WO2022085161A1 - ダイヤモンド焼結体、及びダイヤモンド焼結体を備える工具 - Google Patents
ダイヤモンド焼結体、及びダイヤモンド焼結体を備える工具 Download PDFInfo
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- WO2022085161A1 WO2022085161A1 PCT/JP2020/039755 JP2020039755W WO2022085161A1 WO 2022085161 A1 WO2022085161 A1 WO 2022085161A1 JP 2020039755 W JP2020039755 W JP 2020039755W WO 2022085161 A1 WO2022085161 A1 WO 2022085161A1
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- WIPO (PCT)
- Prior art keywords
- sintered body
- diamond
- group
- diamond sintered
- diamond particles
- Prior art date
Links
- 239000010432 diamond Substances 0.000 title claims abstract description 224
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 223
- 239000002245 particle Substances 0.000 claims abstract description 118
- 229910052751 metal Inorganic materials 0.000 claims description 23
- 239000002184 metal Substances 0.000 claims description 23
- 150000001875 compounds Chemical class 0.000 claims description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 16
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 15
- 229910017052 cobalt Inorganic materials 0.000 claims description 14
- 239000010941 cobalt Substances 0.000 claims description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 13
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 239000000956 alloy Substances 0.000 claims description 7
- 229910045601 alloy Inorganic materials 0.000 claims description 7
- 229910021480 group 4 element Inorganic materials 0.000 claims description 7
- 229910021478 group 5 element Inorganic materials 0.000 claims description 7
- 229910021476 group 6 element Inorganic materials 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 229910052755 nonmetal Inorganic materials 0.000 claims description 7
- 230000000737 periodic effect Effects 0.000 claims description 7
- 239000006104 solid solution Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052796 boron Inorganic materials 0.000 claims description 6
- 150000002739 metals Chemical class 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 description 86
- 239000000843 powder Substances 0.000 description 34
- 238000012360 testing method Methods 0.000 description 30
- 238000000034 method Methods 0.000 description 28
- 239000002994 raw material Substances 0.000 description 23
- 238000005245 sintering Methods 0.000 description 23
- 238000005259 measurement Methods 0.000 description 22
- 239000011812 mixed powder Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 9
- 238000002156 mixing Methods 0.000 description 8
- 238000005096 rolling process Methods 0.000 description 8
- 239000010955 niobium Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 238000000691 measurement method Methods 0.000 description 5
- 238000003801 milling Methods 0.000 description 5
- 229910052758 niobium Inorganic materials 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 229910052715 tantalum Inorganic materials 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 5
- 229910052721 tungsten Inorganic materials 0.000 description 5
- 239000010937 tungsten Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 239000011651 chromium Substances 0.000 description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 4
- 230000005469 synchrotron radiation Effects 0.000 description 4
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000002775 capsule Substances 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000002826 coolant Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 229910052735 hafnium Inorganic materials 0.000 description 3
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910000765 intermetallic Inorganic materials 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000000550 scanning electron microscopy energy dispersive X-ray spectroscopy Methods 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000003776 cleavage reaction Methods 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 238000010884 ion-beam technique Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000003870 refractory metal Substances 0.000 description 2
- 230000007017 scission Effects 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 102100031051 Cysteine and glycine-rich protein 1 Human genes 0.000 description 1
- 101000922020 Homo sapiens Cysteine and glycine-rich protein 1 Proteins 0.000 description 1
- 101001019104 Homo sapiens Mediator of RNA polymerase II transcription subunit 14 Proteins 0.000 description 1
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000009412 basement excavation Methods 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000001226 reprecipitation Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/12—Metallic powder containing non-metallic particles
-
- 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
-
- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
- B23B27/14—Cutting tools of which the bits or tips or cutting inserts are of special material
- B23B27/148—Composition of the cutting inserts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
- B23B27/14—Cutting tools of which the bits or tips or cutting inserts are of special material
- B23B27/18—Cutting tools of which the bits or tips or cutting inserts are of special material with cutting bits or tips or cutting inserts rigidly mounted, e.g. by brazing
- B23B27/20—Cutting tools of which the bits or tips or cutting inserts are of special material with cutting bits or tips or cutting inserts rigidly mounted, e.g. by brazing with diamond bits or cutting inserts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
- C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
-
- 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
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- 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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F2005/001—Cutting tools, earth boring or grinding tool other than table ware
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B2226/00—Materials of tools or workpieces not comprising a metal
- B23B2226/31—Diamond
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/60—Compounds characterised by their crystallite size
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/427—Diamond
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
- C04B2235/786—Micrometer sized grains, i.e. from 1 to 100 micron
Definitions
- the present disclosure relates to a diamond sintered body and a tool including the diamond sintered body.
- the diamond sintered body has excellent hardness and does not have directional hardness and cleavage, it is widely used for tools such as cutting tools, dressers and dies, and excavation bits.
- diamond powder which is a raw material, is used together with a sintering aid or a binder at a high pressure and high temperature (generally, a pressure of about 5 to 8 GPa and a temperature at which diamond is thermodynamically stable). It is obtained by sintering under the condition of (about 1300 to 2200 ° C.).
- a sintering aid iron group element metals such as Fe, Co and Ni, and carbonates such as CaCO 3 are used.
- the binder ceramics such as SiC are used.
- Patent Document 1 Japanese Patent Application Laid-Open No. 2005-239472
- Patent Document 1 describes a high-strength, high-wear-resistant diamond sintered body having sintered diamond particles having an average particle size of 2 ⁇ m or less and the remaining bonded phase.
- the content of the sintered diamond particles in the diamond sintered body is 80% by volume or more and 98% by volume or less, and the content in the bonded phase is 0.5% by mass or more and less than 50% by mass.
- Part or all of at least one element selected from the group consisting of titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, and molybdenum, including the bonded phase with cobalt, has an average particle size of 0.8 ⁇ m.
- a high-strength, high-wear-resistant diamond sintered body which exists as the following carbide particles, the structure of the carbide particles is discontinuous, and the adjacent diamond particles are bonded to each other. Has been done.
