WO2013058338A1 - Matériau fritté composite de composés intermétalliques à base de nickel et procédé pour sa production - Google Patents

Matériau fritté composite de composés intermétalliques à base de nickel et procédé pour sa production Download PDF

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Publication number
WO2013058338A1
WO2013058338A1 PCT/JP2012/076998 JP2012076998W WO2013058338A1 WO 2013058338 A1 WO2013058338 A1 WO 2013058338A1 JP 2012076998 W JP2012076998 W JP 2012076998W WO 2013058338 A1 WO2013058338 A1 WO 2013058338A1
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Prior art keywords
nickel
intermetallic compound
based intermetallic
powder
sintering
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PCT/JP2012/076998
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English (en)
Japanese (ja)
Inventor
隆幸 高杉
泰幸 金野
優 川上
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公立大学法人大阪府立大学
冨士ダイス株式会社
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Priority to JP2013539689A priority Critical patent/JP6011946B2/ja
Publication of WO2013058338A1 publication Critical patent/WO2013058338A1/fr

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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
    • 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
    • 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
    • C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
    • 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
    • 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

Definitions

  • a two-phase structure comprising: a primary phase including a first nickel-based intermetallic compound; and a eutectoid phase including a first nickel-based intermetallic compound and a second nickel-based intermetallic compound.
  • the present invention relates to a nickel-based intermetallic compound composite sintered material and a method for producing the same.
  • Nickel-based superalloys in which intermetallic compounds such as nickel-based intermetallic compounds are precipitated in a matrix of nickel solid solution phase are widely used as materials having excellent high-temperature strength and wear resistance.
  • a first eutectoid of nickel-based intermetallic compound having an L1 2 type crystal structure as shown in Patent Document 1 L1 2 type crystal structure developed co eutectoid comprising a nickel-based intermetallic compound having a crystal structure of the nickel-base intermetallic compound and D0 22 type with, a material having a dual multi-phase microstructure consisting of.
  • the double-duplex structure shown in Patent Document 1 (definition and the like will be described later) has extremely excellent heat resistance because both the primary and eutectoid phases are composed of nickel-based intermetallic compounds as described above. Yes.
  • the present invention comprises a pro-eutectoid phase containing a first nickel-based intermetallic compound and a eutectoid phase containing a first nickel-based intermetallic compound and a second nickel-based intermetallic compound.
  • a material having a double-duplex structure and the obtained double-phase structure is uniform and having high strength, and a method capable of producing the material with better dimensional accuracy (near net shape).
  • the present invention combines a two-duplex structure with particles (hard particles) containing at least one selected from nitrides, carbides, carbonitrides, oxides and borides, thereby increasing the strength. It is also an object to provide a high composite material and a method for producing the same
  • a pro-eutectoid phase including a first nickel-based intermetallic compound, a first nickel-based intermetallic compound, and a second nickel-based intermetallic compound different from the first nickel-based intermetallic compound
  • a nickel-based intermetallic compound composite sintered material comprising a double-phase structure comprising a compound and a eutectoid phase, wherein the double-phase structure has an average crystal grain size of 50 ⁇ m or less. is there.
  • the first nickel-based intermetallic compound has an L1 2 type crystal structure
  • a second nickel based intermetallic compound has a crystal structure of the D0 22 type
  • the 2 multi-phase The structure includes nickel (Ni) of 50 at% or more, aluminum (Al) of 5 at% to 13 at%, vanadium (V) of 9.5 at% to 17.5 at%, and niobium (Nb of 0 at% to 5 at%).
  • Ni nickel
  • Al aluminum
  • V vanadium
  • Nb niobium
  • Aspect 3 of the present invention is that the first nickel-based intermetallic compound is Ni 3 Al or Ni 3 Al containing an element other than nickel and aluminum, and the second nickel-based intermetallic compound is Ni 3 V or nickel. And a nickel-based intermetallic compound composite sintered material according to aspect 2, which is Ni 3 V containing an element other than vanadium.
  • the two-phase structure is such that tantalum (Ta): 0.5 at% to 8 at%, tungsten (W): 0.5 at% to 8 at%, chromium (Cr): 12 at% or less (0 at %), Cobalt (Co): 15 at% or less (not including 0 at%), titanium (Ti): 0.5 at% to 3.5 at%, rhenium (Re): 0.5 at% to 5 at%, and
  • the nickel group according to any one of aspects 1 to 3, further comprising at least one selected from the group consisting of carbon (C, carbon): 12.5 at% or less (not including 0 at%) Intermetallic compound composite sintered material.
  • the double-phase structure further contains boron (B), and the boron content is 10 ppm by weight to 1000% by weight with respect to the total mass of elements other than boron in the double-phase structure.
  • B boron
  • Aspect 6 of the present invention includes titanium (Ti), zirconium (Zr), hafnium (Hf), vanadium (V), niobium (Nb), tantalum (Ta), chromium (Cr), molybdenum (Mo), tungsten (W ), Aluminum (Al), and yttrium (Y), one or more elements selected from the group consisting of carbides, nitrides, carbonitrides, oxides or borides The nickel-based intermetallic compound composite sintered material according to any one of the above.
  • a seventh aspect of the present invention is the nickel-based intermetallic compound composite according to the sixth aspect, wherein the carbide, nitride, carbonitride, oxide or boride is dispersed in the two-phase structure. It is a sintered material.
  • Aspect 8 of the present invention is a mixed powder containing nickel of 50 at% or more, aluminum of 5 at% to 13 at%, vanadium of 9.5 at% to 17.5 at%, and niobium of 0 at% to 5 at%
  • a nickel base comprising: a powder preparation step of preparing an alloy powder; and a sintering step of heating and sintering the mixed powder or alloy powder in a state where pressure is applied to the mixed powder or alloy powder. It is a manufacturing method of an intermetallic compound composite sintered material.
  • Aspect 9 of the present invention is the carbide of one or more elements selected from the group consisting of titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum, tungsten, aluminum and yttrium before the sintering step.
  • the mixed powder or alloy powder contains tantalum: 0.5 at% to 8 at%, tungsten: 0.5 at% to 8 at%, chromium: 12 at% or less (excluding 0 at%), cobalt: 15 at% or less (not including 0 at%), titanium: 0.5 at% to 3.5 at%, rhenium: 0.5 at% to 5 at%, and carbon (carbon): 12.5 at% or less (not including 0 at%)
  • Aspect 11 of the present invention is characterized in that the mixed powder or alloy powder further contains boron, and the content of boron is 10 ppm by weight to 1000 ppm by weight with respect to the total mass of elements other than boron.
  • Aspect 12 of the present invention includes a base material containing nickel of 50 at% or more, aluminum of 5 at% to 13 at%, vanadium of 9.5 at% to 17.5 at%, and niobium of 0 at% to 5 at%
  • a melting step for obtaining a molten metal in which at least the base material is melted, and atomizing the molten metal to form titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum, tungsten in a nickel-based alloy matrix Selected from the group consisting of aluminum, yttrium,
  • the base material is tantalum: 0.5 at% to 8 at%, tungsten: 0.5 at% to 8 at%, chromium: 12 at% or less (excluding 0 at%), cobalt: 15 at% or less. (Not including 0 at%), titanium: 0.5 at% to 3.5 at%, rhenium: 0.5 at% to 5 at%, and carbon (carbon): 12.5 at% or less (not including 0 at%) It is a manufacturing method of the aspect 12 characterized by further containing 1 or more types selected from more.
  • Aspect 14 of the present invention is characterized in that the base material further contains boron, and the content of boron is 10 ppm by weight to 1000 ppm by weight with respect to the total mass of elements other than boron. 13.
  • a pro-eutectoid phase including the first nickel-based intermetallic compound and a eutectoid phase including the first nickel-based intermetallic compound and the second nickel-based intermetallic compound are included. It is possible to provide a nickel-based intermetallic compound composite sintered material having a high strength and including a double-phase structure consisting of In addition, the nickel-based intermetallic compound composite sintered material according to the present invention has an average crystal grain size as fine as 50 ⁇ m or less, and the crystal grain has a uniform two-duplex structure. Moreover, the manufacturing method of the nickel base intermetallic compound composite sintered material which concerns on this invention can manufacture a nickel base intermetallic compound composite sintered material with higher dimensional accuracy.
  • nickel having higher strength can be obtained by combining a two-duplex structure and particles (hard particles) containing at least one selected from nitride, carbide, carbonitride, oxide and boride. It is also possible to provide a base intermetallic compound composite sintered material and a method for producing the same.
  • FIG. 3 is a Ni 3 Al—Ni 3 Nb—Ni 3 V suspicious ternary phase diagram at 1100 ° C. (1373 K). It is a longitudinal cross-section state diagram in Nb amount 2.5at% of the ternary system state diagram shown in FIG.
  • FIG. 3A is a scanning electron microscope (SEM) image of the obtained mixed powder
  • FIG. 3A is an SEM image of Example 1-1
  • FIG. 3B is an SEM image of Example 1-2
  • FIG. 3C is an SEM image of Example 1-3.
  • FIG. 4A is an optical micrograph showing the metal structure of the obtained dispersed nickel-based intermetallic compound composite sintered material
  • FIG. 4A is an optical micrograph of Example 1-1
  • FIG. 4B is an example.
  • FIG. 4A is an optical micrograph showing the metal structure of the obtained dispersed nickel-based intermetallic compound composite sintered material
  • FIG. 4A is an optical micrograph of Example 1-1
  • FIG. 4B is an example.
