JP6815574B1 - 炭化タングステン粉末 - Google Patents
炭化タングステン粉末 Download PDFInfo
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- JP6815574B1 JP6815574B1 JP2020551591A JP2020551591A JP6815574B1 JP 6815574 B1 JP6815574 B1 JP 6815574B1 JP 2020551591 A JP2020551591 A JP 2020551591A JP 2020551591 A JP2020551591 A JP 2020551591A JP 6815574 B1 JP6815574 B1 JP 6815574B1
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- tungsten carbide
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- chromium
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- tungsten
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- 239000000843 powder Substances 0.000 title claims abstract description 105
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 239000011651 chromium Substances 0.000 claims abstract description 69
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 67
- 239000013078 crystal Substances 0.000 claims abstract description 57
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052721 tungsten Inorganic materials 0.000 claims description 27
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000002441 X-ray diffraction Methods 0.000 claims description 4
- 230000005469 synchrotron radiation Effects 0.000 claims description 3
- 239000002245 particle Substances 0.000 description 18
- 238000004519 manufacturing process Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 12
- 238000000034 method Methods 0.000 description 10
- 238000002156 mixing Methods 0.000 description 10
- 239000012298 atmosphere Substances 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 239000011812 mixed powder Substances 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 6
- 239000010937 tungsten Substances 0.000 description 6
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000002216 synchrotron radiation X-ray diffraction Methods 0.000 description 5
- 229910001930 tungsten oxide Inorganic materials 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 239000007864 aqueous solution Substances 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
- 230000007547 defect Effects 0.000 description 4
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
- 229910000967 As alloy Inorganic materials 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 230000005465 channeling Effects 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
- 239000011362 coarse particle Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000002904 solvent Substances 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
- 238000001159 Fisher's combined probability test Methods 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229960000846 camphor Drugs 0.000 description 1
- 229930008380 camphor Natural products 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N chromium trioxide Inorganic materials O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 229940117975 chromium trioxide Drugs 0.000 description 1
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 description 1
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 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
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920003196 poly(1,3-dioxolane) Polymers 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910003470 tongbaite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- C01B32/949—Tungsten or molybdenum carbides
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- 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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Abstract
Description
粉体の嵩を小さくでき、ハンドリング性が向上し、かつ、焼結性が向上した炭化タングステン粉末を提供することが求められている。
[本開示の効果]
粉体の嵩を小さくでき、ハンドリング性が向上し、かつ、焼結性が向上した炭化タングステン粉末を提供できる。
最初に本開示の実施態様を列記して説明する。
本開示の炭化タングステン粉末は、複数の炭化タングステン結晶粒を有する結合体を含み、当該結合体内において複数の前記結晶粒間の結晶粒界に前記炭化タングステン結晶粒内よりもクロムの濃度が高いクロム濃化領域を含む。
本開示に係る炭化タングステン粉末の製造方法の一態様は、例えば、タングステン酸化物粉末と、クロム含有溶液と、炭素源粉末と、を準備し、これらを混合し混合粉末を得る第一工程と、混合粉末を水素雰囲気中で熱処理して還元粉を得る第二工程と、還元粉を不活性雰囲気中や水素を含む雰囲気中で第二工程よりも高温で熱処理して炭化タングステン粉末を得る第三工程と、を備える。ここでクロム含有溶液として利用できる化合物としては、塩化クロム、硝酸クロム、硫酸クロム、酢酸クロム、リン酸クロムが挙げられる。
[実施例]
(混合粉末の製造)
タングステン酸化物粉末として平均粒子径2.0μmの三酸化タングステン粉末と、クロム含有溶液として酢酸クロム(和光純薬)と、炭素源粉末として平均粒子径1.0μmの炭素粉末を準備する。酸化タングステン粉末と炭素源粉末を旋回翼式の混合機に投入する一方、酢酸クロムを純水で溶解して所望の濃度に調整する。クロム含有溶液の濃度は当業者で適宜調整可能であるが、ここでは40体積%酢酸クロム水溶液となるよう調整した。混合機で粉末を撹拌しながら、クロム含有溶液を所望のクロム濃度となるように粉末に噴霧し、これらを混合する(第一工程)。ここで使用する混合機は当業者により適宜選択できるが、一例として日本コークス工業社製のヘンシェルミキサーを利用することができる。また旋回翼式以外の方式であってもよい。ここでは混合条件として旋回翼の直径60cm、外周速度1884m/分、混合時間30分としたが、十分な混合が得られれば良く特に限定されるものではない。
(還元粉末の製造)
この混合粉末を水素雰囲気で温度800〜1000℃で還元処理し、タングステンと炭素とクロムを含有する還元粉末とする(第二工程)。本実施例では全ての粉末において、温度900℃大気圧水素フロー下で還元熱処理を行った。
さらに、この還元粉末を内部容積が幅150mmx奥行150mmx高さ75mmのカーボンケースに入れ、不活性雰囲気下、本実施例においては水素雰囲気大気圧フロー下で1000〜1400℃で熱処理して、炭化タングステン粉末を得る(第三工程)。各粉末の熱処理条件は、表1および表2に記載する。
この製造方法により本開示の炭化タングステン粉末が得られる理由は未だ明確でない。しかしながら、これまでの発明者らの検討の結果、(1)酸化タングステン粉末の各粒子にクロムが均一分散され、(2)酸化タングステンの還元により金属タングステン粒子が生成した際、(3)熱処理によりクロムが金属タングステン粒子へ均一固溶し、(4)炭化の際に金属タングステンからクロムが(W,Cr)2Cの形で吐き出され炭化タングステンの結晶粒界に形成(偏析)される、ことで得られていると推察している。
製造した炭化タングステン粉末を、内径200mmの円筒形ボールミル容器に容器内容積の40体積%となるように充填した。同じ容器に直径3mmの超硬合金製ボールを充填した。1次粒子が粉砕されないように時間調整し解砕処理を実施後、各種粉体特性を測定した。その結果を表1および2に示す。本開示においては、粉体断面のSEM(Scanning Electron Microscope)観察による炭化タングステン結晶の結合体の存在同定、またTEMによるクロム濃化領域の同定、放射光X線回折による(W,Cr)2C相の存在同定および炭化タングステン(101)回折強度Aと(W,Cr)2C(321)回折強度Bとの強度比B/A測定、フィッシャー法によるFsss(Fisher sub-sieve sizer)径測定、JIS Z 2512に記載されるタップ密度(TV:Tap Volume)、誘導結合プラズマ(ICP: Inductively Coupled Plasma)による炭化タングステン粉末中のクロム質量濃度を測定する。
次に、炭化タングステン粉末の焼結性を次の手順で確認する。
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)
- 複数の炭化タングステン結晶粒を有する結合体を含み、当該結合体内において複数の前記炭化タングステン結晶粒間の結晶粒界に、前記炭化タングステン結晶粒内よりもクロムの濃度が高いクロム濃化領域を含み、
さらに、(W,Cr) 2 Cで表される化合物を含む、炭化タングステン粉末。 - 前記炭化タングステン結晶粒の平均結晶粒径が0.6μm以下である請求項1に記載の炭化タングステン粉末。
- 炭化タングステン粉末全体に含まれるクロム濃度が0.1質量%以上7.0質量%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。
- 放射光X線回折により測定する炭化タングステン(101)回折強度Aと(W,Cr)2C(321)回折強度Bとの強度比B/Aが、4.00×10−3以上20.00×10−3以下である請求項1から請求項3のいずれか1項に記載の炭化タングステン粉末。
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