- Patent Document 1 describes a method for manufacturing the high-strength, high-wear-resistant diamond sintered body, which uses a belt-type ultra-high pressure device, has a pressure of 5.7 GPa or more and 7.5 GPa or less, and a temperature of 1400 ° C. or more and 1900.
- a method for producing a high-strength, high-wear-resistant diamond sintered body, which is characterized by sintering under conditions of ° C. or lower, is disclosed.
- the diamond sintered body of the present disclosure is A diamond sintered body containing diamond particles.
- the content of the diamond particles is 80% by volume or more and 99% by volume or less with respect to the diamond sintered body.
- the average particle size of the diamond particles is 0.1 ⁇ m or more and 50 ⁇ m or less.
- the dislocation density of the diamond particles is 1.2 ⁇ 10 16 m -2 or more and 5.4 ⁇ 10 19 m -2 or less.
- the tool of the present disclosure includes the above-mentioned diamond sintered body.
- the present disclosure has been made in view of the above circumstances, and an object of the present disclosure is to provide a diamond sintered body having excellent crack resistance and a tool provided with the diamond sintered body.
- the diamond sintered body according to one aspect of the present disclosure is A diamond sintered body containing diamond particles.
- the content of the diamond particles is 80% by volume or more and 99% by volume or less with respect to the diamond sintered body.
- the average particle size of the diamond particles is 0.1 ⁇ m or more and 50 ⁇ m or less.
- the dislocation density of the diamond particles is 1.2 ⁇ 10 16 m -2 or more and 5.4 ⁇ 10 19 m -2 or less.
- the diamond sintered body has excellent crack resistance.
- crack growth resistance means resistance to the growth of cracks generated in the diamond sintered body during cutting when it receives an external force.
- the dislocation density of the diamond particles is preferably 1.5 ⁇ 10 16 m ⁇ 2 or more and 1.0 ⁇ 10 17 m ⁇ 2 or less.
- the diamond sintered body further contains a bonded phase
- the diamond sintered body further contains a bonded phase.
- the binding phase is Elemental metals, alloys, and intermetal compounds containing at least one metal element selected from the group consisting of Group 4 elements, Group 5 elements, Group 6 elements, iron, aluminum, silicon, cobalt, and nickel in the periodic table. At least one selected from the group consisting of, or It consists of at least one metal element selected from the group consisting of Group 4 elements, Group 5 elements, Group 6 elements, iron, aluminum, silicon, cobalt and nickel in the periodic table, and nitrogen, carbon, boron and oxygen.
- the bonded phase preferably contains cobalt.
- the tool according to one aspect of the present disclosure includes the above diamond sintered body.
- fracture resistance means resistance to chipping of a tool during machining of a material.
- Impact resistance means resistance to momentary forces applied from the outside during processing of a material.
- the present disclosure is not limited to these examples.
- the notation in the form of "A to Z" means the upper and lower limits of the range (that is, A or more and Z or less), and there is no description of the unit in A, and the unit is described only in Z. In the case, the unit of A and the unit of Z are the same.
- the diamond sintered body according to this embodiment is A diamond sintered body containing diamond particles.
- the content of the diamond particles is 80% by volume or more and 99% by volume or less with respect to the diamond sintered body.
- the average particle size of the diamond particles is 0.1 ⁇ m or more and 50 ⁇ m or less.
- the dislocation density of the diamond particles is 1.2 ⁇ 10 16 m -2 or more and 5.4 ⁇ 10 19 m -2 or less.
- the diamond sintered body contains diamond particles. That is, the diamond sintered body has a basic composition of diamond as particles. In one aspect of the present embodiment, diamond particles can also be grasped as diamond crystal grains. It is preferable that the diamond sintered body further contains a bonding phase (binder) formed by one or both of the sintering aid and the binder. The diamond particles and the bonded phase will be described later.
- the diamond sintered body is a polycrystal composed of a plurality of diamond particles. Therefore, the diamond sintered body does not have directional (anisotropic) and cleavage properties like a single crystal, and has isotropic hardness and crack resistance in all directions.
- the diamond sintered body may contain unavoidable impurities as long as the effect of the present embodiment is exhibited.
- unavoidable impurities include hydrogen, oxygen and the like.
- the content of the diamond particles is preferably 80% by volume or more and 99% by volume or less, and preferably 80% by volume or more and 90% by volume or less with respect to the diamond sintered body.
- the content of diamond particles (% by volume) and the content of bonded phase (% by volume) described later in the diamond sintered body are determined by scanning electron microscope (SEM) (“JSM-7800F” (trade name) manufactured by JEOL Ltd.). Using the incidental energy dispersive X-ray analyzer (EDX) (Octane Electro EDS system) (hereinafter also referred to as "SEM-EDX”), microstructure observation, element analysis, etc. are performed on the diamond sintered body. Can be confirmed by implementing.
- SEM scanning electron microscope
- EDX incidental energy dispersive X-ray analyzer
- microstructure observation, element analysis, etc. are performed on the diamond sintered body. Can be confirmed by implementing.
- the specific measurement method is as follows.
- the diamond sintered body First, cut an arbitrary position of the diamond sintered body to prepare a sample containing a cross section of the diamond sintered body.
- a focused ion beam device, a cross-section polisher device, or the like can be used to prepare the cross section.
- the cross section is observed by SEM to obtain a backscattered electron image.
- the region where the diamond particles are present is the black region
- the region where the bonded phase is present is the gray region or the white region.
- the magnification when observing the cross section by SEM is appropriately adjusted so that the number of diamond particles observed in the measurement field of view is 100 or more.
- the magnification when observing the cross section by SEM may be 10000 times.
- the magnification when observing the cross section by SEM may be 200 times.
- the reflected electron image is binarized using image analysis software (Mitani Shoji Co., Ltd.'s "WinROOF ver. 7.4.5", “WinROOF2018”, etc.).
- the above image analysis software automatically sets an appropriate binarization threshold value based on the image information (the measurer does not arbitrarily set the threshold value).
- the inventors have confirmed that there is no significant change in the measurement result even when the brightness of the image is changed.
- the area ratio of the pixels derived from the dark field (pixels derived from the diamond particles) to the area of the measurement field is calculated. By considering the calculated area ratio as% by volume, the content rate (volume%) of diamond particles can be obtained.