  • FIG. 4C is an optical micrograph of Example 1-3
  • FIG. 4C is an optical micrograph of Example 1-3
  • FIG. 5 (a) shows the X-ray diffraction result of Example 1-1
  • FIG. 5 (b) shows the X-ray diffraction result of Example 1-2
  • FIG. (C) shows the X-ray diffraction results of Example 1-3. It is a graph which shows the hardness HV1 measurement result in the temperature between room temperature and 900 degreeC of the obtained sample.
  • FIG. 7A is a scanning electron microscope (SEM) image of a sintering powder containing hard particles
  • FIG. 7A is an SEM image of Example 1-4
  • FIG. 7B is an SEM image of Example 1-5.
  • FIG. 7 (c) is an SEM image of Example 1-6
  • FIG. 7 (d) is an SEM image of Example 1-7
  • FIG. 7 (e) is an image of Example 1-8. It is a SEM image.
  • FIG. 8A is an optical micrograph showing a metal structure of a hard particle-dispersed nickel-based intermetallic compound composite sintered material
  • FIG. 8A is an optical micrograph of Example 1-4
  • FIG. 8 (c) is an optical micrograph of Example 1-6
  • FIG. 8 (d) is an optical micrograph of Example 1-7
  • FIG. 8 (e) These are optical micrographs of Example 1-8.
  • FIG. 8A is an optical micrograph showing a metal structure of a hard particle-dispersed nickel-based intermetallic compound composite sintered material
  • FIG. 8A is an optical micrograph of Example 1-4
  • FIG. 8 (c) is an optical micrograph of Example 1-6
  • FIG. 8 (d) is an optical micrograph of Example 1-7
  • FIG. 8 (e) These
  • FIG. 9A is an SEM image showing a metal structure of a hard particle-dispersed nickel-based intermetallic compound composite sintered material according to Example 1-6, and FIG. 9A is an SEM image of a sample after sintering; FIG. 9 is an SEM image of the sample after sintering at a high magnification, FIG. 9C is an SEM image of the sample after the heat treatment, and FIG. 9D is an SEM image of the sample after the heat treatment at a high magnification.
  • the X-ray diffraction (CuK ⁇ ) results are shown, FIG. 10 (a) shows again the X-ray diffraction results of Example 1-2 not containing TiC, and FIG.
  • FIG. 10 (b) shows the X-ray diffraction results of Example 1-4.
  • 10 (c) shows the X-ray diffraction result of Example 1-5
  • FIG. 10 (d) shows the X-ray diffraction result of Example 1-6
  • FIG. 10 (e) shows Example 1.
  • the X-ray diffraction result of ⁇ 7 is shown
  • FIG. 10F shows the X-ray diffraction result of Example 1-8.
  • the X-ray diffraction (CuK ⁇ ) result of the hard particle-dispersed nickel-based intermetallic compound composite sintered material according to Sample 1-6 is shown in more detail
  • FIG. 11 (a) shows the X-ray diffraction result after sintering.
  • FIG. 11 (b) shows the X-ray diffraction result after the heat treatment.
  • 7 is a graph showing the results of measurement of hardness HV1 at temperatures between room temperature and 900 ° C. of hard particle-dispersed nickel-based intermetallic compound composite sintered materials of Examples 1-6 and 1-8. The results of Example 1-2 are also shown for comparison.
  • FIG. 13 (a) is a SEM image showing the metal structure after sintering of the obtained nickel-based intermetallic compound composite sintered material
  • FIG. 13 (a) is an SEM image of Example 2-1
  • FIG. 13C is an SEM image of Example 2-1 at a high magnification
  • FIG. 13C is an SEM image of Example 2-2
  • FIG. 13D is an SEM image of Example 2-2 at a high magnification. It is.
  • FIG. 14A is an SEM image showing the metal structure after heat treatment of the obtained nickel-based intermetallic compound composite sintered material
  • FIG. 14A is an SEM image of Example 2-1
  • FIG. FIG. 14 (c) is an SEM image of Example 2-2
  • FIG. 14 (d) is an SEM image of Example 2-2 at a high magnification. is there.
  • the X-ray diffraction result of Example 2-1 is shown
  • FIG. 15A shows the X-ray diffraction result after sintering
  • FIG. 15B shows the X-ray diffraction (CuK ⁇ ) result after heat treatment.
  • FIG. 16 shows the X-ray diffraction (CuK ⁇ ) result of Example 2-2
  • FIG. 16 (a) shows the X-ray diffraction result after sintering
  • FIG. 16 (b) shows the X-ray diffraction result after heat treatment.
  • FIG. 17A shows an example of a pattern quality map obtained by performing crystal orientation analysis.
  • FIG. 17A shows an example of Example 2-1
  • FIG. 17B shows an example of Example 2-2.
  • the hardness HV1 after sintering and heat treatment of Examples 2-1 and 2-2 are shown.
  • FIG. 19 is an SEM image showing the metal structure after sintering of the obtained hard particle-dispersed nickel-based intermetallic compound composite sintered material
  • FIG. 19 (a) is an SEM image of Example 2-3.
  • FIG. 19B is an SEM image at a high magnification of Example 2-3
  • FIG. 19C is an SEM image of Example 2-4
  • FIG. 19D is Example 2-4. It is a SEM image in the high magnification.
  • FIG. 20A is an SEM image showing a metal structure after heat treatment of the obtained hard particle-dispersed nickel-based intermetallic compound composite sintered material
  • FIG. 20A is an SEM image of Example 2-3
  • FIG. 20C is an SEM image at a high magnification of Example 2-3
  • FIG. 20C is an SEM image at Example 2-4
  • FIG. 20D is a high magnification of Example 2-4. It is a SEM image.
  • FIG. 21A shows the X-ray diffraction results after sintering
  • FIG. 21B shows the X-ray diffraction results after heat treatment
  • the X-ray diffraction (CuK ⁇ ) result of Example 2-4 is shown
  • FIG. 22 (a) shows the X-ray diffraction result after sintering
  • FIG. 22 (b) shows the X-ray diffraction result after heat treatment.
  • the hardness HV1 after sintering and heat treatment of Examples 2-3 and 2-4 is shown.
  • FIG. 24 (a) shows the atomized powder of Example 3-1
  • FIG. 24 (b) shows the atomized powder of Example 3-2
  • FIG. 24 (c) shows the Example powder. 3-3 Atomized powder is shown.
  • FIG. 25 (a) shows the atomized powder of Example 3-1
  • FIG. 25 (b) shows the atomized powder of Example 3-2
  • FIG. 25 (a) shows the particle size distribution measurement result of the atomized powder.
  • c) shows the atomized powder of Example 3-3.
  • the X-ray-diffraction (CuK (alpha)) result of atomized powder is shown.
  • FIG. 26 (a) shows the X-ray diffraction results of Example 3-1
  • FIG. 26 (b) shows the X-ray diffraction results of Example 3-2
  • FIG. 26 (c) shows the results of Example 3-3. X-ray diffraction results are shown.
  • FIG. 27A is an optical micrograph showing a metal structure of a nickel-based intermetallic compound composite sintered material
  • FIG. 27A is an optical micrograph of Example 3-1A
  • FIG. 27B is an optical micrograph of Example 3-1B
  • Fig. 27 (c) is an optical micrograph of Example 3-2A
  • Fig. 27 (d) is an optical micrograph of Example 3-2B
  • Fig. 27 (e) is an optical micrograph.
  • FIG. 27 (f) is an optical micrograph of Example 3-3B.
  • FIG. 28A is an SEM image of Example 3-2A
  • FIG. 28B is a high magnification of Example 3-2A.
  • FIG. 28C is an SEM image of Example 3-2B
  • FIG. 28D is an SEM image of Example 3-2B at a high magnification.
  • FIGS. 29A and 29B are SEM images of Example 3-3A and Example 3-3B
  • FIG. 29A is an SEM image of Example 3-3A
  • FIG. 29B is a high magnification of Example 3-3A
  • FIG. 29C is an SEM image of Example 3-3B
  • FIG. 29D is an SEM image at a high magnification of Example 3-3B.
  • FIG. 30 (a) shows the X-ray diffraction result of Example 3-1A
  • FIG. 30 (b) shows the X-ray diffraction result of Example 3-2A
  • FIG. 30 (c) shows the X-ray diffraction result. Shows the X-ray diffraction results of Example 3-3A.
  • FIG. 31 (a) is a graph showing the results of measurement of hardness HV1 at temperatures between room temperature and 900 ° C. of Examples 3-1A, 3-2A and 3-3A
  • FIG. 3 is a graph showing the results of measurement of hardness HV1 at temperatures between room temperature and 900 ° C. for 3-1B, 3-2B and 3-3B.
  • FIG. 32A is an optical micrograph showing a metal structure of a hard particle-dispersed nickel-based intermetallic compound composite sintered material according to Examples 3-4 to 3-6
  • FIG. 32A is an optical micrograph of Example 3-4.
  • FIG. 33A is an SEM image showing the metal structure of the hard particle-dispersed nickel-based intermetallic compound composite sintered material according to Examples 3-4 and 3-6.
  • FIG. 33 (a) is an SEM image of Example 3-4.
  • 33 (b) is a higher magnification SEM image of Example 3-4
  • FIG. 33 (c) is an SEM image of Example 3-6
  • FIG. It is a higher magnification SEM image of ⁇ 6.
  • FIG. 34A is an SEM image showing the metal structure of the obtained hard particle-dispersed nickel-based intermetallic compound composite sintered material according to Examples 3-7 and 3-8.
