JP6281875B2 - ニアネット切削工具インサート - Google Patents
ニアネット切削工具インサート Download PDFInfo
- Publication number
- JP6281875B2 JP6281875B2 JP2014550536A JP2014550536A JP6281875B2 JP 6281875 B2 JP6281875 B2 JP 6281875B2 JP 2014550536 A JP2014550536 A JP 2014550536A JP 2014550536 A JP2014550536 A JP 2014550536A JP 6281875 B2 JP6281875 B2 JP 6281875B2
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- JP
- Japan
- Prior art keywords
- powder
- green body
- diamond
- containment
- hard
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000005520 cutting process Methods 0.000 title description 23
- 239000000843 powder Substances 0.000 claims description 92
- 238000000034 method Methods 0.000 claims description 73
- 239000010432 diamond Substances 0.000 claims description 61
- 229910003460 diamond Inorganic materials 0.000 claims description 60
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 58
- 238000005245 sintering Methods 0.000 claims description 48
- 239000010439 graphite Substances 0.000 claims description 41
- 229910002804 graphite Inorganic materials 0.000 claims description 41
- 239000000203 mixture Substances 0.000 claims description 41
- 239000008187 granular material Substances 0.000 claims description 34
- 239000002002 slurry Substances 0.000 claims description 31
- 239000011230 binding agent Substances 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 26
- 239000002131 composite material Substances 0.000 claims description 22
- 229910052582 BN Inorganic materials 0.000 claims description 18
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 18
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 239000002202 Polyethylene glycol Substances 0.000 claims description 14
- 229920001223 polyethylene glycol Polymers 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- 238000001694 spray drying Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 150000004767 nitrides Chemical class 0.000 claims description 7
- 229910052752 metalloid Inorganic materials 0.000 claims description 6
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- 239000012530 fluid Substances 0.000 claims description 5
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- 229910010293 ceramic material Inorganic materials 0.000 claims 2
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- 229910052618 mica group Inorganic materials 0.000 claims 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims 1
- 239000011343 solid material Substances 0.000 claims 1
- 239000000454 talc Substances 0.000 claims 1
- 229910052623 talc Inorganic materials 0.000 claims 1
- 238000009827 uniform distribution Methods 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 24
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 17
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 8
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 5
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