- Obtaining the content rate (volume%) of the coupled phase by calculating the area ratio of the pixels derived from the bright visual field (pixels derived from the coupled phase) to the area of the measured visual field from the image after the binarization process. Can be done.
- the fact that the pixels derived from the dark field are derived from the diamond particles can be confirmed by performing elemental analysis on the diamond sintered body by SEM-EDX.
- the average particle size of the diamond particles is 0.1 ⁇ m or more and 50 ⁇ m or less, and preferably 0.2 ⁇ m or more and 40 ⁇ m or less.
- the average particle size of the diamond particles is 0.1 ⁇ m or more, the diamond particles are densely sintered, and a diamond sintered body having excellent fracture resistance is obtained. Since the average particle size of the diamond particles is 50 ⁇ m or less, the diamond sintered body has no anisotropy and has excellent cutting stability when used as a cutting tool of a cutting tool.
- the average particle size of the diamond particles is obtained by measuring the median diameter d50 of a plurality of diamond particles in each of five arbitrarily selected measurement fields and calculating the average value thereof. Means the value given.
- the specific method is as follows.
- the diamond sintered body First, cut an arbitrary position of the diamond sintered body to prepare a sample containing a cross section of the diamond sintered body.
- a focused ion beam device, a cross-section polisher device, or the like can be used to prepare the cross section.
- the cross section is observed by SEM to obtain a backscattered electron image.
- the region where the diamond particles are present is the black region
- the region where the bonded phase is present is the gray region or the white region.
- the magnification when observing the cross section by SEM is appropriately adjusted so that the number of diamond particles observed in the measurement field of view is 100 or more.
- the magnification when observing the cross section by SEM may be 10000 times.
- the magnification when observing the cross section by SEM may be 200 times.
- the median diameter d50 in each measurement field of view is calculated, and the average value thereof is calculated.
- the average value corresponds to the average particle size of diamond particles.
- the present inventor shows that there is almost no variation in the measurement results even if the selection points of the measurement field of the diamond sintered body are changed and the calculation is performed a plurality of times. Have confirmed. That is, the present inventors think that it is not arbitrary even if the measurement field of view is arbitrarily set.
- the dislocation density of the diamond particles is 1.2 ⁇ 10 16 m -2 or more and 5.4 ⁇ 10 19 m -2 or less, and 1.5 ⁇ 10 16 m -2 or more and 1.0 ⁇ 10 17 m -2 .
- the following is preferable.
- the dislocation density of the diamond particles is 1.2 ⁇ 10 16 m -2 or more, a relatively large number of immobile dislocations are present, so that crack growth generated in the diamond particles is suppressed, and diamond firing with excellent crack growth resistance is achieved. It becomes a unit.
- the dislocation density of the diamond particles is 5.4 ⁇ 10 19 mph or less, the occurrence of cracks in the diamond particles is suppressed, and the diamond sintered body having excellent impact resistance is obtained.
- the present inventors diligently investigated the relationship between the dislocation density of diamond particles in a diamond sintered body and the crack growth resistance of the diamond sintered body.
- the conventional diamond sintered body for example, the diamond sintered body described in Patent Document 1
- the dislocation density of the diamond sintered body is measured at a large synchrotron radiation facility (for example, Kyushu Synchrotron Radiation Research Center (Saga Prefecture)). Specifically, it is measured by the following method.
- test piece made of a diamond sintered body.
- the size of the test piece is 3 mm ⁇ 6 mm on the observation surface and 0.4 mm in thickness.
- the observation surface of the test piece is mirror-polished with a diamond slurry having an average particle size of 3 ⁇ m, and then immersed in hydrochloric acid for 72 hours. As a result, the bound phase is dissolved in hydrochloric acid on the observation surface of the test piece, and diamond particles remain.
- X-ray diffraction measurement was performed on the test piece under the following conditions, and the main orientations of diamond (111), (220), (311), (331), (422), (440), (531). Obtain the line profile of the diffraction peak from each azimuth plane of.
- X-ray diffraction measurement conditions X-ray source: Synchrotron radiation Device condition: Detector NaI (cuts fluorescence by appropriate ROI) Energy: 18 keV (wavelength: 0.6888 ⁇ ) Spectral crystal: Si (111) Incident slit: width 3 mm x height 0.5 mm Light receiving slit: Double slit (width 3 mm x height 0.5 mm) Mirror: Platinum coated mirror Incident angle: 2.5mrad Scanning method: 2 ⁇ - ⁇ scan Measurement peaks: 7 diamonds (111), (220), (311), (331), (422), (440), (531). However, if it is difficult to obtain a profile due to texture, orientation, etc., the peak of the surface index is excluded.
- Measurement conditions Make sure that the number of measurement points is 9 or more within the full width at half maximum corresponding to each measurement peak.
- the peak top intensity shall be 2000 counts or more. Since the tail of the peak is also used for analysis, the measurement range is about 10 times the full width at half maximum.
- the line profile obtained by the above-mentioned X-ray diffraction measurement has a shape including both true spread due to physical quantities such as non-uniform strain of the test piece and spread due to the device.
- the instrument-derived components are removed from the measured line profile to obtain a true line profile.
- the true line profile is obtained by fitting the obtained line profile and the device-derived line profile by a pseudo Voigt function and subtracting the device-derived line profile.
- LaB 6 is used as a standard sample for removing the diffraction line spread caused by the device. Further, when synchrotron radiation having high parallelism is used, the diffraction line spread caused by the device can be regarded as 0.
- the dislocation density is calculated by analyzing the obtained true line profile using the modified Williamson-Hall method and the modified Warren-Averbach method.
- the modified Williamson-Hall method and the modified Warren-Averbach method are known line profile analysis methods used to determine the dislocation density.
- ⁇ K indicates the half width of the line profile.
- D indicates the crystallite size.
- M indicates an arrangement parameter.
- b represents a Burgers vector.
- ⁇ indicates the dislocation density.
- K indicates a scattering vector.
- O (K 2 C) indicates a higher-order term of K 2 C.
- C indicates the average value of the contrast factor.
- C in the above formula (I) is represented by the following formula (II).