  • FIG. 34A is an SEM image showing the metal structure of the obtained hard particle-dispersed nickel-based intermetallic compound composite sintered material according to Examples 3-7 and 3-8.
  • FIG. 34 (a) is an SEM image of Example 3-7.
  • 34 (b) is a higher magnification SEM image of Example 3-7
  • FIG. 34 (c) is an SEM image of Example 3-8
  • FIG. 34 (d) is Example 3. It is an SEM image at a higher magnification of ⁇ 8.
  • 6 is a graph showing the results of measurement of hardness HV1 at temperatures between room temperature and 900 ° C. of hard particle-dispersed nickel-based intermetallic compound composite sintered materials of Examples 3-4 to 3-6.
  • 7 is a graph showing the results of measurement of hardness HV1 at room temperature of hard particle-dispersed nickel-based intermetallic compound composite sintered materials of Examples 3-7 and 3-8.
  • FIG.37 (a) shows the transmission electron microscope (TEM) image of 2 double phase structure
  • FIG.37 (b) shows FIG.37 (a).
  • FIG. 37 (c) shows another electron microscope image of a double-duplicated phase structure, which is obtained from a limited-field electron diffraction image obtained from a region surrounded by a circle inside.
  • 38 is an SEM image showing the metal structure of the obtained dispersed nickel-based intermetallic compound composite sintered material
  • FIG. 38 (a) is an SEM image of Example 1-1, and FIG.
  • FIG. 38 (b) is an example 1- 1 is a higher magnification SEM image of 1; 40 is an optical micrograph showing the metal structure of the hard particle-dispersed nickel-based intermetallic compound composite sintered material according to Example 4, and FIG. 39 (a) is an optical micrograph of Example 4-1, and FIG. ) Is an optical micrograph of Example 4-2, FIG. 39 (c) is an optical micrograph of Example 4-3, and FIG. 39 (d) is an optical micrograph of Example 4-4.
  • 4 is a graph showing measurement results of hardness HV1 at a temperature between room temperature and 900 ° C. of Examples 4-1 to 4-3.
  • 6 is a graph showing room temperature hardness HV1 of samples 5-1 to 5-6 (sintered bodies).
  • FIG. 42 is an optical micrograph showing the metal structure after sintering of the hard particle-dispersed nickel-based intermetallic compound composite sintered material according to Example 6, and FIG. 42 (a) is an optical micrograph of Example 6-1; FIG. 42B is an optical micrograph of Example 6-2. It is a graph which shows the hardness HV1 measurement result in the temperature between room temperature and 900 degreeC of Example 6-1.
  • a nickel-base intermetallic material including a double-phase structure comprising a primary phase containing a base intermetallic compound and a eutectoid phase containing a first nickel-based intermetallic compound and a second nickel-based intermetallic compound It has been found that a compound composite sintered material can be obtained.
  • a composite material having a target nickel-based two-phase structure can be obtained without obtaining a cast material having a target composition (composition of the entire material to be obtained). I found out that I can get it with a near net shape.
  • the inventors of the present invention have obtained a nickel-based intermetallic compound composite sintered material containing a double-phase structure obtained by such a sintering method as compared with a melted material having a similar double-phase structure. It has been found that uniform double-phase structure grains can be obtained by suppressing the grain coarsening that can easily occur in the molten metal, for example, the diameter is remarkably small, for example, 50 ⁇ m or less. This will be described below as a first embodiment.
  • the inventors of the present application added at least one selected from carbides, nitrides, carbonitrides, oxides, and borides when performing the sintering under the above-described pressure, whereby two overlapping phases are obtained. It has been found that a high-strength composite material in which the structure and these carbides, nitrides, carbonitrides, oxides and / or borides are combined can be obtained. This will be described below as a second embodiment.
  • Embodiments 1 and 2 of the present invention a nickel-based intermetallic compound composite sintered material having a dual-phase structure and a manufacturing method thereof will be described in detail. Before that, some terms used in the present specification are described. Let me clarify the meaning of.
  • two-duplex phase structure is a structure including a pro-eutectoid phase and a eutectoid phase, wherein the pro-eutectoid phase includes a first intermetallic compound, and the eutectoid phase is the first eutectoid phase.
  • FIG. 37 illustrates a transmission electron microscope observation result of the double-duplex structure
  • FIG. 37 (a) shows a transmission electron microscope (TEM) image of the double-duplex structure
  • 37 (c) shows another electron microscope image of the double-duplex structure, showing a limited-field electron diffraction image obtained from the circled region in 37 (a).
  • the two-phase structure is formed between the pro-eutectoid phase 1 and the pro-eutectoid phase 1 having a quadrangular shape in the transmission electron microscope image, as shown in FIGS. 37 (a) and 37 (c).
  • the eutectoid phase 3 is formed so as to fill the gap (hereinafter also referred to as “channel portion”).
  • the identification of the first intermetallic compound and the second intermetallic compound may be performed using various known methods including X-ray diffraction and electron diffraction. From electron diffraction image shown in FIG. 37 (b), co-eutectoid 3 shown in FIG. 37 is found to consist of the intermetallic compound Ni 3 V having intermetallic compound Ni 3 Al and D0 22 type crystal structure Yes. Further, first eutectoid 1 shown in FIG. 37 by performing electron diffraction in the same manner is found to consist of intermetallic compound Ni 3 Al having an L1 2 type crystal structure. In eutectoid phase 3, Ni 3 V has a lamellar structure (variant structure) formed in a layered manner, and depending on the observation conditions, the lamellar state is as shown in FIG. 37 (c). May be observable.
  • the first intermetallic compound is Ni 3 Al (including a case where a part thereof is substituted by another element), and the second intermetallic compound is Ni 3. V (including the case where a part is replaced by another element).
  • nickel group means that the amount of nickel is the largest among the respective elements contained, and preferably contains Ni of 50% or more in atomic ratio (at%), more preferably Ni in an atomic ratio (at%) is 60% or more.
  • nickel-based intermetallic compound composite sintered material means a sintered material containing an intermetallic compound, and in the composition of the whole sintered material, The nickel content is the largest, and preferably contains 50% or more Ni by atomic ratio (at%), more preferably 60% or more Ni by atomic ratio (at%).
  • nickel-based intermetallic compound means an intermetallic compound having the largest amount of nickel among the contained elements, and preferably contains Ni of 50% or more in atomic ratio (at%), More preferably, it contains 60% or more of Ni by atomic ratio (at%).
  • average crystal grain size used in the present specification means an average crystal grain size measured by a section method from a structure photograph or the like. Specific examples of the measurement by the intercept method will be shown in Examples described later.
  • Embodiment 1 Powder for sintering (1) Form of sintering powder
  • the powder for sintering which has is produced.
  • the powder for sintering may be a mixed powder obtained by mixing element powders such as nickel powder, aluminum powder, vanadium powder, niobium powder, tantalum powder and boron powder as raw material powders.
  • These raw material powders may contain alloy powders in which a single powder contains two or more elements as long as the composition thereof is within a predetermined range according to the present invention.
  • the alloy powder obtained by atomizing the molten metal (molten alloy) which has a predetermined composition may be sufficient. Further, it may be a mixed powder obtained by mixing element powder and alloy powder.
  • atomized powder is preferable. This is because by using the atomized powder, a two-phase structure can be obtained more reliably, and the hardness of the obtained composite material can be increased to a level equivalent to that of the melted material.
  • a preferable condition for producing the atomized powder is that a molten metal melted at 1400 to 1800 ° C. in an inert gas atmosphere is dropped, and an inert gas is sprayed thereto at a pressure of 30 to 100 kg / cm 2 .
  • the particle diameter of the powder for sintering may have arbitrary particle diameters.
  • any method used in the technical field such as a mortar and pestle may be used, but the mixing is preferably performed using a ball mill. This is because the ball mill can disperse and mix the raw material powder more uniformly.
  • a ball mill a planetary ball mill is used, balls are arranged so as to have a ratio of balls 10 to 50 with respect to the powder 1 in terms of mass ratio, and mixed in a dry manner.
  • the ball mill is preferably carried out in an inert gas atmosphere such as nitrogen gas or argon gas. This is because the powder can be prevented from oxidizing during mixing. Moreover, it may replace with dry type and may perform wet mixing using liquid media, such as alcohol.
  • composition of the powder for sintering is a proeutectoid containing the first nickel-based intermetallic compound by heat treatment appropriately performed as necessary after sintering or after sintering described in detail later.
  • the composition may have any composition capable of forming a double-phase structure comprising a phase and a eutectoid phase including a first nickel-based intermetallic compound and a second nickel-based intermetallic compound.
  • the first nickel-based intermetallic compound is Ni 3 Al
  • the second nickel-based intermetallic compound Ni 3 V
  • the proeutectoid phase is Ni 3 Al.
  • intermetallic compounds Ni 3 Al and Ni 3 V are Ni 3 Al intermetallic compounds containing elements other than nickel and aluminum, such as substitutional elements and interstitial elements, respectively, and other than nickel and vanadium.
  • the sintered body according to the present invention having two overlapping phase structure comprising a Ni 3 Al and Ni 3 V may include a phase other than Ni 3 Al and Ni 3 V.
  • a phase include at least one of Ni 3 Nb and Ni 3 Ta having a crystal structure of D0 a .
  • the double-phase structure according to the present invention is not limited to the double-phase structure including Ni 3 Al and Ni 3 V.
  • the sintering powder is composed of 5 at% to 13 at% aluminum (Al), 9.5 at% It is preferable that vanadium (V) in an amount of 1 to 17.5 at% and niobium Nb in an amount of 0 to 5 at% are contained. In this case, the balance may be nickel and inevitable impurities, and may contain other components as long as nickel is contained at 50 at% or more.
