder can be easily removed from the gaps between the powders when the intermediate formed body is degreased.
- the alloy powder preferably contains 0.002% or more and 0.02% or less of C in terms of mass percentage.
- the grain when manufacturing a high-temperature part made of a ⁇ ′ precipitation-strengthened Ni-based alloy having excellent high-temperature characteristics from a metal powder using a molding method other than forging such as MIM,
- the grain can be coarsened.
- FIG. 1 is a flowchart of a method for manufacturing a high-temperature component.
- FIG. 2 is a flowchart of the process of the molding process.
- FIG. 3 is a table of structure photographs corresponding to the criteria for evaluation of crystal grain coarsening.
- FIG. 4 is a table of the structure photographs corresponding to the evaluation criteria for crystal grain coarsening.
- FIG. 5 is a diagram showing an example of a DSC thermogram of the powder compact.
- FIG. 6 is a chart showing the results of creep tests of high-temperature parts.
- the method for manufacturing a high-temperature component according to the present invention is used as a method for manufacturing a high-temperature component suitable for use in a severe high-temperature environment such as a turbine component of a gas turbine engine.
- This high-temperature component is made of a ⁇ ′ precipitation-strengthened Ni-base alloy having higher high-temperature strength (particularly creep resistance) than stainless steel and heat-resistant steel.
- Table 1 shows the ratio (mass percentage) of elements contained in the ⁇ ′ precipitation-strengthened Ni-based alloy (hereinafter simply referred to as “alloy”) constituting the high-temperature component.
- alloy has a mass percentage of 0.002% or more and 0.07% or less (preferably 0.006% or more and 0.07% or less, more preferably greater than 0.03% and 0.07% or less).
- the sum (Al + Ti) of the content rate of Al (aluminum) and the content rate of Ti (titanium) in the alloy is 5.40% or more and 8.40% or less in mass percentage.
- the alloy includes, in mass percentage, Cr (chromium) of 5.00% to 22.80%, Co (cobalt) of 19.50% or less (including 0%). ), 1.80% to 13.75% Mo (molybdenum) + W (tungsten), 4.60% or less (including 0%) Nb (niobium) + Ta (tantalum), 0.10% or less (0 B) (excluding%), Zr (zirconium) of 1.0% or less (excluding 0%), Hf of 2.0% or less (including 0%), Ni (nickel) and impurities as the balance It may be contained.
- ⁇ ′ precipitation strengthened Ni-based alloys As alloys having the compositions shown in Table 1, ⁇ ′ precipitation strengthened Ni-based alloys (alloy trade names: IN713C, IN713LC, Mar-M246 + Hf, Mar-M247, CM247LC, B1900, B1900 + Hf, Rene'80, IN738) , IN738LC, IN792, Rene'95, IN939, alloy ⁇ (original alloy)), the ratio of C is 0.002% by mass or more and 0.07% by mass or less (preferably, 0.005% or less). 006% by mass or more and 0.07% by mass or less, more preferably more than 0.03% by mass and 0.07% by mass or less).
- the ⁇ ′ precipitation-strengthened Ni-based alloy based on the typical composition of IN713C, IN713LC, and alloy ⁇ shown in Table 2 is 0.002% to 0.07% (preferably 0% by mass). 0.006% or more and 0.07% or less, more preferably more than 0.03% and 0.7% or less) C, 6.00% or more and 7.50% or less Al + Ti, 1.50% or more and 3.00 or more. % Nb + Ta, 11.00% to 15.00% Cr, 3.80% to 5.20% Mo, 0.005% to 0.020% B, 0.05% to 0 .20% or less of Zr, with the balance being Ni and inevitable impurities.
- the ⁇ ′ precipitation-strengthened Ni-based alloy based on the typical composition of alloy ⁇ shown in Table 2 is 0.002% or more and 0.07% or less (preferably 0.006%) by mass percentage. 0.07% or less, more preferably 0.03% or more and 0.7% or less) C, 6.00% or more and 7.50% or less Al + Ti, 1.80% or more and 3.00% or less. Nb + Ta, 13.00% to 15.00% Cr, 3.80% to 5.20% Mo, 0.005% to 0.020% B, 0.05% to 0.20% It contains the following Zr, with the balance being Ni and inevitable impurities.
- FIG. 1 is a flowchart showing a flow of manufacturing a high-temperature component.
- the manufacturing process of a high-temperature part includes a forming step (step S1) for forming a powder formed body having a desired high-temperature part shape from an alloy powder, and pressurizing the formed powder formed body.
- the manufacturing process of the high-temperature component further includes a hardening step (step S4) for hardening the powder compact with the coarsened particle size after the crystal grain coarsening step (step S3) depending on the type of alloy. You can leave.
- step S1 a powder compact is formed from the alloy powder using a specific powder forming method.
- the powder compact takes into account some deformation that occurs in the porosity reduction process (step S2) and the heat treatment process (step S3 and step S4), which will be described later. Presents a near net shape.
- MIM is adopted as a powder molding method.
- the molding method of the powder compact is not limited to MIM, and a powder molding method other than the powder forging method may be employed.
- a powder forming process involves collecting the alloy powder into a high temperature part shape and baking it.
- powder molding methods include MIM, press compression molding, hot isostatic pressing (HIP), cold isostatic pressing (CIP), and additive manufacturing (AM). Any one of them may be adopted.
- HIP hot isostatic pressing
- CIP cold isostatic pressing
- AM additive manufacturing
- alloy powder is filled into a high-temperature part-shaped capsule, an intermediate product is formed by applying uniform high pressure and high temperature to the capsule, and the intermediate product is sintered to obtain a powder compact.
- the cold isostatic pressing method an alloy powder is sealed in a high-temperature part shape, a uniform liquid pressure is applied thereto to form an intermediate product, and the intermediate product is sintered to obtain a powder compact.