- C C h00 [1-q (h 2 k 2 + h 2 l 2 + k 2 l 2 ) / (h 2 + k 2 + l 2 ) 2 ] (II)
- the contrast factor Ch00 and the coefficient q related to the contrast factor in the spiral dislocation and the blade dislocation are calculated code ANIZC, the slip system is ⁇ 110> ⁇ 111 ⁇ , and the elastic stiffness C 11 is 1076 GPa. , C 12 is 125 GPa, and C 44 is 576 GPa.
- h, k and l correspond to the Miller index (hkl) of diamond, respectively.
- the contrast factor C h00 is a spiral dislocation 0.183 and a blade dislocation 0.204.
- the coefficients q with respect to the contrast factor are spiral dislocations 1.35 and blade dislocations 0.30.
- the spiral dislocation ratio is fixed at 0.5 and the blade dislocation ratio is fixed at 0.5.
- a (L) represents a Fourier series.
- AS (L) indicates a Fourier series with respect to crystallite size.
- L indicates the Fourier length.
- the present inventors have confirmed that as long as the dislocation density of diamond particles is measured in the same sample, there is almost no variation in the measurement results even if the measurement range is changed and the calculation is performed multiple times. That is, the present inventors think that it is not arbitrary even if the measurement field of view is arbitrarily set.
- the diamond sintered body further contains a bonded phase.
- the binding phase is At least one metal element selected from the group consisting of Group 4 elements, Group 5 elements, Group 6 elements, iron, aluminum, silicon, cobalt and nickel (hereinafter, also referred to as "Group A") in the periodic table. At least one selected from the group consisting of single metals, alloys, and intermetallic compounds, including At least one metal element selected from the group (Group A) consisting of Group 4 elements, Group 5 elements, Group 6 elements, iron, aluminum, silicon, cobalt and nickel in the periodic table, and nitrogen, carbon and boron.
- group B a compound consisting of at least one non-metal element selected from the group consisting of oxygen (hereinafter, also referred to as "group B"), and at least one selected from the group consisting of a solid solution derived from the above compound.
- group B a compound consisting of at least one non-metal element selected from the group consisting of oxygen
- group B at least one selected from the group consisting of a solid solution derived from the above compound.
- the bonded phase is composed of at least one selected from the group consisting of elemental metals containing at least one metal element selected from group A, alloys, and intermetallic compounds.
- the bonded phase contains at least one selected from the group consisting of elemental metals, alloys, and intermetallic compounds containing at least one metal element selected from group A.
- the bonded phase is selected from the group consisting of a compound consisting of at least one metal element selected from group A, at least one non-metal element selected from group B, and a solid solution derived from the compound. Consists of at least one species.
- the bonded phase is selected from the group consisting of a compound consisting of at least one metal element selected from group A, at least one non-metal element selected from group B, and a solid solution derived from the compound. Includes at least one species.
- the bonded phase is at least one selected from the group consisting of a single metal, an alloy, and an intermetal compound containing at least one metal element selected from group A, and at least one selected from group A. It is composed of a compound composed of the metal element of the above, at least one non-metal element selected from the group B, and at least one selected from the group consisting of a solid solution derived from the above compound.
- the bonded phase is at least one selected from the group consisting of a single metal, an alloy, and an intermetal compound containing at least one metal element selected from group A, and at least one selected from group A.
- Group 4 elements of the periodic table include, for example, titanium (Ti), zirconium (Zr) and hafnium (Hf).
- Group 5 elements include, for example, vanadium (V), niobium (Nb) and tantalum (Ta).
- Group 6 elements include, for example, chromium (Cr), molybdenum (Mo) and tungsten (W).
- the bonded phase preferably contains at least one selected from the group consisting of cobalt, titanium, iron, tungsten and boron, and more preferably contains cobalt.
- composition of the bonded phase contained in the diamond sintered body can be specified by the above-mentioned EDX incidental to SEM.
- the content of the bonded phase is preferably 1% by volume or more and 20% by volume or less, and more preferably 10% by volume or more and 20% by volume or less with respect to the diamond sintered body.
- the content of the bonded phase (% by volume) can be confirmed by performing microstructure observation, elemental analysis, etc. on the diamond sintered body using the above-mentioned SEM-attached EDX.
- the diamond sintered body of the present embodiment has excellent crack growth resistance, it can be suitably used for cutting tools, abrasion resistant tools, grinding tools, friction stirring joining tools and the like. That is, the tool of the present embodiment includes the above-mentioned diamond sintered body.
- the above-mentioned tool has excellent chipping resistance and excellent impact resistance in processing various materials.
- the cutting tool is particularly suitable for turning and turning aluminum alloys (for example, ADC12, AC4B) and the like.
- the above tool may be entirely composed of a diamond sintered body, or only a part thereof (for example, in the case of a cutting tool, a cutting edge portion) may be composed of a diamond sintered body.
- Cutting tools include drills, end mills, replaceable cutting tips for drills, replaceable cutting tips for end mills, replaceable cutting tips for milling, replaceable cutting tips for turning, metal saws, gear cutting tools, and reamers. , Taps, cutting tools, etc.
- wear-resistant tools examples include dies, scribers, scribed wheels, dressers, and the like.
- Examples of the grinding tool include a grinding wheel and the like.
- the method for manufacturing a diamond sintered body according to the present embodiment is as follows.
- a raw material powder for diamond particles (hereinafter, also referred to as “diamond powder”) and a raw material powder for a bonded phase (hereinafter, also referred to as “bonded phase raw material powder”) are prepared.
- the diamond powder is not particularly limited, and known diamond particles can be used as the raw material powder.
- the average particle size of the diamond powder is not particularly limited, and can be, for example, 0.1 ⁇ m or more and 50 ⁇ m or less.
- the bonded phase raw material powder is not particularly limited, and may be any powder containing elements constituting the bonded phase.
- Examples of the bonded phase raw material powder include cobalt powder and titanium powder.
- As the bound phase raw material powder one kind of powder may be used alone or a plurality of kinds of powders may be used in combination depending on the composition of the desired bound phase.
- the raw material powder of the diamond particles (diamond powder) and the raw material powder of the bonded phase (bonded phase raw material powder) are mixed to obtain a mixed powder.