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- 239000003570 air Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
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- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 2
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 229910002515 CoAl Inorganic materials 0.000 description 1
- 229910001141 Ductile iron Inorganic materials 0.000 description 1
- 229910000943 NiAl Inorganic materials 0.000 description 1
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 239000003610 charcoal Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
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- 238000010304 firing Methods 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 238000003698 laser cutting Methods 0.000 description 1
- 150000004668 long chain fatty acids Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
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- 239000001301 oxygen Substances 0.000 description 1
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- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
- B24D18/0009—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for using moulds or presses
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- 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
- B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/026—Spray drying of solutions or suspensions
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- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
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- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
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- B24D3/20—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially organic
- B24D3/28—Resins or natural or synthetic macromolecular compounds
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- 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
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- 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
- C04B35/528—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 obtained from carbonaceous particles with or without other non-organic components
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- 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
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- C04B35/58—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/583—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
- C04B35/5831—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride based on cubic boron nitrides or Wurtzitic boron nitrides, including crystal structure transformation of powder
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- C—CHEMISTRY; METALLURGY
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
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- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62695—Granulation or pelletising
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- 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
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
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- 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/0605—Composition of the material to be processed
- B01J2203/063—Carbides
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J2203/0645—Boronitrides
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- B01J2203/06—High pressure synthesis
- B01J2203/065—Composition of the material produced
- B01J2203/0655—Diamond
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J2203/06—High pressure synthesis
- B01J2203/065—Composition of the material produced
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Description
本出願は2011年12月30日に出願された米国仮出願第61/581664号の利益を主張する。
72wt%のcBN、8wt%のAl、3.2wt%のAl2O3、6.4wt%のTiC及び10.4wt%の化学量論未満のTiNをミリング液体中で混合しそしてミリングすることによりcBN材料のニアネットボディを製造した。粉末混合物をパン乾燥し、その後、82%エタノール/18%水の溶液とブレンドし、そして有機バインダPEG300、PEG1500及びPEG4000を乾燥粉末の20体積%に対応する量まで添加した。スラリー粘度を噴霧乾燥工程の前に注意深く制御した。顆粒化粉末は良好な流動性を有し、そして50トンDorsetプレスを用いて行った単軸プレス加工工程の間にダイを容易に充填することができ、そしてプレス加工圧力は約30kNであった。グリーンを単一工程プロセスで脱バインダ及び予備焼結し、そして脱バインダ工程を水素流下で500℃までのゆっくりとした上昇の間に行い、次いで、900℃まで真空下に上げ、15分間維持することにより予備焼結した。
1=cBN、立方晶窒化ホウ素、PDF番号00−035−1365
2=TiB2、PDF番号01−075−0967
3=α−Al2O3、コランダム、PDF番号00−046−1212
4=AlN、PDF番号00−025−1133
5=TiC、Khamrabaevite、PDF番号00−032−1383
6=TiN0.96、Osbornite、PDF番号01−087−0627。反射の位置は、しかしながら、より低い2θに向けて若干シフトし、若干、より大きい単位セル寸法を示している。
例1で記載したのと同一の粉末から、切削工具幾何学形状SNMNにおけるボディを厚さ=8.016mm及び内接円(IC)=15.712mmで約60%の相対密度にプレス加工し、その後、例1に記載されるのと同様にして予備焼結した。予備焼結後に、ボディをグラファイト粉末中にプレス加工し、MgO容器中に入れ、下方及び上方に高密度グラファイトがあり、そしてトップにMgOリッドを有し、図6に示すとおりである。
72wt%のcBN、8wt%のAl、3.2wt%のAl2O3、6.4wt%のTiC及び10.4wt%の化学量論未満のTiNを有機ミリング液体中で混合しそしてミリングすることによりcBN材料からなる粉末混合物を製造した。スラリーをパン乾燥し、その後、粉末をグラファイト容器中に充填し、そして1500〜1600℃、5GPaで30分間HPHT−処理し、固体焼結PCBNディスクを形成した。
89wt%のcBN、11wt%のAlをミリング液体中で混合しそしてミリングすることによりcBN材料のニアネットボディを製造した。粉末混合物をパン乾燥し、その後、82%エタノールとブレンドし、そして有機バインダPEG300、PEG1500及びPEG4000を乾燥粉末の22体積%に対応する量まで添加した。スラリー粘度を噴霧乾燥工程の前に注意深く制御した。顆粒化粉末は良好な流動性を有し、そして30トンDorsetプレスで行った単軸プレス加工工程の間にダイを容易に充填することができた。グリーンを最大の許容される力を用いてプレス加工し、SNMN幾何学形状を形成した。グリーンを単一工程プロセスで脱バインダ及び予備焼結し、そして脱バインダ工程を水素流下で500℃までのゆっくりとした上昇の間に行い、次いで、900℃まで真空下に上げ、15分間維持することにより予備焼結した。冷却時に、硬質グリーンの正方形物は硬く強固であり、クラック及び歪みを含まず、約14.60mmのIC及び約7.70mmの厚さの寸法であり、2.1〜2.3g/cm3の密度であり、それは65%±1%の相対密度に対応する。予備焼結後に、硬質グリーンは図26で低いほうのディフラクトグラム(900°)に示すとおり、cBN、Al及び少量のAlNを含んだ。
1=cBN、立方晶窒化ホウ素、PDF番号00−035−1365、
2=AlN、PDF番号00−025−1133
97wt%のcBN及び3wt%のAlを有機ミリング液体中で混合しそしてミリングすることによりcBN材料からなる粉末混合物を製造した。スラリーをパン乾燥した。その後、粉末を、下方にAl−ディスクを含むグラファイト容器中に充填し、そして1600℃、5.5GPaで25分間行うHPHTの間にAlを掃去しそしてAlNへと反応させた。この方法において、最終材料中のAl−含有分はHPHT及び浸透の前の粉末密度及び粉末床の均一性により、粉末バッチ毎に異なった。
例4(ニアネットA及びBインサート)及び例5(標準、STDインサート)に記載の方法により製造されたSNMN1204インサートを全面研削して、約12.70mmのIC及び4.75mmの厚さの寸法を有する面取りされた切削工具を製造した。得られた工具を、V=314m/分、フィード=0.03mm/rev及び切削深さ=0.05mmで鋳鉄を機械加工することにより試験した。図10は2つの例示のニアネットインサートの性能をHPHT焼結ブランク材料の従来のレーザーカッティングにより製造された同一のインサートと比較する。結果は、標準製造材料、STDにおける約7〜8wt%Alと比較して、ニアネットA及びBインサートにおけるAlN含有分が11wt%のAlという、より高いAlN含有分であるにも係わらず、ニアネット法により製造される材料が従来法により製造されたものと同一の品質であることを示す。