- the alloy powder is melted and solidified layer by layer with a laser or an electron beam to form a powder molded body having a desired shape. Note that a method including plastic working such as forging, extrusion, rolling, and drawing is not used as a method for forming the powder compact.
- cold plastic processing and isothermal plastic processing below the recrystallization temperature of the material such that dislocations due to plastic strain applied to the material remain are not used for forming a powder compact.
- FIG. 2 is a flowchart of processing in the molding process.
- the alloy powder and the binder are uniformly kneaded to obtain a compound thereof (step S11).
- the compound is formed into pellets with good moldability using a pelletizer.
- the binder may be one conventionally used for MIM, for example, polypropylene (PP), polyethylene (PE), polyacetal (POM), polymethyl methacrylate (PMMA), carnauba wax (CW). ), Paraffin wax (PW), and stearic acid (St).
- Table 3 shows the ratio (mass percentage) of elements contained in the alloy powder.
- This alloy powder is a Ni-based alloy powder containing, by mass percentage, 0.002% or more and 0.02% or less of C and 5.40% or more and 8.40% or less of Al + Ti.
- this alloy powder is 4.60% or less (including 0%) Nb + Ta, 5.00% or more and 22.80% or less of Cr, 19.50 by mass percentage.
- % Of Co (including 0%), Mo + W of 1.80% or more and 13.75% or less, B of 0.10% or less (excluding 0%), 1.0% or less (excluding 0%) Zr, Hf of 2.0% or less (including 0%), Ni and impurities may be contained as the balance.
- the alloy powder has an average particle diameter of 20 ⁇ m or more and 60 ⁇ m or less, desirably 30 ⁇ m or more and 50 ⁇ m or less.
- the average particle diameter is represented by a volume-based median diameter (d50).
- the volume-based median diameter is 50% when the sample is measured using a particle size distribution measuring device based on the laser diffraction / scattering method and the particle size distribution (cumulative distribution) is obtained. Is defined as the particle size.
- This average particle size is larger than the average particle size (about 10 ⁇ m) of the metal powder used in the conventional general MIM.
- the compound obtained as described above is injected into a cavity of a desired high-temperature part shape of a mold using an injection molding machine (step S12). Then, the mold is opened, and the green body (intermediate molded body) is released from the mold (step S13).
- the green body is obtained by injection molding a compound that is a kneaded product of an alloy powder and a binder.
- Degreasing methods include a method of degreasing by immersing the green body in an organic solvent or water, and a method of degreasing by heating the green body in a degreasing incinerator at 100 to 600 ° C.
- the degreased green body is sintered to obtain a powder compact (step S15).
- the degreased green body is generally heated at 1200 to 1300 ° C. for 0.5 to 3 hours.
- the sintering conditions used are determined in consideration of economics so that the powder compact is sufficiently densified (for example, a specific density of 95% or more) and a combination of temperature and time. This sintering process may be performed continuously with the above-described degreasing process.
- the carbon content of the powder molded body is 0.002% or more and 0.07% or less (desirably, 0.006% or more and 0.07% or less, more preferably greater than 0.03% by mass percentage).
- the process of the molding process of the powder compact is controlled so that it becomes 0.07% or less.
- the carbon content of the alloy powder is limited to 0.002% or more and 0.02% or less.
- the binder is removed from the gaps between the powders of the powder compact in the degreasing process by adopting an alloy powder having a larger particle size than in the past. Easy to use.
- step S2 a gas pressure is applied to the powder compact so as to reduce the porosity of the powder compact obtained in the molding step (step S1). Since the porosity in the powder compact can also be a pinning factor that inhibits the growth of crystal grains, the smaller the porosity of the powder compact after the porosity reduction step (step S2), the better.
- step S2 for example, HIP (hot isostatic pressing) is used.
- HIP hot isostatic pressing
- a gas pressure a high temperature of 900 to 1300 ° C. and an isotropic pressure of several tens to 200 MPa are simultaneously applied to a powder compact that is an object to be treated.
- the type of gas used in HIP is an inert gas (eg, Ar), and the parameters of HIP can be changed according to the alloy composition and the target cycle time of processing, but the temperature, pressure, and time are It is preferable to set it to a degree sufficient to substantially eliminate the porosity.
- step S3 a coarsening heat treatment for coarsening the crystal grains of the powder compact is performed.
- the powder compact is heated at a predetermined coarsening temperature for a predetermined coarsening time in a vacuum or an inert gas atmosphere.
- the vacuum atmosphere means a space state where the pressure is less than 1000 Pa.
- the “inert gas atmosphere” means a space state substituted with an inert gas such as Ar of 1000 Pa or more.
- carbides composed of metal atoms and carbon atoms such as Ti, Nb, Ta, Hf, Mo, Cr, and Ni contained in the alloy.
- carbides composed of metal atoms and carbon atoms such as Ti, Nb, Ta, Hf, Mo, Cr, and Ni contained in the alloy.
- MC carbide in which Ti, Nb, Ta, Hf and C are bonded at a ratio of about 1: 1, M 6 C carbide in which C and Mo, Ni, Cr, etc. are bonded in a ratio of about 6: 1, Cr, Mo, etc.
- M 23 C 6 carbide in which C and C are bonded at a ratio of about 23: 6 is known (“M” represents a metal element).
- MC carbide is the most stable at high temperature, and the inventors of the present application have described a pinning force in which carbide present in the crystal grain boundary of the powder molded body, mainly MC carbide, tries to hinder the movement of the grain boundary. I think that is expressed. It has been found from experiments that this pinning effect drops sharply at a certain temperature. Hereinafter, the temperature at which the pinning effect rapidly decreases is referred to as “pinning effect disappearing temperature”. At the temperature at which the pinning effect disappears, the carbide that exists at the grain boundary and exhibits the pinning effect is decomposed, or the energy of grain boundary movement overcomes the pinning force and is swallowed by the grain boundary where the carbide moves.