  • One or more elements selected from can be exemplified.
  • Ta 0.5 at% to 8 at%
  • W 0.5 at% to 8 at%
  • Cr 12 at (not including 0 at%)
  • Co 15 at %: Not including 0 at%
  • Ti 0.5 at% to 3.5 at%
  • Re 0.5 at% to 5 at%
  • C 12.5 at% or less (not including 0 at%)
  • One or more selected may be contained.
  • FIG. 1 is a Ni 3 Al—Ni 3 Nb—Ni 3 V suspicious ternary phase diagram at 1100 ° C. (1373 K)
  • FIG. 2 is an Nb amount of 2.5 at% of the ternary phase diagram shown in FIG. FIG.
  • the horizontal axis indicates the Al content (at%)
  • the vertical axis indicates the temperature (K). Since Nb is contained at 2.5 at%, the V content represented by at% can be obtained by the following equation (1).
  • V content (at%) 22.5-Al content (at%) (1)
  • Ni 3 Al has an L1 2 structure
  • Ni 3 V has an A1 structure
  • Ni 3 Nb has a D0 a structure.
  • the A1 structure is a solid solution having an fcc structure having no regular structure.
  • Niobium has the effect of improving strength. This effect tends to increase with an increase in the amount of niobium up to 5 at%. However, when the niobium amount exceeds 5 at%, this effect is saturated, and in addition to the L1 2 phase and the D0 22 phase in the two- duplex structure. Since an intermetallic compound phase such as a Ni 3 Nb phase may be coarsened and appear more, the niobium content is preferably 5 at% or less (including the case where it is not contained).
  • tantalum Ti
  • B boron
  • W tungsten
  • Cr chromium
  • Co cobalt
  • Ti titanium
  • Re rhenium
  • carbon carbon
  • Tantalum is an element effective for solid solution strengthening (hardening). The effect is limited when the tantalum content is less than 0.5 at%, and when it exceeds 8 at%, the effect of improving the hardness is saturated, and a metal such as Ni 3 Ta is contained in the two-phase structure. There may be a problem that more intermetallic phases appear. Accordingly, the tantalum content is preferably 0.5 at% to 8 at%.
  • Tungsten has the effect of improving hardness.
  • the effect is limited when the tungsten content is less than 0.5 at%, and when it exceeds 8 at%, it is considered that the effect of improving the hardness may be saturated. Accordingly, the content of tungsten is preferably 0.5 at% to 8 at%.
  • Chrome has the effect of improving oxidation resistance and reducing weight. The effect becomes more pronounced as the chromium content increases up to 12 at%. However, when the chromium content exceeds 12 at%, the effect becomes saturated, and the appearance (stabilization) of the nickel solid solution phase occurs, resulting in a decrease in strength. In some cases, the chromium content is preferably 12 at% or less (not including 0 at%).
  • Cobalt has the effect of improving oxidation resistance. The effect becomes more pronounced as the cobalt content increases until the cobalt content is 15 at%, but saturates when the cobalt content exceeds 15 at%. Furthermore, since it is considered that the nickel solid solution phase may appear, the cobalt content is preferably 15 at% or less (not including 0 at%).
  • Boron has an effect of suppressing grain boundary destruction.
  • the effect is limited if it is less than 10 ppm by weight with respect to the total mass of elements other than boron (total content indicated by mass), and if it exceeds 1000 ppm with respect to the total mass of elements other than boron, boron compounds ( Boride) may be formed to cause embrittlement.
  • Titanium has an effect of improving strength. In particular, it is considered that the effect of strengthening the Ni 3 Al (L1 2 ) phase is great. This effect becomes significant when the titanium content is 0.5 at% or more. On the other hand, if it exceeds 3.5 at%, the effect is considered to be saturated. On the other hand, if it exceeds 3.5 at%, coarse Ni 3 Ti may be formed to deteriorate the strength and ductility.
  • Rhenium has the effect of precipitating and hardening the two-duplex phase structure.
  • a dual-phase structure containing Ni 3 Al and Ni 3 V with rhenium added is aged at an appropriate temperature, precipitates with a rhenium-rich composition appear in the channel and the hardness increases remarkably. .
  • This effect is prominent when the rhenium content is 0.5 at% or more, and tends to be saturated when it exceeds 5 at%. Since rhenium is an expensive element, it is not economical to add more than 5 at% where the effect is saturated.
  • the two-phase structure is strengthened by solid solution, and the ductility at high temperatures is greatly improved.
  • the carbon content is large, it is dispersed as a carbide such as VC (vanadium carbide) in the two-layered structure, which contributes to an increase in strength and ductility. If the content is more than 12.5 at%, the carbide may be coarsened and toughness may be reduced.
  • sintering is performed using a sintering powder having a desired composition.
  • Sintering is, for example, a general sintering method in which a powder for sintering is placed in a die and pressure is applied with a punch to obtain a molded body (a green compact) and then heated to a predetermined sintering temperature. May be performed.
  • the sintered body obtained by sintering can have an average crystal grain size of 50 ⁇ m or less, which is one digit or more smaller than that of the melted material. And by making the crystal grains fine and uniform in this way, mechanical properties such as strength, ductility, toughness, etc. of the double phase structure can be greatly improved.
  • a double-duplex structure can be obtained at a lower temperature. For this reason, a shape (near net shape) close to the final product can be obtained.
  • a sintered body having the shape of the final product or a shape close to this (near net shape) can be easily obtained by using the sintering method. That is, a sintered body can be manufactured with high dimensional accuracy.
  • pressure sintering it is preferable to sinter while applying pressure to the sintering powder (pressure sintering). This is because the density of the obtained sintered body can be increased and closer to the density of the molten material.
  • applying pressure to the sintering powder means that when sintering is performed after obtaining the compact, pressure is applied to the sintering powder in the compact by applying pressure to the compact. Including being done.
  • a preferred example of such a method of sintering while applying pressure to the sintering powder is a hot press.
  • hot pressing include hot isostatic pressing (HIP treatment) or gas pressure sintering after vacuum sintering.
  • the pressure sintering by the hot press method may be performed as follows. For example, a lower punch is inserted from below into a through-hole extending in a vertical direction provided in a die made of graphite, and the above-mentioned sintering powder or powder containing the above-mentioned sintering powder is formed inside the through-hole and above the lower punch Place. Thereafter, an upper punch is inserted from above the through hole, and stress is applied to the upper punch and the lower punch so that a predetermined pressure is applied to the sintering powder. Then, in a state where a predetermined pressure is applied to the sintering powder, the sintering powder is heated and sintered, for example, by heating a die.
  • the sintering powder or powder containing the sintering powder instead of placing the sintering powder or powder containing the sintering powder inside the die through-hole and on the upper part of the lower punch, it is produced using the sintering powder or powder containing the sintering powder. You may arrange the formed object.
  • Sintering conditions such as the sintering temperature, the heating rate, the sintering time, the stress for pressing the sintering powder (or compact), the sintering atmosphere, etc. when using the hot press method are the composition of the sintering powder used. What is necessary is just to adjust suitably according to the characteristic of the composite sintered material to obtain.
  • illustrating preferred conditions for obtaining the 2 multi-phase structure comprising a Ni 3 Al and Ni 3 V.
  • the sintering temperature is preferably 1000 ° C. to 1300 ° C. This is because a dual-phase structure can be obtained within this temperature range. More preferably, the sintering temperature is 1250 ° C to 1280 ° C. This is because a two-duplex phase structure can be obtained more reliably. In addition, by setting the sintering temperature to 1250 to 1280 ° C., the average crystal grain size of the obtained sintered body can be reliably reduced to, for example, 40 ⁇ m or less, and therefore, a high-strength and high-toughness double-phase structure. Can be definitely obtained.
  • the heating rate when heating up to the sintering temperature is preferably 10 ° C./min or less. This is because if the temperature rising rate is too high, the temperature distribution becomes non-uniform and there may be a difference in the characteristics of the sintered body.
  • the holding time at the above-mentioned preferable sintering temperature is preferably 60 minutes to 360 minutes. This is because if the holding time is too short, the densification may be insufficient, and if it is too long, the crystal grains may become coarse and the characteristics may deteriorate (or deteriorate).
  • the stress applied to the sintering powder (or molded body) is preferably 10 MPa to 60 MPa. This is because if the stress is too low, densification may be insufficient, and if it is too high, the carbon mold may be destroyed.
  • the sintering is preferably performed in a vacuum or in a reduced-pressure atmosphere of an inert gas such as argon, nitrogen and helium. This is because the powder may be oxidized in an atmosphere containing oxygen, and densification may be inhibited.
  • Heat treatment In the composite sintered material (sintered body) produced in this way, depending on the sintering conditions, a double-duplex structure is formed only in a part of the sintered body, and other parts are other than the double-duplex structure. May be an organization. Heat treatment may be performed so that at least a part of such a portion has a double-duplex structure. It is preferable to perform a heat treatment that is higher than the sintering temperature and does not produce a liquid phase and is heated to a temperature of 1320 ° C. or lower, preferably 1300 ° C. or lower.
  • the heat treatment temperature is selected to be lower than the melting temperature at the time of producing the molten material (cast material), so that it is possible to obtain a two-phase structure at a lower temperature.
  • the effect of this application that it is possible is acquired.