ダイヤモンド、シリコン及び窒化ケイ素粉末を湿式ミリング法を用いてミリング流体としてのイソプロピルアルコールとブレンドして、均質混合物を形成した。混合物の質量百分率は90%ダイヤモンド、9.5%シリコン、0.5%窒化ケイ素であった。ダイヤモンドは20〜30ミクロンダイヤモンド80%及び4〜8ミクロンダイヤモンド20%の混合物であった。シリコンは、Alfa Aesarシリコン粉末であり、結節性でAPS1〜5ミクロン、99.999%(金属基準)であった。窒化ケイ素は、Alfa Aesarの窒化ケイ素(IV)、α相、99.5%(金属基準)、<1ミクロンであった。スラリーは、流体として水を用い、バインダーとして、この混合物の24体積%のPEGを用いて調製した。スラリーを噴霧凍結造粒し、プレス加工用顆粒を製造した。
ダイヤモンドスラリー及び顆粒を例3に記載の方法と同一の方法を用いて製造した。顆粒を用いて24mm直径及び12mm高さと測定される円筒物をプレス加工した。ドリルプレスを用いて4.8mm直径と測定される中央穴をドリルした。次いで、例7に記載したのと同一の方法を用いて円筒物を予備焼結した。硬質グリーンの写真を図11に示す。
例7に記載の方法と同一の方法を用いて採掘ピックを製造したが、使用したシリコン粉末はElkem Silgrain HQ 0.05 Fe <10ミクロンであった。軟質グリーンピックの相対密度は64%であった。HPHT焼結後に、採掘ピックは密度が3.419g/cm3であった。ピックの円筒形ボディをセンターレスグラインダーで14.00mmに研削し、ピックの基部をワイヤEDMを用いてある長さに切断し、そしてダイヤモンド研削ホイールを用いてピックの底部上を研削して45°面取りを行った。ピックの円錐切削表面を形成するために研削又は他の仕上げ操作を行わなかった。試験前のピックのCTスキャンを図19に示す。これらのスキャンのために用いたCT装置は以下の設定を用いたGe Sensig and Inspection Technologiesからのv/tome/xs240であった。
2つの顆粒化粉末を例1(PCBN)に記載のとおりに製造したが、粉末2を製造するときに、分散剤として作用する0.52wt%のTEA(トリエタノールアミン)もスラリーに添加した。粉末をコールドプレスし、55及び59%相対密度を有する円筒物を製造し、有機バインダ及び分散剤を除外した。円筒形ピルを片面プレスインし、そしてKZKからのPowder Testing Center モデルPTC-03DT装置を用いて軸強度を測定した。プレスインしたダイの寸法はOD=12.700mm及び高さ=10.033mmであった。55から59%へのプレス密度の増加により、2.9MPaから5.4MPaの軸軟質グリーン強度の増加をもたらした。
例4(PCBN)に記載のとおりに製造した顆粒粉末をコールドプレスし、59%相対密度を有する円筒物を製造し、有機バインダ及び分散剤を除外した。円筒形ピルを片面プレスインし、そしてKZKからのPowder Testing Center モデルPTC-03DT装置を用いて軸強度を測定した。プレスインしたダイの寸法はOD=12.700mm及び高さ=10.020mmであった。円筒物を、その後、例1に記載のとおりに脱バインダしそして予備焼結し、そして硬質グリーンの軸強度を測定し、軸強度は、13.6MPaと比較して80.6MPaと、軟質グリーンよりも有意に高いことが分かった。
同一の組成を有しそして例7に記載のとおりに製造した顆粒化粉末を円筒形ピルにプレス加工し、それは60%相対密度を有し、有機バインダを除外した。例7に記載のとおりに円筒形ピルを片面プレスし、そして1200、1300、1350及び1400℃に予備焼結する前及び後に軸強度を測定した。プレス及び強度測定はKZKからのPowder Testing Center モデルPTC-03DT装置を用いて行った。プレスインしたダイの寸法はOD=12.700mm及び高さ=10.033mmであった。
1=C、ダイヤモンド、PDF番号00−006−0675
2=Si、シリコン、PDF番号00−027−1402
3=SiC、モアッサナイト−3C、PDF番号00−029−1129
4=α−Si3N4、α−窒化ケイ素、PDF番号00−041−0360
予備焼結温度を変更することにより、HPHT前の組成及びグリーン強度は変化することがあり、各組成について最適化されうる。900℃及び1100℃に予備焼結した例4(PCBN7000)に記載のとおりのグリーンについての予備焼結反応の例を下記に示した。図26は900℃及び1100℃に予備焼結した例に記載の組成を有する2つの硬質グリーンの回折パターンを示す。ディフラクトグラムはXPERT-PROディフラクトメータを用いてCuKa線を用いて室温で得られた。ステップサイズ0.008°を用いて2θで10〜95°の間でデータを回収したが、2θで30〜80°の範囲のみを示している。バックグランド及びCuKa2−ピークをDIFFRAC Plus Evaluation ソフトウエアを用いて差し引いた。ディフラクトグラムは、また、内部標準としてcBN(PDF番号00−035−1365)の111−ピークを用いてサンプル変位について補正した。ディファクトグラムの反射を指数化し、図中の数は下記の相に対応する。
1=cBN、立方晶窒化ホウ素、PDF番号00−035−1365
2=Al、アルミニウム、PDF番号00−004−0787
3=AlN、PDF番号00−025−1133
例7に記載した方法と同一の方法を用いて6つのダイヤモンド複合材採掘ピックを製造したが、1つの硬質グリーンボディを各封じ込め手段に封入するのではなく、3つの硬質グリーンボディを各封じ込め手段に封入した。封じ込め手段を高圧セルに組み立て、そして例7に記載した条件と同一の条件を用いて処理した。図12は焼結後のHPHTセルの写真を示し、セルの片側は露出して、グラファイト封じ込め手段に埋め込まれたニアネット形状ボディを現している。