- the pinning effect disappearance temperature is experimentally obtained in advance, and the coarsening temperature is set to a temperature equal to or higher than the pinning effect disappearance temperature and equal to or lower than the solidus temperature of the powder compact.
- the solidus temperature of the powder compact is a temperature at which a liquid phase is first generated from the powder compact, and depends on the composition of the powder compact and its carbon content. When the coarsening temperature exceeds the soridus temperature, a liquid phase having a low melting point of some of the elements constituting the powder compact is formed and a partially molten layer is formed at the grain boundary.
- FIG. 5 shows an example of a DSC thermogram obtained by measuring the powder compact with a differential scanning calorimeter (DSC).
- the differential scanning calorimeter measures the temperature of the reference material and the sample while applying a certain amount of heat to the sample, captures the thermal properties of the sample as a temperature difference, and measures endothermic and exothermic reactions due to changes in the sample state.
- Device In the DSC thermogram shown in FIG. 5, the vertical axis represents heat flow (Heat Flow) [mJ / s], and the horizontal axis represents temperature [° C.].
- an exothermic peak is observed at the solvus temperature, and an endothermic peak is observed between the solidus temperature and the liquidus temperature.
- the temperature at the beginning of the end of the endothermic peak is defined as the solidus temperature, and the temperature at which the endothermic peak is fully increased is defined as the liquidus temperature.
- the coarsening time is affected by the coarsening temperature in addition to the shape of the powder compact and the carbon content.
- the longer the coarsening treatment time the greater the degree of coarsening of the crystal grains, but it is uneconomical if the coarsening treatment time is long. Therefore, the coarsening time may be determined based on the balance between the size of the crystal grains for the high temperature parts to have the desired creep resistance and the economy, based on the results obtained through experiments.
- the coarsening heat treatment is performed in a vacuum atmosphere, Cr contained in the alloy evaporates, or Cr diffuses at the grain boundary in the process of evaporating, so that Cr is concentrated at the grain boundary. . Therefore, in order to avoid the evaporation of Cr in the alloy, the coarsening heat treatment is performed in an inert gas atmosphere.
- the porosity reduction step (step S2) is performed between the forming step (step S1) and the crystal grain coarsening step (step S3).
- the porosity reduction step (step S2) is a crystal grain coarsening. It may be performed simultaneously with the process (Step S3). Further, as will be described later, when the porosity reduction step (step S2) is omitted, the grain coarsening step (step S3) is performed continuously to the sintering process of the forming step (step S1). Also good.
- step S4 predetermined solution treatment and aging treatment are performed for each alloy, and an appropriate ⁇ ′ phase is dispersed and precipitated in the matrix phase. These conditions are determined in consideration of the required mechanical characteristics. Some alloys exhibit strength without being subjected to a hardening treatment (step S4) by performing slow cooling after the crystal grain coarsening step (step S3). Further, the solution treatment can be omitted by performing rapid cooling after the crystal grain coarsening step (step S3). High-temperature components can be manufactured by the above steps (S1 to S4 or S1 to S3).
- the method for manufacturing a high-temperature part described above is to produce a powder molded body having a desired high-temperature part shape from an alloy powder of a ⁇ ′ precipitation-strengthened Ni-base alloy by using a specific powder forming method (excluding the powder forging method).
- a crystal grain coarsening step (step S3) for coarsening the crystals of the body by heat treatment.
- the porosity reduction process (step S2) and the crystal grain coarsening process (step S3) may proceed simultaneously. Further, after the crystal grain coarsening step (step S3), a heat treatment for precipitating the ⁇ ′ phase from the powder compact with the coarse crystal grain size may be performed.
- the forming step includes collecting the alloy powder into a high temperature part shape and baking it.
- a powder molding method any one of a metal powder injection molding method, a press compression molding method, a hot isostatic compression molding method, a cold isostatic compression molding method, and an additive manufacturing method is adopted. Good.
- the powder compact contains 0.002% or more and 0.07% or less of C and 5.40% or more and 8.40% or less of Al + Ti by mass percentage.
- this powder compact is 4.60% or less (including 0%) of Nb + Ta, 5.00% or more and 22.80% or less of Cr, 19.50 by mass percentage.
- % Or less (including 0%) Co, 1.80% or more and 13.75% or less Mo + W, 0.10% (excluding 0%) or less B, 1.0% or less (excluding 0%) Zr and 2.0% or less (including 0%) of Hf may be contained.
- the powder compact corresponds to IN713LC and alloy ⁇ in Table 2 in terms of mass percentage of C greater than 0.03% and less than or equal to 0.07%, Al + Ti greater than or equal to 6.00% and less than or equal to 7.50%, 50% to 3.00% Nb + Ta, 11.00% to 15.00% Cr, 3.80% to 5.20% Mo, 0.005% to 0.020% B And 0.05% or more and 0.20% or less of Zr, and the balance may be made of Ni and inevitable impurities.
- a high-temperature component having such a composition becomes a ⁇ ′ precipitation-strengthened Ni-base alloy having excellent creep resistance.
- the content of C that is present in the grain boundary of the powder molded body and that is considered to inhibit the growth of the crystal is limited, and undergoes a grain coarsening step. It is known that the crystal grain size grows from the grain size of the alloy powder. The growth of the crystal grain size is expected to improve the creep resistance of high-temperature parts. That is, according to the manufacturing method for high-temperature parts, a high-temperature part made of a ⁇ ′ precipitation-strengthened Ni-base alloy having excellent high-temperature characteristics can be manufactured from metal powder using a molding method other than forging such as MIM. it can.
- (gamma) 'precipitation strengthening type containing 0.002% or more and 0.07% or less C and 5.40% or more and 8.40% or less Al + Ti by mass percentage
- a high-temperature component made of a Ni-based alloy, having an average crystal grain size of 150 ⁇ m or more, having a crystal grain structure in which the cross sections in all three orthogonal directions are equiaxed, and a non-dendritic structure is obtained.