  • the heat treatment temperature is preferably 1250 ° C. to 1280 ° C. This is because when the heat treatment is performed in this temperature range, the nickel solid solution single-phase region is heated, and in the subsequent cooling process, a dual-phase structure containing Ni 3 Al and Ni 3 V can be obtained more reliably. It is preferable to hold at this heat treatment temperature for 0.5 to 24 hours.
  • the heat treatment is preferably performed in a vacuum or in an inert gas atmosphere such as argon.
  • the nickel-based intermetallic compound composite sintered material containing a double-phase structure according to the present invention can have an average crystal grain size as fine as, for example, 50 ⁇ m or less, and thus can have a uniform structure.
  • the nickel-based intermetallic compound composite sintered material according to the present embodiment is substantially composed entirely of a two-duplex structure.
  • a nickel base intermetallic compound composite sintered material containing a double phase structure can be obtained at a lower temperature. It becomes possible. Therefore, a shape close to the final product can be obtained more easily.
  • Embodiment 2 a nickel-based metal in which a double-phase structure and particles containing one or more selected from carbides, nitrides, and carbonitrides (hereinafter sometimes referred to as “hard particles”) are combined.
  • the intermetallic compound sintered material and the manufacturing method thereof will be described.
  • the composite sintered material according to the second embodiment one or more selected from carbides, nitrides, and carbonitrides contained in the hard particles exist in addition to the two-phase structure shown in the first embodiment.
  • this composite material may be referred to as “hard particle-dispersed nickel-based intermetallic compound composite sintered material”.
  • the hard particle-dispersed nickel-based intermetallic compound composite sintered material preferably one or more (or hard particles) selected from carbides, nitrides, carbonitrides, oxides and borides contained in the hard particles. Evenly distributed. In the conventional melt casting method, it was difficult to uniformly disperse the hard particles in the metal / alloy. However, in the present invention, since the sintering method is used as will be described in detail later, it is a matrix. It has the effect that hard particles can be uniformly dispersed in the two-phase structure.
  • the hard particle-dispersed nickel-based intermetallic compound composite sintered material has higher strength (hardness) due to the presence of carbides, nitrides and carbonitrides contained in the hard particles in addition to the dual phase structure.
  • Have Hard particle-dispersed nickel-based intermetallic compound composite sintered material has a higher high-temperature strength (hardness) in applications where a cemented carbide alloy such as tungsten carbide cobalt (WC-Co) has been used. It is possible to provide an alloy having Examples of such applications include hot extrusion dies and hot forging tools.
  • hard particle-dispersed nickel-based intermetallic compound composite sintered materials are more suitable for applications where tool materials and heat-resistant materials such as die steel, WC-Co cemented carbide, and Inconel have been used. It becomes possible to have high oxidation resistance and corrosion resistance.
  • Such applications include hot extrusion dies, hot drawing tools, hot forging dies, hot rolls and guide rollers, hot bending mandrels, friction stir welding tools, lens molding, etc. Examples of mold peripheral parts can be given.
  • hard particles are particles containing at least one selected from carbide, nitride, carbonitride, oxide or boride. .
  • Preferred hard particles are Group 4A (group 4) elements (titanium (Ti), zirconium (Zr), hafnium (Hf)), group 5A (group 5) elements (vanadium (V), niobium (Nb), Carbides, nitrides, carbonitrides, oxides of one or more elements selected from tantalum (Ta)) and group 6A (group 6) elements (chromium (Cr), molybdenum (Mo), tungsten (W)) Or a boride is included.
  • the hard particles may be aluminum (Al) or yttrium (Y) carbides, nitrides, carbonitrides, oxides or borides.
  • the hard particle is a group 4A (group 4) element (titanium (Ti), zirconium (Zr), hafnium (Hf)) of the periodic table, group 5A (group 5) element (vanadium (V), niobium). (Nb), tantalum (Ta)) and group 6A (group 6) elements (chromium (Cr), molybdenum (Mo), tungsten (W)), carbides, nitrides, and charcoal of one or more elements selected from Nitride, oxide, or boride is a main component (mass ratio of 50% or more).
  • the hard particles may contain aluminum (Al) or yttrium (Y) carbide, nitride, carbonitride, oxide or boride as a main component (50% or more by mass ratio).
  • hard particles examples include TiC particles, TiCN particles, TiN particles, TaC particles, and WC particles.
  • yttria Y 2 O 3 , alumina Al 2 O 3 and tria ThO 2 can be exemplified as oxides other than the above, and MB 2 and MB 6 (M is a metal element) as borides.
  • nitrides, carbonitrides, oxides and borides, carbides, nitrides, and carbides can be supplied from the viewpoint of being able to supply interstitial elements carbon or nitrogen from the hard particles to the double-phase structure of the matrix.
  • Carbonitride is more preferred.
  • the particle size of the hard particles is preferably 0.5 to 10 ⁇ m.
  • the powder size may be measured by various methods, and a method using a Fischer sub-sieve sizer can be exemplified as one of the measuring methods.
  • the above-mentioned hard particles and sintering powder are mixed to obtain a hard particle-containing sintering powder.
  • various methods used for mixing powders may be used.
  • the powder for sintering is a mixed powder in which elemental powder is mixed
  • hard particles are added to produce the mixed powder, mixed powder and hard
  • the particles may be mixed simultaneously.
  • the mixed powder and hard particles may be put in a bag and mixed by, for example, vibrating the bag.
  • the sintering powder is an alloy powder such as an atomized powder
  • the alloy powder and hard particles in a bag or mortar, and mix by vibrating the bag or mortar, for example. Then, a hard particle-containing sintering powder may be obtained.
  • the mixing ratio between the hard particles and the sintering powder may be adjusted in accordance with the characteristics of the hard particle-dispersed nickel-based intermetallic compound composite sintered material to be obtained.
  • the hard particles are 10 to 90% by volume with respect to the hard particle-containing sintering powder (that is, the total of the hard particles and the sintering powder).
  • the hardness value of the obtained hard particle-dispersed nickel-based intermetallic compound composite sintered material tends to increase.
  • a base material for obtaining the composition of the powder for sintering and hard particles are mixed in advance, and this mixture is, for example, 2000 ° C.
  • the base material may be melted by heating as described above and atomized to obtain an atomized powder containing hard particles therein, which may be used as a hard particle-containing sintering powder.
  • the hard particles may be partially or wholly melted.
  • the base material may be in any form such as an alloy ingot, a pure metal ingot corresponding to each component (that is, a plurality of types of ingots), an alloy powder, a mixed powder, and the like.
  • Sintering may be performed by the same method as in the first embodiment. That is, in the sintering method shown in the first embodiment, the sintering can be performed by replacing the sintering powder with the hard particle-containing sintering powder. Other sintering conditions may be the same as those in the first embodiment.
  • Heat treatment In the obtained hard particle-dispersed nickel-based intermetallic compound composite sintered material (sintered body), so that at least a part of the portion other than the double-phase structure (excluding hard particles) has a double-phase structure, Heat treatment may be performed in the same manner as in the first embodiment.
  • the conditions for the heat treatment may be the same as those in the first embodiment.
  • Example 1 1-1 Nickel-based intermetallic compound composite sintered material (1) Preparation of mixed powder Using the element powder having the powder size (particle diameter) shown in Table 1, mixed powder (sintering powder) having the composition shown in Table 2 was prepared. Produced. In addition, about boron (B), it showed by the ratio (weight ppm) with respect to the total mass of elements other than boron. As shown in Table 3, mixing was performed using a mortar and pestle for the sample of Example 1-1, and using a planetary ball mill for the samples of Example 1-2 and Example 1-3. The mixing by the planetary ball mill was performed by a dry method, and 2300 g of balls were used for 50 g of powder.
  • the powder size was measured using a Fischer sub-sieve sizer for Ni and a mesh for others.
  • FIG. 3 is a scanning electron microscope (SEM) image of the obtained mixed powder
  • FIG. 3A is an SEM image of Example 1-1
  • FIG. 3B is an SEM image of Example 1-2
  • FIG. 3C is an SEM image of Example 1-3.
  • the mixed powders of Examples 1-2 and 1-3 obtained by the ball mill aggregate and have a particle size larger than that of the mixed powder of Example 1-1.
  • FIG. 4 is an optical micrograph showing the metal structure of the obtained dispersed nickel-based intermetallic compound composite sintered material
  • FIG. 4 (a) is an optical micrograph of Example 1-1
  • 4B is an optical micrograph of Example 1-2
  • FIG. 4C is an optical micrograph of Example 1-3
  • FIG. 38 is an SEM image showing the metal structure of the obtained dispersed nickel-based intermetallic compound composite sintered material
  • FIG. 38 (a) is an SEM image of Example 1-1
  • FIG. 38 (b) 2 is a higher magnification SEM image of Example 1-1. From the results of FIGS. 4 and 38, it can be seen that a sufficiently dense structure can be obtained even in the sample of Example 1-1 in which the mortar was mixed.
  • FIG. 5 shows the X-ray diffraction results
  • FIG. 5 (a) shows the X-ray diffraction results of Example 1-1
  • FIG. 5 (b) shows the X-ray diffraction results of Example 1-2
  • FIG. (C) shows the X-ray diffraction results of Example 1-3.
  • the peak positions of Ni 3 Al and Ni 3 V are shown at the bottom of FIG. From the X-ray diffraction results of FIG. 5, it was confirmed that Ni 3 Al and Ni 3 V were present in each of Examples 1-1 to 1-3 due to the formation of a double-phase structure.
  • Table 4 shows the measurement results of the oxygen content, nitrogen content, density and room temperature hardness of the nickel-based intermetallic compound composite sintered material obtained.