例8に記載の方法と同一の方法を用いて14個の硬質グリーンボディを製造したが、HPHT焼結の前に硬質グリーンボディに穴をドリルで空けず、また、予備焼結を1200℃〜1550℃の範囲の種々の最大温度で行った。横断方向破断強度を測定するためのテストバー、及び、XRD定性スキャン及び定量相分析のためのディスクをワイヤEDM機械を用いて焼結体から切った。XRD定量相分析をJade XRD分析ソフトウエアの"Easy Quantitative Analysis"ルーチンを用いて行った。図15は1200℃、1300℃及び1430℃で予備焼結したHPHT焼結体の組成の比較を示す。図16はHPHT焼結体の曲げ強度(横断方向破断強度)に対する予備焼結温度の効果を示す。図17はHPHT焼結体のSiC含有分に対する予備焼結温度の効果を示す。図18は1200℃、1300℃、1350℃及び1400℃に焼結した硬質グリーンボディ中に存在する相に対する予備焼結温度の効果を示す。相1はダイヤモンドであり、相2はシリコンであり、相3は炭化ケイ素であり、そして相4は窒化ケイ素である。予備焼結温度を増加させると、SiC含有分が増加する。硬質グリーンボディの組成の変化はHPHT焼結体の最終組成及び強度を変化させる。図17はHPHT焼結体中のSiC含有分が約1400℃の予備焼結温度を超えると、有意に高くなることを示している。図16は材料強度に対するこの組成変化の効果を示し、これは約1400℃の予備焼結温度を超えると、有意に低下することを示す。
Claims (20)
- ダイヤモンド及び/又は立方晶窒化ホウ素粉末と、金属粉末、半金属粉末、酸化物粉末、炭化物粉末、窒化物粉末、炭窒化物粉末、カルボオキシ窒化物粉末及びホウ化物粉末の群から選択される粉末とを含む粉末、分散剤、バインダ及び流体の混合物から顆粒を調製すること、
該顆粒を圧縮して、画定された形状の軟質グリーンボディを形成すること、
該軟質グリーンボディを炉内で加熱し、硬質グリーンボディを形成すること、
封じ込め粉末中に1つ以上の硬質グリーンボディを埋め込み、そして該封じ込め粉末を圧縮して、圧力セルを形成すること、
該圧力セルを高圧高温下で焼結すること、及び、
該圧力セルから封じ込め粉末を取り出し、1つ以上のニアネットボディを現すこと、
を含む、ニアネット超硬材料体の製造方法。 - 前記顆粒は立方晶窒化ホウ素、窒化物及び/又はホウ化物形成性金属及び一時的な有機バインダの混合物を含む、請求項1に記載の方法。
- 前記顆粒はダイヤモンド及び炭化物形成性金属又は炭化物形成性半金属及び一時的な有機バインダの混合物を含む、請求項1に記載の方法。
- セラミック材料を更に含む、請求項2に記載の方法。
- 前記顆粒はダイヤモンド及び炭化物形成性金属又は炭化物形成性半金属、セラミック材料及び一時的な有機バインダの混合物を含む、請求項1に記載の方法。
- 前記顆粒は立方晶窒化ホウ素及びアルミニウムのポリエチレングリコールバインダ中の混合物を含む、請求項1に記載の方法。
- 前記封じ込め粉末は高圧高温焼結プロセスの間の圧力の均一な分散を可能とするために、硬質グリーンボディを包囲する、請求項1に記載の方法。
- 前記封じ込め粉末は粉末化グラファイト、六方晶窒化ホウ素、酸化アルミニウム又はタルクのうちの少なくとも1種である、請求項1に記載の方法。
- 前記封じ込め粉末は高圧高温焼結プロセスの前に硬質グリーンボディ以上の相対密度を有する、請求項1に記載の方法。
- 前記硬質グリーンボディを含む封じ込め手段は少なくとも1.35GPaの圧力及び少なくとも1080℃の温度で焼結される、請求項1に記載の方法。
- エタノール−水混合物中のポリエチレングリコールのバインダと、立方晶窒化ホウ素及びアルミニウムの粉末及び分散剤とを混合し、スラリーを形成すること、
該スラリーを噴霧乾燥して、顆粒を形成すること、
該顆粒を圧縮して、軟質グリーンボディを形成すること、
該軟質グリーンボディを炉内で脱バインダしそして予備焼結して、硬質グリーンボディを形成すること、
該硬質グリーンボディをグラファイト粉末中に埋め込み、そして該グラファイト粉末を圧縮して、セルを形成すること、
該セルを高圧高温下で焼結すること、及び、
該セルから封じ込め粉末を取り出し、1つ以上のニアネットボディを現すこと、
を含む、ニアネット超硬材料体の製造方法。 - ダイヤモンド及び/又は立方晶窒化ホウ素粉末と、金属粉末、半金属粉末、酸化物粉末、炭化物粉末、窒化物粉末、炭窒化物粉末、カルボオキシ窒化物粉末及びホウ化物粉末の群から選択される粉末とを含む粉末、分散剤、バインダ及び流体の混合物から顆粒を調製すること、
該顆粒を圧縮して、画定された形状の軟質グリーンボディを形成すること、
該軟質グリーンボディを炉内で加熱し、硬質グリーンボディを形成すること、
1つ以上の硬質グリーンボディを、該硬質グリーンボディを閉じ込めるための封じ込め手段中に予備形成されたキャビティ―に挿入し、圧力セルを形成すること、
該圧力セルを高圧高温下で焼結すること、及び、
該圧力セルから封じ込め手段を取り出し、1つ以上のニアネットボディを現すこと、
を含む、ニアネット超硬材料体の製造方法。 - 前記粉末が、立方晶窒化ホウ素、ダイヤモンド及びダイヤモンド複合材料の群より選ばれる材料を含む、請求項12に記載の方法。
- 前記顆粒は立方晶窒化ホウ素及びアルミニウムのポリエチレングリコールバインダ中の混合物を含む、請求項12に記載の方法。
- 前記封じ込め手段はグラファイト、焼結サーメット及びそれらの組み合わせの群より選ばれる固体材料を含む、請求項12に記載の方法。
- 焼結サーメット封じ込め手段は、不活性層により硬質グリーンボディから分離される、請求項12に記載の方法。
- 前記不活性層が、マイカ、マイカ箔、hBN又はTiNである、請求項16に記載の方法。
- 硬質グリーンボディを含む前記封じ込め手段は少なくとも1.35GPaの圧力及び少なくとも1080℃の温度で焼結される、請求項12に記載の方法。
- 前記硬質グリーンボディはへこみ、穴、くぼみ、うね、まるみ、面取り、へリックス形状、スクリュー及びそれらの組み合わせの群より選ばれる特徴を含む、請求項12に記載の方法。
- 請求項12に記載の方法を含む、インサートの製造方法。
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CN104159871B (zh) | 2016-09-14 |
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WO2013102184A9 (en) | 2014-09-12 |
RU2014131412A (ru) | 2016-02-20 |
JP2015510546A (ja) | 2015-04-09 |
US20130167447A1 (en) | 2013-07-04 |
KR101946097B1 (ko) | 2019-04-17 |
IN2014KN01373A (ja) | 2015-10-16 |
KR20140116174A (ko) | 2014-10-01 |
CN104159871A (zh) | 2014-11-19 |
EP3406582A1 (en) | 2018-11-28 |
WO2013102184A1 (en) | 2013-07-04 |
US9327385B2 (en) | 2016-05-03 |
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