- the powder compact in the method for producing a high-temperature component, in the crystal grain coarsening step, is heated at a predetermined coarsening temperature in a vacuum atmosphere or an inert gas atmosphere.
- the “roughening treatment temperature” is a temperature in the range from the pinning effect disappearance temperature inherent to the powder compact to the solidus temperature of the powder compact.
- the heat treatment for coarsening the grains rapidly reduces the pinning effect of the carbide existing at the grain boundaries of the powder compact, and the temperature within the range of the pinning effect disappearance temperature to the solidus temperature of the powder compact. In this case, there is no obstacle to the movement of the grain boundary of the powder molded body, so that growth of crystal grains is expected to be promoted.
- the molding step includes injecting a compound obtained by kneading the alloy powder and the resin binder into a mold to mold an intermediate molded body (green body), and degreasing the intermediate molded body. And sintering the degreased intermediate molded body to obtain a powder molded body.
- the MIM As described above, by using the MIM to obtain a powder molded body molded into the shape of a high-temperature part, a high-temperature part with high shape accuracy can be obtained. Furthermore, by using MIM, the yield of the material is high, the material cost and the post-processing cost can be reduced, the production running time is relatively short, and the improvement of productivity can be expected.
- the volume-based average particle diameter (d50) of the alloy powder is set to 20 ⁇ m or more and 60 ⁇ m or less.
- the alloy powder used in MIM contains 0.002% or more and 0.02% or less of C by mass percentage.
- the C content of the powder compact can be suppressed to 0.07% or less.
- Step S1 A compound in which the alloy powder and the binder were uniformly kneaded was injected into a mold to obtain a plate-like green body having a thickness of about 1 to 3 mm.
- the binder used what mixed PP, POM, and PW, and what mixed PP, PMMA, and PW depending on the sample.
- Table 4 shows the ratio (mass percentage) of the elements contained in the alloy powder of each sample. In the alloy powders of samples a1-6, b1-7, c1-5, d1-12, e1-6, f1, g1, and h1, the ratio of C was changed from the composition of “alloy ⁇ ” in Table 2.
- the average particle diameter (d50) of the alloy powder is 48.0 ⁇ m in all cases except for samples a1 to 4, f2, and g2 described later.
- the obtained green body is heated and degreased while gradually raising the temperature from room temperature to 500 ° C., and further continuously heated under appropriate sintering conditions (furnace temperature and time) so that sufficient densification proceeds.
- a powder molded body was obtained.
- HIP was performed on the powder compact obtained in step S1 under an atmosphere of 1204 ° C. and 102 to 104 MPa for 4 hours. In some samples, this HIP is intentionally omitted.
- Step S3 The powder compact with the pores reduced in step S2 was heated at a coarsening treatment temperature for a coarsening treatment time in a vacuum or an Ar atmosphere.
- the coarsening treatment temperature and the coarsening treatment time are different for each sample.
- Step S4 After performing the solution heat treatment at 1204 ° C. for 2 hours on the powder compact after the coarsening heat treatment in Step S3, two-stage aging treatment is performed at 840 ° C. for 4 hours and 760 ° C. for 12 hours, A sample was obtained. In any process, a gas fan cool is performed for cooling. Step S4 was performed only for the sample for which the strength test was performed, and was omitted for the sample for which the structure was observed.
- sample observation and evaluation procedure The plate-like sample was cut so that the thickness direction was included in the visual field and then embedded in the resin, the cut surface was polished, etched with marble liquid, and the cut surface was imaged with an optical microscope. Then, using the structure photograph (image) obtained by imaging, the average grain size of the crystal was determined by the following procedures (1) to (3). In addition, when the sharpness of the image is insufficient for the evaluation of the crystal grain size in the entire thickness direction in one structural photograph, a composite photograph of a plurality of structural photographs was used as the structural photograph. In addition, the imaging range of the tissue photograph was set such that the aspect ratio between the thickness direction and the orthogonal direction was about 1: 1.
- the average particle size was 150 ⁇ m or more, it was evaluated that the crystal particle size was coarsened, and when the average particle size was less than 150 ⁇ m, it was evaluated that the crystal particle size was insufficiently coarsened.
- tissue photograph the presence or absence of the uneven distribution of the non-roughened crystal grain, the presence or absence of the partial melting of a grain boundary, and the presence or absence of evaporation of Cr were also evaluated.
- Table 5 below shows the criteria for evaluation of crystal grain coarsening
- FIGS. 3 and 4 show structural photographs corresponding to the criteria for evaluation of crystal grain coarsening.
- step S1 An experiment was conducted to verify that the carbon content of the powder compact can be reduced by the alloy powder size.
- the average particle diameter (d50) of the alloy powder is 10.9 ⁇ m, the coarsening temperature is 1280 ° C., the coarsening time is 12 hours, and the coarsening atmosphere is 10 kPa Ar. Got.
- the carbon content of the powder compact of sample a1 was 0.074% by mass.
- the average particle diameter (d50) of the alloy powder is 23.6 ⁇ m, the coarsening temperature is 1280 ° C., the coarsening time is 12 hours, and the coarsening atmosphere is 10 kPa Ar. Got.
- the carbon content of the powder compact of sample a2 was 0.050% by mass.
- the average particle size (d50) of the alloy powder is 30.7 ⁇ m, the coarsening temperature is 1280 ° C., the coarsening time is 12 hours, and the coarsening atmosphere is 10 kPa Ar. ⁇ 4 were obtained.
- the carbon content of the powder compact of sample a3 was 0.061% by mass, and the carbon content of the powder compact of sample a4 was 0.046% by mass.
- the average particle size (d50) of the alloy powder is 48.0 ⁇ m, the coarsening temperature is 1280 ° C., the coarsening time is 12 hours, and the coarsening atmosphere is 10 kPa Ar. ⁇ 6 were obtained.
- the carbon content of the powder compact of sample a5 was 0.058% by mass, and the carbon content of the powder compact of sample a6 was 0.034% by mass.