  • the oxygen content was measured by an infrared absorption method.
  • the nitrogen content was measured by a heat conduction method.
  • the density was determined by the following method. Each sample was wet-polished to # 1500 with water-resistant emery paper, the dry weight, the weight in water and the water content were measured using a suspended electronic balance, and the bulk density was calculated by the Archimedes method. For comparison, the density measurement was performed in the same manner for the ingots having the same composition.
  • the density (bulk density) was calculated using the following formula (2).
  • ⁇ b W 1 ⁇ 1 / (W 2 ⁇ W ′) (2)
  • ⁇ b is a density (bulk density)
  • W 1 is a dry weight
  • W 2 is a hydrous weight
  • W ′ is a weight in water.
  • Hardness was determined by the following method. Each sample was wet-polished to # 1500 with water-resistant emery paper and then buffed with alumina powder. Thereafter, a micro Vickers hardness test was performed using the polished sample. Measurement was performed at 12 points for each sample, and the average value of 10 measurement values excluding the maximum value and the minimum value was calculated to be the hardness.
  • the measurement conditions of the micro Vickers hardness meter were a load of 1 kg and a holding time of 20 seconds.
  • FIG. 6 is a graph showing the hardness HV1 measurement result of the obtained sample at a temperature between room temperature and 900 ° C.
  • Any sample of Examples 1-1 to 1-3 exhibits a sufficiently high high-temperature hardness, for example, 400 HV1 or higher at 400 ° C., thereby having high strength and wear resistance at high temperatures. I understand. Further, up to 600 ° C., the samples of Examples 1-2 and 1-3 in which the mixed powder was obtained by a ball mill were higher in hardness than the samples obtained by using the mortar / breast.
  • Hard particle-dispersed nickel-based intermetallic compound composite sintered material (1) Preparation of powder for sintering containing hard particles Next, the raw material powder shown in Table 1 was prepared to have the composition shown in Table 2, and this raw material powder After adding TiC particles having an average particle size of 1.5 ⁇ m as hard particles (powder size is measured by a Fischer sub-sieve sizer) to a content of 8 to 80% by volume as shown in Table 5, A powder for sintering containing hard particles was produced by a ball mill. The ball mill conditions were the same as in Example 1-2 above.
  • FIG. 7 is a scanning electron microscope (SEM) image of a sintering powder (mixed powder) containing hard particles
  • FIG. 7A is an SEM image of Example 1-4
  • FIG. 7 is an SEM image of Example 1-5
  • FIG. 7C is an SEM image of Example 1-6
  • FIG. 7D is an SEM image of Example 1-7
  • FIG. ) Is an SEM image of Example 1-8.
  • SEM scanning electron microscope
  • Example 1-6 the sintered sample was subjected to a heat treatment.
  • the heat treatment conditions were maintained at 1280 ° C. in a vacuum for 3 hours.
  • FIG. 8 is an optical micrograph showing the metal structure of the hard particle-dispersed nickel-based intermetallic compound composite sintered material
  • FIG. 8 (a) is an optical micrograph of Example 1-4
  • FIG. 8 (b) is an optical micrograph of Example 1-5
  • FIG. 8 (c) is an optical micrograph of Example 1-6
  • FIG. 8 (d) is an optical microscope of Example 1-7
  • FIG. 8 (e) is an optical micrograph of Example 1-8. From the optical microscope observation result of FIG. 8, it can be seen that the dark gray TiC particles are uniformly dispersed.
  • FIG. 9 is an SEM image showing the metal structure of the hard particle-dispersed nickel-based intermetallic compound composite sintered material according to Example 1-6
  • FIG. 9A is an SEM image of the sample after sintering
  • 9 (b) is an SEM image of the sample after sintering at a high magnification
  • FIG. 9 (c) is an SEM image of the sample after the heat treatment
  • FIG. 9 (d) is an SEM image of the sample after the heat treatment at a high magnification. It is. From FIG. 9, it can be confirmed that the dark gray TiC particles are uniformly dispersed, and a two-duplex structure is formed in the light gray portion therebetween. In addition, it can be seen that the sample after the heat treatment has a coarsened double-duplex structure formed on the entire surface as compared with the sample after sintering.
  • FIG. 10 shows the X-ray diffraction (CuK ⁇ ) result
  • FIG. 10 (a) shows again the X-ray diffraction result of Example 1-2 not containing TiC
  • FIG. 10 (b) shows the X-ray diffraction result of Example 1-4
  • FIG. 10C shows the X-ray diffraction results of Example 1-5
  • FIG. 10D shows the X-ray diffraction results of Example 1-6
  • FIG. The X-ray diffraction result of Example 1-7 is shown, and FIG.
  • FIG. 10 (f) shows the X-ray diffraction result of Example 1-8.
  • peak positions of TiC, Ni 3 Al, and Ni 3 V are shown in the lower part of FIG.
  • FIG. 11 shows the X-ray diffraction (CuK ⁇ ) result of the hard particle-dispersed nickel-based intermetallic compound composite sintered material according to Sample 1-6 in more detail
  • FIG. 11 (a) shows the X-ray diffraction result after sintering.
  • FIG. 11B shows the X-ray diffraction result after the heat treatment.
  • FIG. 12 shows the hardness HV1 measurement results at temperatures between room temperature and 900 ° C. of the hard particle-dispersed nickel-based intermetallic compound composite sintered materials of Examples 1-6 and 1-8. It is a graph to show. The results of Example 1-2 are also shown for comparison. The samples of Examples 1-6 and 1-8 with the addition of hard particle TiC had a higher hardness than Example 1-2 without the addition of hard particle TiC at any temperature, and more, It turns out that it is excellent in high temperature hardness and abrasion resistance at high temperature. Further, comparing Example 1-6 with Example 1-8, Example 1-8 to which more hard particles TiC were added at all temperatures has higher hardness.
  • Example 2 2-1 Nickel-based intermetallic compound composite sintered material (1) Preparation of mixed powder Using an element powder having a powder size (particle diameter) shown in Table 7, a mixed powder (sintering powder) having the composition shown in Table 8 was prepared. Produced. As shown in Table 9, mixing was performed using a mortar and pestle in the sample of Example 2-1, and using a planetary ball mill in the sample of Example 2-2. The mixing by the planetary ball mill was performed by a dry method, and 2300 g of balls were used for 50 g of powder.
  • the powder size was measured using a Fischer sub-sieve sizer for Ni and a mesh for others.
  • FIG. 13 is an SEM image showing a sintered metal structure of the obtained nickel-based intermetallic compound composite sintered material
  • FIG. 13A is an SEM image of Example 2-1
  • FIG. 13B is an SEM image at a high magnification of Example 2-1
  • FIG. 13C is an SEM image of Example 2-2
  • FIG. 13D is Example 2.
  • 2 is a SEM image at a high magnification of -2. From FIG. 13, it can be seen that a sufficiently dense structure can be obtained even in the sample of Example 2-1 which was mixed with the mortar. Further, in the sample of Example 2-2 subjected to ball mill mixing, it was observed that the homogeneity and uniformity were improved.
  • FIG. 14 is an SEM image showing the metal structure after heat treatment of the obtained nickel-based intermetallic compound composite sintered material.
  • FIG. 14A is an SEM image of Example 2-1, and FIG. ) Is an SEM image of Example 2-1 at high magnification
  • FIG. 14C is an SEM image of Example 2-2
  • FIG. 14D is high magnification of Example 2-2. It is a SEM image of.
  • FIG. 14 shows that the heat-treated material has a clearer two-phase structure.
  • FIG. 15 shows the X-ray diffraction result of Example 2-1
  • FIG. 15 (a) shows the X-ray diffraction result after sintering
  • FIG. 15 (b) shows the X-ray diffraction result after heat treatment
  • 16 shows the X-ray diffraction results of Example 2-2
  • FIG. 16 (a) shows the X-ray diffraction results after sintering
  • FIG. 16 (b) shows the X-ray diffraction results after heat treatment. From the X-ray diffraction results of FIGS. 15 and 16, it was confirmed that Ni 3 Al and Ni 3 V were present in both Examples 2-1 and 2-2 due to the formation of a double-duplex structure.
  • FIG. 17 is an example of a pattern quality map obtained by crystal orientation analysis.
  • FIG. 17 (a) shows an example of Example 2-1
  • FIG. 17 (b) shows an example of Example 2-2.
  • the average particle size obtained was 19 ⁇ m for the sample of Example 2-1 and 2 ⁇ m for the sample of Example 2-2.
  • Hardness test result Hardness was measured by the same method as in Example 1.
  • FIG. 18 shows the hardness HV1 after sintering and heat treatment of Examples 2-1 and 2-2.
  • Example 2-1 has an average value of HV1 of about 500 both after sintering and after heat treatment
  • Example 2-2 has an average value of HV1 of about 600 both after annealing and after heat treatment. Both samples have sufficient strength. (Hardness).
  • Example 2-2 Hard particle-dispersed nickel-based intermetallic compound composite sintered material (1) Preparation of sintering powder containing hard particles Next, the raw material powder shown in Table 7 was prepared to have the composition shown in Table 8, and this raw material powder After adding TiC particles having an average particle size of 1.5 ⁇ m as hard particles (powder size is measured by a Fischer sub-sieve sizer) to a content of 30% by volume, in Example 2-3, a mortar and A powder for sintering containing hard particles was produced with a pestle and with a ball mill in Example 2-4. The conditions for mixing with a mortar and pestle were the same as in Example 2-1, and the conditions for mixing with a ball mill were the same as in Example 2-2.