- the diamond powder and the bonded phase raw material powder may be mixed at an arbitrary blending ratio so that the content of diamond particles in the diamond sintered body is within the above range.
- the method of mixing both powders is not particularly limited, and may be a mixing method using an attritor or a mixing method using a ball mill.
- the mixing method may be wet or dry.
- Step of forming dislocations in diamond particles the mixed powder is heated at a holding pressure of 4 GPa or more and 7 GPa or less, a holding temperature of 30 ° C. or more and 600 ° C. or less, and a holding time of 50 minutes or more and 190 minutes or less to generate dislocations in the diamond particles. do.
- the route from the state of normal temperature (23 ⁇ 5 ° C.) and atmospheric pressure to the state of the holding pressure and the holding temperature is not particularly limited.
- the high-pressure and high-temperature generator used in the method for manufacturing a diamond sintered body of the present embodiment is not particularly limited as long as it can obtain the desired pressure and temperature conditions.
- the high-pressure and high-temperature generator is preferably a belt-type high-pressure and high-temperature generator.
- the container for storing the mixed powder is not particularly limited as long as it is a high-pressure and high-temperature resistant material, and for example, tantalum (Ta), niobium (Nb) and the like are preferably used.
- the mixed powder is first placed in a capsule made of a refractory metal such as Ta or Nb, heated in a vacuum and sealed, and then the mixed powder is used. Remove adsorbed gas and air. After that, it is preferable to carry out a step of forming dislocations in the diamond particles described above and a step of sintering the mixed powder described later.
- the step of sintering the mixed powder as it is without taking out the mixed powder from the capsule made of the refractory metal is performed. It is preferable to do it.
- the holding pressure is preferably 4 GPa or more and 7 GPa or less, and more preferably 4.5 GPa or more and 6 GPa or less.
- the holding temperature is preferably 30 ° C. or higher and 600 ° C. or lower, and more preferably 50 ° C. or higher and 500 ° C. or lower.
- the holding time is preferably 50 minutes or more and 190 minutes or less, and more preferably 60 minutes or more and 180 minutes or less.
- the mixed powder is sintered at a sintering pressure of 4 GPa or more and 8 GPa or less and a sintering temperature of 1400 ° C. or higher and 1700 ° C. or lower for a sintering time of 1 minute or more and 60 minutes or less.
- a sintering pressure of 4 GPa or more and 8 GPa or less
- a sintering temperature of 1400 ° C. or higher and 1700 ° C. or lower for a sintering time of 1 minute or more and 60 minutes or less.
- the sintering pressure is preferably 4 GPa or more and 8 GPa or less, and more preferably 4.5 GPa or more and 7 GPa or less.
- the sintering temperature is preferably 1400 ° C. or higher and 1700 ° C. or lower, and more preferably 1450 ° C. or higher and 1550 ° C. or lower.
- the sintering time is preferably 1 minute or more and 60 minutes or less, and more preferably 5 minutes or more and 20 minutes or less.
- Each prepared raw material powder is added in various blending ratios and mixed by a dry method using a ball mill so that the finally obtained diamond sintered body has the composition shown in Table 3-1 or Table 3-2.
- a mixed powder was prepared.
- the mixed powder is sintered in a state of being in contact with a disk made of WC-6% Co cemented carbide as described later. Therefore, it is considered that cobalt and tungsten are infiltrated into the diamond sintered body from the disk during sintering, and the cobalt content and the tungsten content in the diamond sintered body increase.
- the blending ratio of each raw material powder was determined in consideration of the increase in the cobalt content and the increase in the tungsten content in advance.
- the mixed powder was placed in a capsule made of Ta in contact with a disk made of WC-6% Co cemented carbide, heated in vacuum, and sealed. Then, the mixed powder was heat-treated at the holding pressure, holding temperature and holding time shown in Table 2-1 or Table 2-2 using a high-pressure high-temperature generator.
- composition of the bonded phase in the diamond sintered body was specified by SEM-EDX. Since the specific measurement method is the same as the method described in the above [Details of Embodiments of the present disclosure] column, the description thereof will not be repeated. The results are shown in Tables 3-1 and 3-2 (see "Composition of bound phase” column).
- ⁇ Cutting test 2 Turning test> Using each of the diamond sintered bodies of the samples 15 to 20 prepared as described above, a cutting tool (holder: CSRP R3225-N12, chip: SPGN120308, tool equipped with the diamond sintered body on the cutting edge portion of the chip) is prepared. Then, a turning test was carried out. The cutting conditions for the turning test are shown below. The turning test can be evaluated as a cutting tool having excellent chipping resistance and wear resistance as the cutting distance (km) is longer. Further, in this case, the diamond sintered body used for the cutting tool can be evaluated to have excellent crack growth resistance. The results are shown in Table 3-1. In the cutting test 2, the samples 15 to 19 correspond to the examples. Sample 20 corresponds to a comparative example.
- ⁇ Cutting test 3 Rolling test> Cutting tool using each of the diamond sintered bodies of samples 21 to 32 produced as described above (cutter: RF4080R, tip: SNEW1204ADFR, tool equipped with the diamond sintered body on the cutting edge portion of the tip in the tip exchange type cutter) was prepared and a milling test was carried out.
- the cutting conditions for the rolling test are shown below.
- the larger the cutting volume (cm 3 ) the more excellent the chipping resistance and the impact resistance can be evaluated as a cutting tool.
- the diamond sintered body used for the cutting tool can be evaluated to have excellent crack growth resistance.
- Table 3-2 In the cutting test 3, the samples 23 to 30 and the sample 32 correspond to the examples. Sample 21, sample 22 and sample 31 correspond to comparative examples.