- Table 6 shows the characteristics of the alloy powders of Samples a1 to 6 and the observation and evaluation results of those samples. As is clear from Table 6, in sample a1, coarsened crystal grains were observed even inside the cross section of the sample, but the average crystal grain size did not satisfy the predetermined standard (150 ⁇ m or more). In Samples a2 to 6, coarsening of the crystal grain size was observed. In samples a2 to a6, the carbon amount of the alloy powder is the same, but the average particle size of the alloy powder is different, so that the carbon amount of the powder compact is different. Therefore, samples a2 to a6 showed differences in the degree of coarsening of the crystal grain size and the distribution of crystal grains with insufficient coarsening.
- the carbon content of the powder compact is in the range of 0.034% by mass or more and 0.061% by mass or less (generally more than 0.03% by mass and 0.07% by mass or less). Sufficient coarsening is observed. Further, when the carbon content of the powder compact was 0.074% by mass, the crystal grain size was coarsened although the standard was not satisfied. Furthermore, since the carbide is responsible for the pinning effect on the coarsening of the crystal grain size, it is easily guessed that the grain size of the crystal grain is increased even when the carbon content is smaller than 0.034% by mass. From this, it can be said that the crystal grain size is sufficiently coarsened when the carbon content of the powder compact is 0.07% or less.
- step S1 Verification of differences in grain growth due to differences in carbide-forming elements contained in alloy powder.
- the average particle diameter (d50) of the alloy powder is 48.0 ⁇ m, the coarsening temperature is 1280 ° C., the coarsening time is 12 hours, and the coarsening atmosphere is 10 kPa Ar. Got.
- elements that combine with C to form MC carbide are Ti and Nb.
- Sample Ta was obtained by the same sample preparation procedure as Sample h1 by adding Powder Ta having an average particle diameter of 25 ⁇ m to the alloy powder used in Sample h1 at a ratio of 1.65% by mass.
- Ti, Nb, and Ta are elements that combine with C to form MC carbide.
- Sample H3 was obtained by adding the powder Hf having an average particle size of 25 ⁇ m to the alloy powder used in sample h1 at a ratio of 1.50 mass% and following the same sample preparation procedure as that of sample h1.
- elements that combine with C to form MC carbide are Ti, Nb, and Hf.
- Table 7 shows the characteristics of the alloy powders of the samples h1, h2, and h3, and the observation and evaluation results of these samples.
- the crystal grain size was coarsened in all of the samples h1, h2, and h3. From the above, it has been found that in an alloy containing at least one element of Ti, Nb, Ta, and Hf, the grain size of the powder compact is increased by limiting the carbon content of the powder compact. Since not only the MC carbides formed by Ti and Nb contained in alloy ⁇ but also MC carbides formed by Ta and Hf, the coarsening of the crystal grain size was expressed, so the similar alloys shown in Table 2 Also, it is easily guessed that the grain size becomes coarse by limiting the carbon content of the powder compact.
- step S3 In the crystal grain coarsening step (step S3), an experiment for verifying an appropriate coarsening time was performed.
- the coarsening treatment temperature is set to 1280 ° C.
- the coarsening treatment time is changed to 4, 12, 36 hours
- the coarsening treatment atmosphere is set to a vacuum atmosphere higher than 10 ⁇ 2 Pa
- the coarsening treatment is performed by the above-described sample preparation procedure.
- Four types of samples b5 to 7 having different times were obtained.
- the carbon content of the powder compact was 0.034 to 0.058% by mass.
- Table 8 shows the observation and evaluation results of samples b1 to b7 having different coarsening times.
- the coarsening treatment time is 2 hours or more, and the crystal grain size is confirmed to be coarse. The particle size was coarsened.
- the coarsening treatment time was 4 hours or longer, and coarsening of the crystal grain size was confirmed, but Cr evaporation was observed.
- sample b7 partial melting was also observed. From the above, it was found that the grain size becomes coarse when the coarsening time is 2 hours or longer, but the coarsening time is desirably 4 hours or longer.
- step S3 An experiment was conducted to verify an appropriate coarsening atmosphere.
- the coarsening temperature is 1280 ° C.
- the coarsening time is 4 hours
- the coarsening atmosphere is a vacuum atmosphere higher than 10 ⁇ 2 Pa
- an Ar atmosphere of 100 Pa an Ar atmosphere of 1300 Pa
- an Ar atmosphere of 10 kPa an Ar atmosphere of 104 MPa.
- five types of samples c1 to 5 having different coarsening atmospheres were obtained by the above-described sample preparation procedure.
- the carbon content of the powder compact was 0.034 to 0.058% by mass.
- Table 9 shows the observation and evaluation results of samples c1 to 5 having different roughening treatment atmospheres. As apparent from Table 9, coarsening of the crystal grain size was confirmed in any of the samples c1 to c5, but Cr evaporation was observed in the samples c1 and c2, and partial melting was observed in the sample c5. Samples c3 and 4 showed good coarsening of the crystal grain size. From this, it was found that the evaporation of Cr can be suppressed by setting the coarsening atmosphere to an inert gas atmosphere higher than 100 Pa.
- step S3 In the crystal grain coarsening step (step S3), an experiment for verifying an appropriate coarsening temperature was performed.
- samples having different coarsening treatment temperature and coarsening treatment atmosphere were prepared, and observed and evaluated, respectively.
- the coarsening treatment temperature was varied at 1300, 1280, 1260, 1250, 1240, and 1220 ° C.
- the coarsening treatment time was 12 hours
- the coarsening treatment atmosphere was 10 kPa Ar atmosphere.
- samples d1 to d6 In each sample, the carbon content of the powder compact was 0.034 to 0.058% by mass.
- the coarsening treatment temperature was varied at 1300, 1280, 1260, 1250, 1240, 1220 ° C.
- the coarsening treatment time was 12 hours
- the coarsening treatment atmosphere was a vacuum atmosphere higher than 10 ⁇ 2 Pa.