  • FIG. 19 is an SEM image showing the metal structure after sintering of the obtained hard particle-dispersed nickel-based intermetallic compound composite sintered material
  • FIG. 19B is an SEM image at a high magnification of Example 2-3
  • FIG. 19C is an SEM image of Example 2-4
  • FIG. 19D is an SEM image. It is a SEM image at a high magnification of Example 2-4. From FIG. 19, it can be seen that the dark gray TiC phase is uniformly dispersed, and the light gray phase therebetween has a double-layered structure.
  • FIG. 20 is an SEM image showing a metal structure after heat treatment of the obtained hard particle-dispersed nickel-based intermetallic compound composite sintered material, and FIG.
  • FIG. 20 (a) is an SEM image of Example 2-3.
  • 20 (b) is an SEM image at a high magnification of Example 2-3
  • FIG. 20 (c) is an SEM image of Example 2-4
  • FIG. 20 (d) is an example of Example 2-4. It is a SEM image in high magnification. From FIG. 20, it is observed that the dark gray TiC phase is dispersed in any sample. Moreover, it turns out that dispersion
  • FIG. 21 shows the X-ray diffraction results of Example 2-3
  • FIG. 21 (a) shows the X-ray diffraction results after sintering
  • FIG. 21 (b) shows the X-ray diffraction results after heat treatment
  • 22 shows the X-ray diffraction results of Example 2-4
  • FIG. 22 (a) shows the X-ray diffraction results after sintering
  • FIG. 22 (b) shows the X-ray diffraction results after heat treatment. From the X-ray diffraction results of FIGS.
  • FIG. 23 shows the hardness HV1 after sintering and heat treatment of Examples 2-3 and 2-4.
  • the average value of HV1 after annealing is about 700
  • the average value of HV1 after heat treatment is about 650
  • the average value of HV1 after heat treatment is about 770
  • the average value of HV1 after heat treatment is about 750, and it can be seen that both samples have sufficient hardness.
  • it has higher hardness than Examples 2-1 and 2-2 to which no hard particle TiC is added, and it can be seen that the addition of hard particles further increases the strength (hardness). .
  • Example 3 In this example, atomized powder was used to obtain a nickel-based intermetallic compound composite sintered material and a hard particle-dispersed nickel-based intermetallic compound composite sintered material.
  • Nickel-based intermetallic compound composite sintered material (1) Preparation of atomized powder An atomized powder (alloy powder) having the composition shown in Table 10 was obtained. In Table 10, boron (B) is shown as a ratio (weight ppm) to the total mass of other elements. The atomized powder was prepared by melting and dropping an ingot of each element having a predetermined composition at 1600 ° C. in an argon gas atmosphere, and blowing argon gas at a pressure of 50 kg / cm 2 there.
  • FIG. 24 is an SEM image of atomized powder
  • FIG. 24 (a) shows the atomized powder of Example 3-1
  • FIG. 24 (b) shows the atomized powder of Example 3-2
  • FIG. ) Shows the atomized powder of Example 3-3.
  • FIG. 25 is a graph showing the particle size distribution measurement results of the atomized powder.
  • FIG. 25 (a) shows the atomized powder of Example 3-1
  • FIG. 25 (b) shows the atomized powder of Example 3-2
  • FIG. 25 (c) shows the atomized powder of Example 3-3.
  • the particle size distribution was measured by the mesh method.
  • FIG. 26 shows the X-ray diffraction (CuK ⁇ ) results of the atomized powder.
  • FIG. 26 (a) shows the X-ray diffraction results of Example 3-1
  • FIG. 26 (b) shows the X-ray diffraction results of Example 3-2
  • FIG. 26 (c) shows the results of Example 3-3.
  • X-ray diffraction results are shown.
  • the peak positions of Ni 3 Al and Ni 3 V are shown at the bottom of FIG.
  • Example 3-1A a sample sintered at a sintering temperature of 1250 ° C., for example, as in “Example 3-1A”
  • Example 3- a sample sintered at a sintering temperature of 1280 ° C.
  • FIG. 27 is an optical micrograph showing the metal structure of the nickel-based intermetallic compound composite sintered material
  • FIG. 27A is an optical micrograph of Example 3-1A
  • b) is an optical micrograph of Example 3-1B
  • FIG. 27 (c) is an optical micrograph of Example 3-2A
  • FIG. 27 (d) is an optical micrograph of Example 3-2B
  • FIG. 27 (e) is an optical micrograph of Example 3-3A
  • FIG. 27 (f) is an optical micrograph of Example 3-3B.
  • FIG. 28 shows SEM images of Example 3-2A and Example 3-2B
  • FIG. 28A shows an SEM image of Example 3-2A
  • FIG. 28B shows Example 3-2A
  • FIG. 28C is an SEM image of Example 3-2B
  • FIG. 28D is an SEM image of Example 3-2B at a high magnification.
  • FIG. 29 shows SEM images of Example 3-3A and Example 3-3B
  • FIG. 29A shows an SEM image of Example 3-3A
  • FIG. 29B shows Example 3-3A
  • FIG. 29C is an SEM image of Example 3-3B
  • FIG. 29D is an SEM image of Example 3-3B at a high magnification.
  • Example 3-2A and 3-2B a double-phase structure was observed in the entire sample in the state after sintering.
  • Example 3-3A an intermetallic compound phase other than needle-like or plate-like Ni 3 Al or Ni 3 V appears in the entire double-phase structure.
  • Example 3-3B such Ni No intermetallic compound phase other than 3 Al and Ni 3 V has appeared, and the entire sample has a double-phase structure.
  • the sintering temperature is preferably 1280 ° C.
  • FIG. 30 shows the X-ray diffraction results
  • FIG. 30 (a) shows the X-ray diffraction results of Example 3-1A
  • FIG. 30 (b) shows the X-ray diffraction results of Example 3-2A
  • FIG. (C) shows the X-ray diffraction result of Example 3-3A.
  • the lower part of FIG. 30 shows the peak positions of Ni 3 Al and Ni 3 V. From the X-ray diffraction results of FIG.
  • Table 11 shows the measurement results of the density and room temperature hardness of the nickel-based intermetallic compound composite sintered materials of Examples 3-1A to 3-3B obtained. The same methods as in Examples 1-1 to 1-3 were used for measuring the density and hardness.
  • Table 11 shows that sufficient density and hardness were obtained in any of the example samples. However, in Example 3-3A, the formation of the double-phase structure was a part, or the hardness was slightly higher. It became low. It can be seen that an appropriate sintering temperature is 1280 ° C.
  • FIG. 31 (a) is a graph showing the hardness HV1 measurement results of Examples 3-1A, 3-2A and 3-3A at a temperature between room temperature and 900 ° C.
  • FIG. 31 (b) is a graph showing the results of measurement of hardness HV1 at temperatures between room temperature and 900 ° C. in Examples 3-1B, 3-2B, and 3-3B.
  • Each sample exhibits a sufficiently high high temperature hardness such as 400 HV1 (according to the indication of JIS (JIS-R1610)) at 400 ° C., and thus has high strength and wear resistance at high temperatures. I understand that.
  • Hard particle-dispersed nickel-based intermetallic compound composite sintered material (1) Preparation of sintering powder containing hard particles In the atomized powder of Example 3-2, an average particle size of 1.5 ⁇ m (the method of measuring the powder size is 50% by volume of TiC (based on a Fischer sub-sieve sizer) (fine TiC) was mixed to prepare a sintering powder containing hard particles according to Example 3-4. Similarly, 30% by volume of TiC (coarse TiC) having an average particle size of 50 ⁇ m (the method of measuring the powder size is based on mesh) is mixed with the atomized powder of Example 3-2, and Example 3-5 is used. A sintering powder containing hard particles was prepared.
  • NbC fine NbC having an average particle diameter of 2 ⁇ m (the method for measuring the powder size is by Fisher sub-sieving) is mixed with the atomized powder of Example 3-2, and Example 3-6 is performed.
  • a powder for sintering containing hard particles was prepared.
  • the hardened particles according to Example 3-7 were mixed with the atomized powder of Example 3-2 with 30% by volume of WC powder having an average particle size of 1.5 ⁇ m (the method of measuring the powder size is by using a Fisher sub-sieve sizer). The powder for sintering containing this was produced.
  • the hardened particles according to Example 3-8 were mixed with 30% by volume of TaC powder having an average particle size of 2.0 ⁇ m (the method for measuring the powder size is by using a Fisher sub-sieve sizer) to the atomized powder of Example 3-2.
  • the powder for sintering containing this was produced.
  • sintering was performed by a hot press method, and hard particle-dispersed nickel-based intermetallic compound composite sintering was performed.
  • a material (sintered body) was obtained.
  • the sintering conditions were the same as in Examples 1-1 to 1-3 for Examples 3-4 to 3-6, that is, the sintering temperature was 1250 ° C.
  • the sintering temperature was 1280 ° C.
  • the other sintering conditions were the same as those in Examples 3-4 to 3-6.
  • FIG. 32 is an optical micrograph showing the metal structure of the hard particle-dispersed nickel-based intermetallic compound composite sintered material according to Examples 3-4 to 3-6.
  • FIG. 32B is an optical micrograph of Example 3-4
  • FIG. 32B is an optical micrograph of Example 3-5
  • FIG. 32C is an optical micrograph of Example 3-6.
  • FIG. 33 is an SEM image showing the metal structure of the obtained hard particle-dispersed nickel-based intermetallic compound composite sintered material according to Examples 3-4 and 3-6.