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Abstract
Description
また、特許文献1には、当該高強度・高耐摩耗性ダイヤモンド焼結体の製造方法であって、ベルト型超高圧装置を用いて圧力5.7GPa以上7.5GPa以下、温度1400℃以上1900℃以下の条件で焼結することを特徴とする、高強度・高耐摩耗性ダイヤモンド焼結体の製造方法が開示されている。
ダイヤモンド粒子を含むダイヤモンド焼結体であって、
上記ダイヤモンド粒子の含有率は、上記ダイヤモンド焼結体に対して、80体積%以上99体積%以下であり、
上記ダイヤモンド粒子の平均粒径は、0.1μm以上50μm以下であり、
上記ダイヤモンド粒子の転位密度は、1.2×1016m-2以上5.4×1019m-2以下である。
特許文献1のダイヤモンド焼結体は、切削工具等に適用すると、刃先の欠損が生じる場合がある。また、近年はより高効率な(例えば、送り速度が大きい)切削加工が求められており、ダイヤモンド焼結体の更なる性能の向上(例えば、亀裂進展の抑制等)が期待されている。
本開示によれば、優れた耐亀裂進展性を有するダイヤモンド焼結体、及びダイヤモンド焼結体を備える工具を提供することが可能になる。
最初に本開示の実施態様を列記して説明する。
[1]本開示の一態様に係るダイヤモンド焼結体は、
ダイヤモンド粒子を含むダイヤモンド焼結体であって、
上記ダイヤモンド粒子の含有率は、上記ダイヤモンド焼結体に対して、80体積%以上99体積%以下であり、
上記ダイヤモンド粒子の平均粒径は、0.1μm以上50μm以下であり、
上記ダイヤモンド粒子の転位密度は、1.2×1016m-2以上5.4×1019m-2以下である。
上記結合相は、
周期表の第4族元素、第5族元素、第6族元素、鉄、アルミニウム、珪素、コバルト及びニッケルからなる群より選ばれる少なくとも1種の金属元素を含む単体金属、合金、及び金属間化合物からなる群より選ばれる少なくとも1種、又は、
周期表の第4族元素、第5族元素、第6族元素、鉄、アルミニウム、珪素、コバルト及びニッケルからなる群より選ばれる少なくとも1種の金属元素と、窒素、炭素、硼素及び酸素からなる群より選ばれる少なくとも1種の非金属元素とからなる化合物、及び、上記化合物由来の固溶体からなる群より選ばれる少なくとも1種、
を含むことが好ましい。このように規定することで、更に耐亀裂進展性に優れるダイヤモンド焼結体となる。
本開示の実施形態の詳細を、以下に説明する。なお、本開示はこれらの例示に限定されるものではない。ここで、本明細書において「A~Z」という形式の表記は、範囲の上限下限(すなわちA以上Z以下)を意味し、Aにおいて単位の記載がなく、Zにおいてのみ単位が記載されている場合、Aの単位とZの単位とは同じである。
本実施形態に係るダイヤモンド焼結体は、
ダイヤモンド粒子を含むダイヤモンド焼結体であって、
上記ダイヤモンド粒子の含有率は、上記ダイヤモンド焼結体に対して、80体積%以上99体積%以下であり、
上記ダイヤモンド粒子の平均粒径は、0.1μm以上50μm以下であり、
上記ダイヤモンド粒子の転位密度は、1.2×1016m-2以上5.4×1019m-2以下である。
(ダイヤモンド粒子の含有率)
本実施形態において、上記ダイヤモンド粒子の含有率は、上記ダイヤモンド焼結体に対して、80体積%以上99体積%以下であり、80体積%以上90体積%以下であることが好ましい。
ダイヤモンド粒子の平均粒径は、0.1μm以上50μm以下であり、0.2μm以上40μm以下であることが好ましい。ダイヤモンド粒子の平均粒径が0.1μm以上であることによって、ダイヤモンド粒子が緻密に焼結され、耐欠損性に優れるダイヤモンド焼結体となる。ダイヤモンド粒子の平均粒径が50μm以下であることによって、異方性が無く、切削工具の刃先として用いた場合切削安定性に優れるダイヤモンド焼結体となる。
上記ダイヤモンド粒子の転位密度は、1.2×1016m-2以上5.4×1019m-2以下であり、1.5×1016m-2以上1.0×1017m-2以下であることが好ましい。ダイヤモンド粒子の転位密度が1.2×1016m-2以上であることによって、不動転位が比較的多く存在するため、ダイヤモンド粒子に発生する亀裂進展が抑制され、耐亀裂進展性に優れるダイヤモンド焼結体となる。ダイヤモンド粒子の転位密度が5.4×1019m-2以下であることによって、ダイヤモンド粒子の亀裂の発生を抑制し、耐衝撃性に優れるダイヤモンド焼結体となる。
X線源:放射光
装置条件:検出器NaI(適切なROIにより蛍光をカットする。)
エネルギー:18keV(波長:0.6888Å)
分光結晶:Si(111)
入射スリット:幅3mm×高さ0.5mm
受光スリット:ダブルスリット(幅3mm×高さ0.5mm)
ミラー:白金コート鏡
入射角:2.5mrad
走査方法:2θ-θscan
測定ピーク:ダイヤモンドの(111)、(220)、(311)、(331)、(422)、(440)、(531)の7本。ただし、集合組織、配向などによりプロファイルの取得が困難な場合は、その面指数のピークを除く。
測定条件:各測定ピークに対応する半値全幅中に、測定点が9点以上となるようにする。ピークトップ強度は2000counts以上とする。ピークの裾も解析に使用するため、測定範囲は半値全幅の10倍程度とする。
C=Ch00[1-q(h2k2+h2l2+k2l2)/(h2+k2+l2)2] (II)
<ε(L)2>=(ρCb2/4π)ln(Re/L) (III)
lnA(L)=lnAS(L)-(πL2ρb2/2)ln(Re/L)(K2C)+O(K2C)2 (IV)
本実施形態において、上記ダイヤモンド焼結体は、結合相を更に含み、
上記結合相は、
周期表の第4族元素、第5族元素、第6族元素、鉄、アルミニウム、珪素、コバルト及びニッケルからなる群(以下、「群A」とも記す。)より選ばれる少なくとも1種の金属元素を含む単体金属、合金、及び金属間化合物からなる群より選ばれる少なくとも1種、又は、