- Samples d7 to 12 were obtained by the sample preparation procedure described above.
- the carbon content of the powder compact was 0.034 to 0.058% by mass.
- Table 10 shows the observation and evaluation results of samples d1 to d12. From Table 10, in samples d1 to 6, in the Ar atmosphere, coarsening was confirmed in sample d4 having a coarsening temperature of 1250 ° C., and no coarsening was confirmed in sample d5 having a coarsening temperature of 1240 ° C. . From this, it is estimated that in the alloys of Samples d1 to 6, the pinning effect disappearance temperature in the Ar atmosphere is 1241 ° C. or higher and 1250 ° C. or lower.
- step S2 [Verification of influence of porosity reduction process on coarsening temperature] An experiment was conducted to verify the influence of the porosity reduction step (step S2) included in the high-temperature component manufacturing method on the coarsening temperature of the crystal grain coarsening step (step S3).
- the coarsening temperature was varied at 1300, 1280 and 1260 ° C.
- the coarsening time was 12 hours
- the coarsening atmosphere was a vacuum atmosphere higher than 10 ⁇ 2 Pa
- the porosity reduction treatment Samples e3 to e6 were obtained by the above-described sample preparation procedure omitting HIP (procedure (iii)).
- the carbon content of the powder compact was 0.034 to 0.058% by mass.
- Table 11 shows the observation and evaluation results of samples e1 to e5.
- the aforementioned high-temperature part manufacturing method in which the porosity reduction step (step S2) is omitted that is, a molding step (step S1) for molding a powder compact of a desired high-temperature part shape from Ni-based alloy powder,
- the ⁇ ′ precipitation-strengthened Ni-base whose crystal grain size is increased also by a method for producing a high-temperature part including a crystal grain coarsening step (step S3) in which the crystal grain size of the powder compact is coarsened by heat treatment.
- step S3 when the porosity reduction step (step S2) was omitted and the crystal grain coarsening step (step S3) was performed in an Ar atmosphere, the crystal grains became coarse at a coarsening temperature of 1300 ° C. Since the crystal grains did not coarsen at the coarsening temperature of 1280 ° C., it is presumed that the pinning effect disappearance temperature is 1281 ° C. or higher and 1300 ° C. or lower when the porosity reduction step is omitted. Furthermore, when the porosity reduction step (step S2) was omitted and the crystal grain coarsening step (step S3) was performed in a high vacuum atmosphere, the crystal grains became coarse at a coarsening temperature of 1280 ° C.
- the pinning effect disappearance temperature is 1261 ° C. or higher and 1280 ° C. or lower when the porosity reduction step is omitted.
- Table 12 shows the pinning effect disappearance temperature estimated from the verification experiment results regarding the above coarsening temperature.
- Table 13 shows the measurement results of the solidus temperature and liquidus temperature of the powder compacts having carbon contents of 0.034 to 0.058 mass% and 0.10 mass%.
- the solidus temperature and liquidus temperature were measured by preparing samples f1 and f2 of powder compacts having carbon contents of 0.034 to 0.058% by mass and 0.10% by mass, and measuring each sample with a differential scanning calorimeter ( DSC), and the solidus temperature and liquidus temperature of each sample were determined from the results.
- the powder compact of sample f1 is molded by MIM as shown in step S1 of the above-described sample preparation procedure, but the powder compact of sample f2 is hot isostatic pressing (HIP). It is formed by.
- the powder compact of sample f2 has a predetermined composition shown in Table 4, and an alloy powder having an average particle diameter (d50) of 26.9 ⁇ m is enclosed in a can made of mild steel, and is 104 MPa at 1204 ° C. This was obtained by performing hot isostatic pressing for 4 hours in an Ar atmosphere and finally removing the mild steel.
- the porosity reduction step when the porosity reduction step is omitted, the crystal grain size of the powder compact becomes coarser in both the Ar atmosphere and the vacuum atmosphere as compared with the case of performing the porosity reduction step. It turns out that the temperature to do is high. From these, the pores in the powder compact become a pinning factor that hinders the coarsening of the crystal grain size, and when omitting the porosity reduction step, compared to the case of performing the porosity reduction step, It is inferred that the temperature at which the pinning effect disappeared became high. Therefore, in order to increase the crystal grain size of the powder compact at a relatively low coarsening temperature in the crystal grain coarsening step (step S3), the porosity reduction step (step S2) is not omitted. It can be said that this is preferable.
- test pieces and comparative test pieces were prepared by the following method, and a creep rupture test was performed in accordance with ASTM E139.
- the coarsening temperature was 1280 ° C.
- the coarsening time was 12 hours
- the coarsening atmosphere was 10 kPa Ar
- sample g1 was obtained by the above-described sample preparation procedure. From this sample g1, a test piece g1 'having a gauge distance of 12 mm, a width of 3.2 mm, and a thickness of 1.5 to 2 mm was produced. Note that the shape of the test piece g1 'deviates from the standard of ASTM E139. A creep rupture test was performed on the test piece g1 'by changing the test conditions at 927 ° C / 227 MPa and 980 ° C / 90 MPa.
- step S3 the coarsening process (step S3) is omitted in the above-described sample preparation procedure.
- a comparative sample g2 was obtained by the same procedure except that the solution treatment was performed at 1176 ° C. for 2 hours in the curing treatment (step S4) and then the aging treatment was performed at 925 ° C. for 16 hours.
- the content of C in the powder compact of Comparative Sample g2 was 0.12% by mass. From this comparative sample g2, a comparative test piece g2 'having a gauge distance of 16 to 20 mm and a size of 4 mm was prepared.
- a creep rupture test was performed on the test piece g2 ′ by changing the test conditions at 927 ° C./227 MPa, 980 ° C./90 MPa, 760 ° C./690 MPa, 816 ° C./172 MPa, 927 ° C./90 MPa, 927 ° C./50 MPa. It was.
