JP6815575B1 - 炭化タングステン粉末およびその製造方法 - Google Patents
炭化タングステン粉末およびその製造方法 Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 114
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000011651 chromium Substances 0.000 claims abstract description 64
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 63
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 14
- 239000010937 tungsten Substances 0.000 claims abstract description 14
- 238000004458 analytical method Methods 0.000 claims abstract description 13
- 238000009826 distribution Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims description 29
- 238000002156 mixing Methods 0.000 claims description 15
- 239000011812 mixed powder Substances 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 9
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 4
- 238000010000 carbonizing Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- 238000003763 carbonization Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000005452 bending Methods 0.000 description 4
- WYYQVWLEPYFFLP-UHFFFAOYSA-K chromium(3+);triacetate Chemical compound [Cr+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WYYQVWLEPYFFLP-UHFFFAOYSA-K 0.000 description 4
- 238000012937 correction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000002093 peripheral effect Effects 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 description 2
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 239000003966 growth inhibitor Substances 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000007619 statistical method Methods 0.000 description 2
- 229910003470 tongbaite Inorganic materials 0.000 description 2
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 1
- 229910021555 Chromium Chloride Inorganic materials 0.000 description 1
- 241000723346 Cinnamomum camphora Species 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229960000846 camphor Drugs 0.000 description 1
- 229930008380 camphor Natural products 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 description 1
- 229910000151 chromium(III) phosphate Inorganic materials 0.000 description 1
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 description 1
- IKZBVTPSNGOVRJ-UHFFFAOYSA-K chromium(iii) phosphate Chemical compound [Cr+3].[O-]P([O-])([O-])=O IKZBVTPSNGOVRJ-UHFFFAOYSA-K 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000010187 selection method Methods 0.000 description 1
- 238000012764 semi-quantitative analysis Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/949—Tungsten or molybdenum carbides
-
- 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
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
- B01J6/001—Calcining
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- 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
- C04B35/56—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 carbides or oxycarbides
- C04B35/5607—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 carbides or oxycarbides based on refractory metal carbides
- C04B35/5626—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 carbides or oxycarbides based on refractory metal carbides based on tungsten carbides
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- 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
- C04B35/626—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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- C04B35/626—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
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62695—Granulation or pelletising
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Abstract
Description
超硬合金の製造に好適な炭化タングステン粉末が求められていた。
[本開示の効果]
本開示によれば、超硬合金の製造に好適な炭化タングステン粉末を提供することができる。
最初に本開示の実施態様を列記して説明する。
次に本開示の実施例を説明する。なお本実施例は発明の一態様に過ぎず、当業者に自明の範囲で変更可能であることは言うまでもない。
(1)粉末外観に対するSEM/EDS分析
まず観察ホルダ上にカーボン両面粘着テープなどを利用して、炭化タングステン粒子の集合体である炭化タングステン粉末を固定する。これをSEM内に挿入し、加速電圧15kVで観察する。使用するSEMおよびEDS検出器のタイプは特に限定されない。本実施例においてはBRUKER製のXFlash Detectorを用いて分析する。観察倍率は対象の炭化タングステン粒度に合わせて選択する。例えば平均粒子径が0.5μmであれば、3000倍程度が好適である。この視野に対し、無作為に所定の数以上、望ましくは、炭化タングステン粉末の100箇所以上の解析点からEDSプロファイルを採取する。粒子の選択手順については無作為であれば特に限定されない。例えば、格子間距離1.5μm程度の10点×10点正方格子メッシュを解析点とする。100個の解析点から機械的にEDSプロファイルを取得することができる。本実施例では格子間距離2.0μmの12点×9点正方格子メッシュを解析点とし、108(12×9)点において炭化タングステン粒子からEDSプロファイルを取得する。
(2)クロム濃度の標準偏差解析
上記の手法を用いて測定したタングステンおよびクロムの濃度より、既知の表計算ソフト等を用いて統計解析し、炭化タングステン粉末中のクロム濃度の標準偏差を得る。既知の表計算ソフトの一例として、Microsoft社製のExcelを用いることができる。より具体的には、Excel中のSTDEV.P関数を用いることで、炭化タングステン粉末中のクロム濃度の標準偏差が求まる。
本開示においては、以下の手順で超硬合金の均質性を評価した。
この乾燥粉末にバインダーとして樟脳を2質量%添加して150μmメッシュの篩を通し、造粒粉を作製する。
Claims (4)
- 炭化タングステンを主成分とすると共にクロムを含有する炭化タングステン粉末であって、
前記炭化タングステン粉末をSEM観察した視野から無作為に選択した100以上の解析点においてタングステンとクロムの質量濃度を測定したとき、タングステンとクロムの合計濃度に対するクロム濃度の割合を百分率で表したときの分布の標準偏差σが0.5以下である炭化タングステン粉末。 - 前記炭化タングステン粉末全体に含まれるタングステンとクロムの合計濃度に対するクロム濃度の割合が、0.1質量%以上7.0質量%以下である請求項1に記載の炭化タングステン粉末。
- 前記炭化タングステン粉末の平均粒子径が1.0μm以下である請求項1または請求項2に記載の炭化タングステン粉末。
- タングステン酸化物とクロム含有溶液とを混合して撹拌しながら乾燥し混合乾燥粉を得る工程と、
前記乾燥粉を大気雰囲気で仮焼し仮焼粉を得る工程と、
前記仮焼粉と炭素源粉末とを混合して混合粉を得る工程と、
前記混合粉を水素ガスを含有する雰囲気で熱処理して還元、および温度1000℃以上で炭化し炭化タングステン粉末を得る工程と、を備える炭化タングステン粉末の製造方法。
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US (1) | US11396451B2 (ja) |
EP (1) | EP3971136B1 (ja) |
JP (1) | JP6815575B1 (ja) |
KR (1) | KR20220007062A (ja) |
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Citations (2)
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JP2005060224A (ja) * | 2003-08-12 | 2005-03-10 | Sandvik Ab | サブミクロンの超硬合金を作製する方法 |
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