周期表の第4族元素、第5族元素、第6族元素、鉄、アルミニウム、珪素、コバルト及びニッケルからなる群(群A)より選ばれる少なくとも1種の金属元素と、窒素、炭素、硼素及び酸素からなる群(以下、「群B」とも記す。)より選ばれる少なくとも1種の非金属元素とからなる化合物、及び、上記化合物由来の固溶体からなる群より選ばれる少なくとも1種、
を含むことが好ましい。換言すると上記結合相は、下記の(a)から(f)のいずれかの形態とすることができる。
上記結合相の含有率は、上記ダイヤモンド焼結体に対して、1体積%以上20体積%以下であることが好ましく、10体積%以上20体積%以下であることがより好ましい。結合相の含有率(体積%)は、上述したSEM付帯のEDXを用いて、ダイヤモンド焼結体に対し、組織観察、元素分析等を実施することによって確認することができる。
本実施形態のダイヤモンド焼結体は、耐亀裂進展性に優れているため、切削工具、耐摩工具、研削工具、摩擦撹拌接合用ツール等に好適に用いることができる。すなわち、本実施形態の工具は、上記のダイヤモンド焼結体を備えるものである。上記工具は、各種材料の加工において優れた耐欠損性及び優れた耐衝撃性を有する。上記工具が切削工具である場合、上記切削工具はアルミ合金(例えば、ADC12、AC4B)等の転削加工及び旋削加工に特に適している。
本実施形態に係るダイヤモンド焼結体の製造方法は、
ダイヤモンド粒子の原料粉末と結合相の原料粉末とを準備する工程と、
上記ダイヤモンド粒子の原料粉末と上記結合相の原料粉末とを混合して混合粉末を得る工程と、
4GPa以上7GPa以下の保持圧力、30℃以上600℃以下の保持温度で、50分以上190分以下の保持時間の間、上記混合粉末を加熱して、上記ダイヤモンド粒子に転位を生成する工程と、
4GPa以上8GPa以下の焼結圧力、1400℃以上1900℃以下の焼結温度で、1分以上60分以下の焼結時間の間、上記混合粉末を焼結する工程と、
を備える。
本工程では、ダイヤモンド粒子の原料粉末(以下「ダイヤモンド粉末」とも記す。)と結合相の原料粉末(以下、「結合相原料粉末」とも記す。)とを準備する。ダイヤモンド粉末は、特に限定されず、公知のダイヤモンド粒子を原料粉末として用いることができる。
本工程では、上記ダイヤモンド粒子の原料粉末(ダイヤモンド粉末)と上記結合相の原料粉末(結合相原料粉末)とを混合して混合粉末を得る。このとき、上記ダイヤモンド粉末と上記結合相原料粉末とは、ダイヤモンド焼結体中におけるダイヤモンド粒子の含有率が上述の範囲内となるように、任意の配合比率にて混合してもよい。
本工程では、4GPa以上7GPa以下の保持圧力、30℃以上600℃以下の保持温度で、50分以上190分以下の保持時間の間、上記混合粉末を加熱して、上記ダイヤモンド粒子に転位を生成する。ダイヤモンドの溶解及び再析出が生じない低温でダイヤモンド粉末を加圧することで、ダイヤモンドの結晶構造が変化し、転位が発生する。
本工程では、4GPa以上8GPa以下の焼結圧力、1400℃以上1700℃以下の焼結温度で、1分以上60分以下の焼結時間の間、上記混合粉末を焼結する。これにより本開示のダイヤモンド焼結体が得られる。
<ダイヤモンド粒子の原料粉末と結合相の原料粉末とを準備する工程>
原料粉末として、表1-1及び表1-2に示す平均粒径又は組成の粉末を準備した。
最終的に得られるダイヤモンド焼結体が表3-1又は表3-2に記載の組成となるように、準備した各原料粉末を種々の配合割合で加えて、ボールミルを用いて乾式で混合し、混合粉末を作製した。ここで、上記混合粉末は、後述するようにWC-6%Co超硬合金製の円盤に接した状態で焼結が行われる。そのため焼結の際、当該円盤からコバルト及びタングステンがダイヤモンド焼結体に溶浸し、ダイヤモンド焼結体中のコバルトの含有率及びタングステンの含有率が上昇すると考えられる。このコバルトの含有率の上昇分及びタングステンの含有率の上昇分を予め考慮して、各原料粉末の配合割合を決定した。
次に、上記混合粉末を、WC-6%Co超硬合金製の円盤に接した状態でTa製のカプセルに入れて真空中で加熱して密閉した。その後、高圧高温発生装置を用いて、表2-1又は表2-2に示す保持圧力、保持温度及び保持時間で上記混合粉末を加熱処理した。
上述のダイヤモンド粒子に転位を生成する工程に引き続いて、表2-1又は表2-2に示す焼結圧力、焼結温度及び焼結時間で上記混合粉末を焼結した。以上の工程を経て、試料1~32のダイヤモンド焼結体を製造した。
<ダイヤモンド焼結体の組成>
ダイヤモンド焼結体におけるダイヤモンド粒子と結合相との含有率(体積比)を測定した。具体的な測定方法は、上記の[本開示の実施形態の詳細]の欄に記載された方法と同一であるため、その説明は繰り返さない。各試料において、ダイヤモンド焼結体におけるダイヤモンド粒子の含有率は、表3-1及び表3-2(「含有率」の欄参照)に示される通りであることが確認された。
ダイヤモンド焼結体におけるダイヤモンド粒子の平均粒径を測定した。具体的な測定方法は、上記の[本開示の実施形態の詳細]の欄に記載された方法と同一であるため、その説明は繰り返さない。結果を表3-1及び表3-2(「平均粒径」の欄参照)に示す。
ダイヤモンド焼結体における結合相の組成をSEM-EDXにより特定した。具体的な測定方法は、上記の[本開示の実施形態の詳細]の欄に記載された方法と同一であるため、その説明は繰り返さない。結果を表3-1及び表3-2(「結合相の組成」の欄参照)に示す。
ダイヤモンド焼結体におけるダイヤモンド粒子の転位密度を測定した。具体的な測定方法は、上記の[本開示の実施形態の詳細]の欄に記載された方法と同一であるため、その説明は繰り返さない。結果を表3-1及び表3-2(「転位密度」の欄参照)に示す。
<切削試験1:転削加工試験>
上述のようにして作製した試料1~14のダイヤモンド焼結体それぞれを用いて切削工具(カッタ:RF4080R、チップ:SNEW1204ADFR、チップ交換型カッタにおけるチップの刃先部分に上記ダイヤモンド焼結体を備える工具)を作製し、転削加工試験を実施した。転削加工試験の切削条件を以下に示す。上記転削加工試験は、切削体積(cm3)が大きいほど耐欠損性、耐衝撃性に優れる切削工具として評価することができる。また、この場合、切削工具に用いたダイヤモンド焼結体は、耐亀裂進展性に優れると評価することができる。結果を表3-1に示す。切削試験1において、試料3~10及び試料12~14が実施例に相当する。試料1、試料2及び試料11が比較例に相当する。