- FIG. 6 shows the results of plotting the results of the creep rupture test converted into Larson mirror parameters.
- literature values of In713C castings described in “SUPERALLOYS II” Chester T. Sims, Norman S. Stoloff, William C. Hagel (1987) are also included for comparison.
- the degree of divergence between the curve of the sample g1 and the curve of the In713C casting is smaller than the degree of divergence between the curve of the comparative sample g2 and the curve of the In713C casting.
- the sample g1 whose crystal grain size is coarsened by the crystal grain coarsening treatment has excellent high temperature creep strength (creep resistance) compared to the comparative sample g2 whose crystal grain size is not coarsened. It can be seen that the high-temperature creep strength is improved to a level close to that of the cast product.
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Abstract
Description
γ'析出強化型Ni基合金の合金粉末から、特定の粉末成形方法を用いて所望の高温部品形状の粉末成形体を成形する成形工程と、
前記粉末成形体の結晶粒径を熱処理により粗大化させる結晶粒粗大化工程とを含み、
前記粉末成形体は、質量百分率で、0.002%以上0.07%以下のCと、5.40%以上8.40%以下のAl+Tiとを含有することを特徴としている。
成形工程(ステップS1)では、特定の粉末成形法を用いて、合金粉末から粉末成形体を成形する。粉末成形体は、後述する気孔率低減工程(ステップS2)や熱処理工程(ステップS3及びステップS4)で生じる幾分の変形が考慮されているが、実質的に所望の高温部品形状(ネットシェイプ・ニアネットシェイプ)を呈する。
気孔率低減工程(ステップS2)では、成形工程(ステップS1)で得られた粉末成形体の気孔率を減少させるように、粉末成形体にガス圧を与える。粉末成形体中の気孔も結晶粒の成長を阻害するピン止め因子となりうることから、気孔率低減工程(ステップS2)後の粉末成形体の気孔率は、少ないほどよい。
結晶粒粗大化工程(ステップS3)では、粉末成形体の結晶粒を粗大化するための粗大化熱処理を行う。粗大化熱処理は、粉末成形体を、真空又は不活性ガス雰囲気下において、所定の粗大化処理温度で、所定の粗大化処理時間だけ加熱する。この熱処理では、粉末成形体が再結晶するために十分な自由エネルギーを持っていないため、再結晶は殆ど生じないと考えられる。なお、上記において「真空雰囲気」とは、圧力が1000Pa未満の空間状態のことをいう。また、上記において「不活性ガス雰囲気」とは、1000Pa以上のArなどの不活性ガスで置換された空間状態のことをいう。
硬化工程(ステップS4)では、合金ごとに所定の溶体化処理及び時効処理を施し、母相中に適切なγ’相を分散析出させる。これらの条件は、必要とされる機械特性を勘案して決定される。なお、合金によっては、結晶粒粗大化工程(ステップS3)後に徐冷することにより、硬化処理(ステップS4)を施さずに強度を発揮するものがある。また、結晶粒粗大化工程(ステップS3)後に急冷を施すことにより、溶体化処理を省略することもできる。以上の工程(S1~S4又はS1~S3)により、高温部品を製造することができる。
次に、本発明に係る高温部品の製造方法の実施例を説明する。
以下で説明する各試料に共通する試料作製手順は、以下の通りである。
(ステップS1)
合金粉末とバインダーとを均一に混練したコンパウンドを、金型に射出して、厚さ約1~3mmの板状のグリーン体を得た。なお、バインダーは、PP、POM、及びPWを混ぜ合わせたものと、PP、PMMA,及びPWを混ぜ合わせたものとを、試料によって使い分けた。各試料の合金粉末に含まれる元素の割合(質量百分率)を表4に示す。なお、試料a1‐6、b1-7、c1-5、d1-12、e1-6、f1、g1、及び、h1の合金粉末は、表2の「alloyα」の組成からCの割合を変更したものである。
また、合金粉末の平均粒子径(d50)は、後述する試料a1~4,f2,g2を除いて、いずれも48.0μmである。
得られたグリーン体を、室温から500℃まで徐々に昇温させながら加熱脱脂し、更に連続して、十分な緻密化が進むような適切な焼結条件(炉内温度と時間)で加熱して、粉末成形体を得た。
(ステップS2)
上記ステップS1で得られた粉末成形体に対し、1204℃、102~104MPaのAr雰囲気下、4時間の条件でHIPを行った。なお、試料によっては、このHIPが意図的に省略されたものがある。
(ステップS3)
上記ステップS2によって気孔が低減された粉末成形体に対し、真空又はAr雰囲気下で、粗大化処理温度で、粗大化処理時間だけ加熱した。粗大化処理温度及び粗大化処理時間は、試料ごとに異なる。
(ステップS4)
上記ステップS3の粗大化熱処理を終えた粉末成形体に対し、1204℃で2時間の溶体化処理を施したのち、840℃で4時間と760℃で12時間の2段階の時効処理を行い、試料を得た。いずれの処理においても、冷却にはガスファンクールを実施している。なお、ステップS4は、強度試験を行う試料に対してのみ行い、組織観察を行う試料では省略した。