  • FIG. 33 (b) is a higher magnification SEM image of Example 3-4
  • FIG. 33 (c) is an SEM image of Example 3-6
  • FIG. 33 (d) These are higher magnification SEM images of Example 3-6.
  • FIG. 34 is an SEM image showing the metal structure of the obtained hard particle-dispersed nickel-based intermetallic compound composite sintered material according to Examples 3-7 and 3-8.
  • FIG. 34 (a) shows Example 3- Fig. 34 (b) is a higher magnification SEM image of Example 3-7, Fig. 34 (c) is an SEM image of Example 3-8, and Fig. 34 (d) is a SEM image of Example 3-7. These are higher magnification SEM images of Example 3-8.
  • FIG. 35 shows the hardness HV1 measurement results at temperatures between room temperature and 900 ° C. of the hard particle-dispersed nickel-based intermetallic compound composite sintered materials of Examples 3-4 to 3-6. It is a graph to show. From FIG. 35, the hardness at room temperature is increased by dispersing hard particles. Moreover, it turns out that the fall of the hardness accompanying a temperature rise is low, and this seems to be based on the feature of a nickel base intermetallic compound. As the particle size of the hard particles, it can be seen that the fine particles are more effective in improving the hardness. As for the influence of the type of hard particles, fine TiC and NbC have almost the same hardness at room temperature, but higher hardness can be obtained by using fine TiC at 200 ° C to 600 ° C. understood.
  • FIG. 36 is a graph showing the measurement results of the hardness HV1 at room temperature of the hard particle-dispersed nickel-based intermetallic compound composite sintered materials of Examples 3-7 and 3-8. From FIG. 36, it can be seen that both WC and TaC can increase the hardness by dispersion hardening, and TaC has a greater increase in hardness.
  • the invention of the present application includes a first eutectoid phase containing a first nickel-based intermetallic compound, a co-polymer containing a first nickel-based intermetallic compound and a second nickel-based intermetallic compound.
  • a nickel-based intermetallic compound composite sintered material having a double-phase structure comprising the deposited phase, and the obtained double-phase structure being uniform and having high strength (hardness), and powder It is clear to provide a method by which a nickel-based intermetallic compound composite sintered material can be manufactured with better dimensional accuracy (near net shape) by using a forming method. Furthermore, it is clear that the nickel-based intermetallic compound composite sintered material according to the present invention has even higher strength (hardness) by using hard particles.
  • Example 4 vanadium carbide (VC) and tungsten carbide (WC) were used as the hard particles.
  • VC vanadium carbide
  • WC tungsten carbide
  • (1) Preparation of sintering powder containing hard particles As in Example 2, the raw material powder shown in Table 7 was prepared to have the composition shown in Table 8, and the average particle diameter 1 was used as hard particles in this raw material powder.
  • Example 4-1 VC particles were added to a content of 30% by volume, and in Example 4-2, VC particles were added to a content of 50% by volume.
  • Example 4-3 VC particles were added to a content of 70% by volume, and in Example 4-4, WC particles were added to a content of 50% by volume.
  • a sintering powder containing hard particles was prepared using a mortar and pestle.
  • FIG. 39 is an optical micrograph showing the metal structure of the obtained hard particle-dispersed nickel-based intermetallic compound composite sintered material according to Example 4, and FIG. 39 (b) is an optical micrograph of Example 4-2, FIG. 39 (c) is an optical micrograph of Example 4-3, and FIG. 39 (d) is an optical micrograph of FIG. 4 is an optical micrograph of Example 4-4.
  • 39 (a) to 39 (c) it can be seen that the dark gray VC phase is uniformly dispersed, and the light gray phase therebetween has a double-duplex structure. It can also be seen that the amount of the VC phase increases as the volume fraction of the VC particles increases. From FIG. 39 (d), it can be seen that the dark gray WC phase is uniformly dispersed, and the light gray phase therebetween has a double-layered structure.
  • Hardness test results Hardness at room temperature was measured by the same method as in Example 1. Table 12 shows the results of the hardness test of the samples of Examples 4-1 to 4-4 (after heat treatment). It can be seen that any sample of Examples 4-1 to 4-4 has sufficient hardness. Further, from Examples 4-1 to 4-3, it can be seen that the room temperature hardness HV1 greatly increases from 658 to 1237 as the volume fraction of VC particles increases from 30% to 70%.
  • FIG. 40 is a graph showing the hardness HV1 measurement results of the samples of Examples 4-1 to 4-3 at a temperature between room temperature and 900 ° C.
  • any sample for example, any sample shows a sufficiently high high-temperature hardness, such as 400 HV1 (according to JIS (JIS-R1610) indication) or higher at 600 ° C. It can be seen that it has wear resistance.
  • Example 5 titanium carbide (TiC), titanium carbonitride (TiCN), titanium nitride (TiN), tantalum carbide (TaC) and tungsten carbide (WC) were used as hard particles.
  • the atomized powder of Example 3-3 was mixed with 30% by volume of TiN having an average particle size of 2.0 ⁇ m (the method of measuring the powder size is based on a mesh), and the sintered powder containing hard particles according to Example 5-3 was mixed.
  • a powder for ligation was prepared.
  • the atomized powder of Example 3-3 was mixed with 30% by volume of TaC having an average particle size of 2.0 ⁇ m (the method for measuring the powder size is based on a mesh), and the sintered powder containing hard particles according to Example 5-4 was mixed.
  • a powder for ligation was prepared.
  • the atomized powder of Example 3-3 was mixed with 15% by volume of WC having an average particle size of 1.5 ⁇ m (the method of measuring the powder size is based on a mesh), and the sintered powder containing hard particles according to Example 5-5 was mixed.
  • a powder for ligation was prepared.
  • the atomized powder of Example 3-3 was mixed with 60% by volume of WC having an average particle size of 6.0 ⁇ m (the method for measuring the powder size is based on a mesh), and the sintered powder containing hard particles according to Example 5-6 was mixed.
  • a powder for ligation was prepared.
  • FIG. 41 is a graph showing the room temperature hardness HV1 of the samples (sintered bodies) of Examples 5-1 to 5-6. It can be seen that the samples of Examples 5-1 to 5-6 have a high room temperature hardness HV1 of 629 to 789.
  • Example 6 in addition to atomizing the hard particles, the particles were melted to obtain atomized powder, and the atomized powder was used to obtain a hard particle-dispersed nickel-based intermetallic compound composite sintered material.
  • FIG. 42 is an optical micrograph showing the metal structure after sintering of the obtained hard particle-dispersed nickel-based intermetallic compound composite sintered material
  • FIG. FIG. 42B is an optical micrograph of Example 6-1
  • FIG. 42B is an optical micrograph of Example 6-2. 42 (a) and 42 (b), it can be seen that the dark gray TiC phase is uniformly dispersed, and the light gray phase therebetween has a double-duplex structure.
  • Example 6-1 The room temperature hardness of the sample (sintered body) of Example 6-1 was 523 HV1, and the room temperature hardness of the sample (sintered body) of Example 6-2 was 551HV1.
  • FIG. 43 is a graph showing the hardness HV1 measurement results of the sample of Example 6-1 at a temperature between room temperature and 900 ° C.
  • the high temperature hardness such as 400 HV1 (according to JIS (JIS-R1610) display) or higher at 400 ° C., and it can be seen that it has high strength and wear resistance at high temperatures.

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Abstract

L'invention concerne : un matériau qui présente une structure double-phase composée d'une phase primaire comprenant un premier composé intermétallique à base de nickel et d'une phase proeutectoïde comprenant le premier composé intermétallique à base de nickel et un deuxième composé intermétallique à base de nickel, et qui présente une excellente résistance ; et un procédé de production du matériau à une température inférieure. Un matériau fritté composite de composés intermétalliques à base de nickel, qui comprend une structure double-phase composée d'une phase primaire comprenant un premier composé intermétallique à base de nickel et d'une phase proeutectoïde comprenant le premier composé intermétallique à base de nickel et un deuxième composé intermétallique à base de nickel différent du premier composé intermétallique à base de nickel, le matériau étant caractérisé en ce que la structure double-phase présente un diamètre moyen de particules cristallines de 50 µm ou moins, est décrit. Le matériau peut être produit par un procédé métallurgique à base de poudres.
PCT/JP2012/076998 2011-10-19 2012-10-18 Matériau fritté composite de composés intermétalliques à base de nickel et procédé pour sa production WO2013058338A1 (fr)

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JP2015063752A (ja) * 2013-08-27 2015-04-09 公立大学法人大阪府立大学 Ｎｉ基金属間化合物合金の溶射皮膜、溶射皮膜被覆部材および溶射皮膜の製造方法
JP2016160495A (ja) * 2015-03-03 2016-09-05 本田技研工業株式会社 Ｍｏ添加Ｎｉ基金属間化合物合金及びその製造方法
JP6128671B1 (ja) * 2017-02-02 2017-05-17 ハイテン工業株式会社 熱間鍛造用金型、熱間鍛造装置、及び熱間鍛造用金型の製造方法
JP2018135585A (ja) * 2017-02-23 2018-08-30 公立大学法人大阪府立大学 金属部材及びクラッド層の製造方法
JP2020056106A (ja) * 2018-09-27 2020-04-09 株式会社アテクト ニッケル基合金製または鉄基合金製の耐熱部材の製造方法
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JP6128671B1 (ja) * 2017-02-02 2017-05-17 ハイテン工業株式会社 熱間鍛造用金型、熱間鍛造装置、及び熱間鍛造用金型の製造方法
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