被削材 :ADC12(60mm×290mm×60mm)
切削速度 :3000m/分
送り量 :0.2mm/t
切り込み :0.4mm
クーラント :wet
評価方法 :被削材の290mm×60mm面を転削加工して、切削工具の平均逃げ面摩耗幅が250μmに達するまでの切削体積(cm3)
上述のようにして作製した試料15~20のダイヤモンド焼結体それぞれを用いて切削工具(ホルダ:CSRP R3225-N12、チップ:SPGN120308、チップの刃先部分に上記ダイヤモンド焼結体を備える工具)を作製し、旋削加工試験を実施した。旋削加工試験の切削条件を以下に示す。上記旋削加工試験は、切削距離(km)が長いほど耐欠損性、耐摩耗性に優れる切削工具として評価することができる。また、この場合、切削工具に用いたダイヤモンド焼結体は、耐亀裂進展性に優れると評価することができる。結果を表3-1に示す。切削試験2において、試料15~19が実施例に相当する。試料20が比較例に相当する。
被削材 :Ti-6Al-4V(φ120mm×280mm)
切削速度 :270m/分
送り量 :0.12mm/rev
切り込み :0.35mm
クーラント :wet
評価方法 :被削材の外径を旋削加工して、切削工具の平均逃げ面摩耗幅が200μmに達するまでの切削距離(km)
切削試験1の結果から試料3~10及び試料12~14の切削工具(実施例の切削工具)は、切削体積が、3800cm3以上という良好な結果が得られた。一方試料1、試料2及び試料11の切削工具(比較例の切削工具)は、切削加工の初期の段階で欠けが発生し、切削体積を求めることができなかった。以上の結果から、実施例の切削工具は、比較例の切削工具に比べて耐欠損性、耐衝撃性に優れることが分かった。また、実施例のダイヤモンド焼結体は、比較例のダイヤモンド焼結体に比べて耐亀裂進展性に優れることが分かった。
上述のようにして作製した試料21~32のダイヤモンド焼結体それぞれを用いて切削工具(カッタ:RF4080R、チップ:SNEW1204ADFR、チップ交換型カッタにおけるチップの刃先部分に上記ダイヤモンド焼結体を備える工具)を作製し、転削加工試験を実施した。転削加工試験の切削条件を以下に示す。上記転削加工試験は、切削体積(cm3)が大きいほど耐欠損性、耐衝撃性に優れる切削工具として評価することができる。また、この場合、切削工具に用いたダイヤモンド焼結体は、耐亀裂進展性に優れると評価することができる。結果を表3-2に示す。切削試験3において、試料23~30及び試料32が実施例に相当する。試料21、試料22及び試料31が比較例に相当する。
被削材 :AC4B(60mm×290mm×60mm)
切削速度 :3300m/分
送り量 :0.1mm/t
切り込み :0.3mm
クーラント :wet
評価方法 :被削材の290mm×60mm面を転削加工して、切削工具の平均逃げ面摩耗幅が250μmに達するまでの切削体積(cm3)
切削試験3の結果から試料23~30及び試料32の切削工具(実施例の切削工具)は、切削体積が、4700cm3以上という良好な結果が得られた。一方試料21、試料22及び試料31の切削工具(比較例の切削工具)は、切削加工の初期の段階で欠けが発生し、切削体積を求めることができなかった。以上の結果から、実施例の切削工具は、比較例の切削工具に比べて耐欠損性、耐衝撃性に優れることが分かった。また、実施例のダイヤモンド焼結体は、比較例のダイヤモンド焼結体に比べて耐亀裂進展性に優れることが分かった。
Claims (5)
- ダイヤモンド粒子を含むダイヤモンド焼結体であって、
前記ダイヤモンド粒子の含有率は、前記ダイヤモンド焼結体に対して、80体積%以上99体積%以下であり、
前記ダイヤモンド粒子の平均粒径は、0.1μm以上50μm以下であり、
前記ダイヤモンド粒子の転位密度は、1.2×1016m-2以上5.4×1019m-2以下である、ダイヤモンド焼結体。 - 前記ダイヤモンド粒子の転位密度は、1.5×1016m-2以上1.0×1017m-2以下である、請求項1に記載のダイヤモンド焼結体。
- 結合相を更に含み、
前記結合相は、
周期表の第4族元素、第5族元素、第6族元素、鉄、アルミニウム、珪素、コバルト及びニッケルからなる群より選ばれる少なくとも1種の金属元素を含む単体金属、合金、及び金属間化合物からなる群より選ばれる少なくとも1種、又は、
周期表の第4族元素、第5族元素、第6族元素、鉄、アルミニウム、珪素、コバルト及びニッケルからなる群より選ばれる少なくとも1種の金属元素と、窒素、炭素、硼素及び酸素からなる群より選ばれる少なくとも1種の非金属元素とからなる化合物、及び、前記化合物由来の固溶体からなる群より選ばれる少なくとも1種、
を含む、請求項1に記載のダイヤモンド焼結体。 - 前記結合相は、コバルトを含む、請求項3に記載のダイヤモンド焼結体。
- 請求項1から請求項4のいずれか一項に記載のダイヤモンド焼結体を備える工具。
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JP7042989B1 (ja) | 2022-03-28 |
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JPWO2022085161A1 (ja) | 2022-04-28 |
EP4234135A1 (en) | 2023-08-30 |
EP4234135A4 (en) | 2023-11-22 |
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TW202225126A (zh) | 2022-07-01 |
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