板状の試料を厚み方向が視野に含まれるように切断してから樹脂埋めし、その切断面を研磨し、マーブル液でエッチングし、切断面を光学顕微鏡で撮像した。そして、撮像で得られた組織写真(画像)を用いて、以下の(1)~(3)の手順で結晶の平均粒径を求めた。なお、1枚の組織写真では厚み方向の全域について画像の鮮明度が結晶粒径の評価のために不十分である場合には、複数枚の組織写真を合成したものを組織写真として用いた。また、組織写真の撮像範囲を、厚み方向とその直行方向のアスペクト比が約1:1となるようにした。
(1)組織写真の撮像範囲全域に対し、縦横それぞれ等間隔で20本ずつの線を引き、各線について粒界とが交差する数を数える。
(2)組織写真中の金属組織上(つまり樹脂上ではない)に引かれた各線の長さを写真中のスケールバーに基づいて実寸法に変換した値を、(1)で求めた数で割った値を、各線における粒径とした。
(3)樹脂部を通る線を除く各線について求めた粒径の平均値を平均結晶粒径とした。
粉末成形体の炭素量は、板状の試料をドリル等で切子状に削り出し、非分散型赤外線吸収表法を用いて測定した。ただし、MIMにより作製された粉末成形体は、バインダーの抜け性の違いから、試料最表面の炭素量が低く測定される場合があるため、試料内部から切子を採取するよう留意した。
成形工程(ステップS1)において、合金粉末サイズによって、粉末成形体の含有炭素量を減少できることを検証するための実験を行った。
成形工程(ステップS1)において、合金粉末に含まれる炭化物形成元素の違いによる結晶の粒成長を検証するための実験を行った。
結晶粒粗大化工程(ステップS3)において、適切な粗大化処理時間を検証するための実験を行った。
結晶粒粗大化工程(ステップS3)において、適切な粗大化処理雰囲気を検証するための実験を行った。
結晶粒粗大化工程(ステップS3)において、適切な粗大化処理温度を検証するための実験を行った。
高温部品の製造方法に含まれる気孔率低減工程(ステップS2)が、結晶粒粗大化工程(ステップS3)の粗大化処理温度に与える影響を検証するための実験を行った。
高温部品の高温クリープ特性を評価するために、以下に示す方法で試験片及び比較試験片を作製し、ASTM E139に準拠してクリープラプチャー試験を行った。
Claims (14)
- γ'析出強化型Ni基合金の合金粉末から、特定の粉末成形方法を用いて所望の高温部品形状の粉末成形体を成形する成形工程と、
前記粉末成形体の結晶粒径を熱処理により粗大化させる結晶粒粗大化工程とを含み、
前記粉末成形体は、質量百分率で、0.002%以上0.07%以下のCと、5.40%以上8.40%以下のAl+Tiとを含有する、
高温部品の製造方法。 - 前記成形工程と前記結晶粒粗大化工程の間に、又は、前記結晶粒粗大化工程と同時に行われる、ガス圧を利用して前記粉末成形体に等方的な圧力を加えることにより気孔率を低減させる気孔率低減工程を更に含む、
請求項1に記載の高温部品の製造方法。 - 前記結晶粒粗大化工程が、前記粉末成形体を、真空雰囲気下又は不活性ガス雰囲気下において、所定の粗大化処理温度で加熱することを含み、
前記粗大化処理温度が、前記粉末成形体に固有のピン止め効果消失温度以上前記粉末成形体のソリダス温度以下の範囲の温度である、
請求項1又は2に記載の高温部品の製造方法。 - 前記粉末成形体のCの含有量が、質量百分率で0.03%より多く0.07%以下である、
請求項1~3のいずれか一項に記載の高温部品の製造方法。 - 前記粉末成形体は、C、Al、及びTiの他に、質量百分率で、4.60%以下のNb+Ta、5.00%以上22.80%以下のCr、19.50%以下のCo、1.80%以上13.75%以下のMo+W、0.10%以下のB、1.0%以下のZr、及び、2.0%以下のHfを含有する、
請求項1~4のいずれか一項に記載の高温部品の製造方法。 - 前記粉末成形体が、質量百分率で、0.03%より多く0.07%以下のC、6.00%以上7.50%以下のAl+Ti、1.50%以上3.00%以下のNb+Ta、11.00%以上15.00%以下のCr、3.80%以上5.20%以下のMo、0.005%以上0.020%以下のB、及び、0.05%以上0.20%以下のZrを含有し、残部がNi及び不可避的不純物からなる、
請求項1~3のいずれか一項に記載の高温部品の製造方法。 - 前記特定の粉末成形方法は粉末鍛造法を除き、前記成形工程は前記合金粉末を前記高温部品形状に集めてそれを焼き固めることを含む、
請求項1~6のいずれか一項に記載の高温部品の製造方法。 - 前記成形工程が、
前記合金粉末と樹脂バインダーとを混練したコンパウンドを金型に射出して中間成形体を成形することと、
前記中間成形体を脱脂することと、
脱脂された前記中間成形体を焼結して前記粉末成形体を得ることとを含む、
請求項1~7のいずれか一項に記載の高温部品の製造方法。 - 前記合金粉末の平均粒子径が、20μm以上60μm以下である、
請求項8に記載の高温部品の製造方法。 - 前記合金粉末は、質量百分率で、0.002%以上0.02%以下のCを含む、
請求項8又は9に記載の高温部品の製造方法。 - 質量百分率で、0.002%以上0.07%以下のCと、5.40%以上8.40%以下のAl+Tiとを含有するγ'析出強化型Ni基合金からなり、平均結晶粒径が150μm以上であり、その結晶粒組織が、直交する3方向全ての断面が等軸組織であり、且つ、非デンドライト組織である、
高温部品。 - Cの含有量が、質量百分率で0.03%より多く0.07%以下である、
請求項11に記載の高温部品。 - 前記γ'析出強化型Ni基合金が、C、Al、及びTiの他に、質量百分率で、4.60%以下のNb+Ta、5.00%以上22.80%以下のCr、19.50%以下のCo、1.80%以上13.75%以下のMo+W、0.10%以下のB、1.0%以下のZr、及び、2.0%以下のHfを含有する、
請求項11に記載の高温部品。 - 前記γ'析出強化型Ni基合金が、質量百分率で、0.03%より多く0.07%以下のC、6.00%以上7.50%以下のAl+Ti、1.50%以上3.00%以下のNb+Ta、11.00%以上15.00%以下のCr、3.80%以上5.20%以下のMo、0.005%以上0.020%以下のB、及び、0.05%以上0.20%以下のZrを含有し、残部がNi及び不可避的不純物からなる、
請求項11に記載の高温部品。
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