JP5896968B2 - 炭化ジルコニウムのインゴット及び粉末の製造方法 - Google Patents
炭化ジルコニウムのインゴット及び粉末の製造方法 Download PDFInfo
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- JP5896968B2 JP5896968B2 JP2013196717A JP2013196717A JP5896968B2 JP 5896968 B2 JP5896968 B2 JP 5896968B2 JP 2013196717 A JP2013196717 A JP 2013196717A JP 2013196717 A JP2013196717 A JP 2013196717A JP 5896968 B2 JP5896968 B2 JP 5896968B2
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- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 title claims description 92
- 229910026551 ZrC Inorganic materials 0.000 title claims description 91
- 239000000843 powder Substances 0.000 title claims description 39
- 238000004519 manufacturing process Methods 0.000 title claims description 35
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 50
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 48
- 229910052799 carbon Inorganic materials 0.000 claims description 42
- 238000000034 method Methods 0.000 claims description 34
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 34
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 34
- 238000002844 melting Methods 0.000 claims description 30
- 230000008018 melting Effects 0.000 claims description 30
- 229910052786 argon Inorganic materials 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 17
- 239000000155 melt Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 239000008187 granular material Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- GEIAQOFPUVMAGM-UHFFFAOYSA-N Oxozirconium Chemical compound [Zr]=O GEIAQOFPUVMAGM-UHFFFAOYSA-N 0.000 description 10
- 239000012535 impurity Substances 0.000 description 10
- 239000002245 particle Substances 0.000 description 10
- 239000002994 raw material Substances 0.000 description 9
- 239000007858 starting material Substances 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- 239000001569 carbon dioxide Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000005469 granulation Methods 0.000 description 5
- 230000003179 granulation Effects 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000001307 helium Substances 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052754 neon Inorganic materials 0.000 description 4
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 230000007423 decrease Effects 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
- 239000011261 inert gas Substances 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 description 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000005049 combustion synthesis Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000010583 slow cooling Methods 0.000 description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 2
- 229910052845 zircon Inorganic materials 0.000 description 2
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 2
- 229910006501 ZrSiO Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Description
1. 下記工程を有し,得られる炭化ジルコニウムのインゴットの大きさが50mm以上であり,密度が5.7g/cm3以上であり,ビッカース硬度が1500以上であることを特徴とする炭化ジルコニウムのインゴットの製造方法:
(1)酸化ジルコニウムと炭素とを混合して混合物を得る工程であって,前記混合物中の酸化ジルコニウムに対する炭素の質量比率が15〜20質量%である工程1,
(2)前記混合物を造粒して造粒物を得る工程2,
(3)アーク式電融炉をアルゴンガスで満たしてプラズマを発生させることにより当該炉内を炭化ジルコニウムの融点以上の温度に保持することにより,前記造粒物を溶融して溶融物を得る工程3,
(4)前記溶融物を徐冷して炭化ジルコニウムのインゴットを得る工程4。
2. 得られる炭化ジルコニウムのインゴットの大きさが80mm以上であり,密度が6.0g/cm3以上であり,ビッカース硬度が2000以上である,上記項1に記載の製造方法。
3. 上記項1又は2に記載の製造方法により得られる炭化ジルコニウムのインゴットを粉砕することを特徴とする炭化ジルコニウム粉末の製造方法。
本発明の炭化ジルコニウムのインゴットの製造方法は,
(1)酸化ジルコニウムと炭素とを混合して混合物を得る工程であって,前記混合物中の酸化ジルコニウムに対する炭素の質量比率が15〜20質量%である工程1,
(2)前記混合物を造粒して造粒物を得る工程2,
(3)前記造粒物をアルゴンプラズマにより溶融する工程3,
(4)前記溶融物を徐冷して炭化ジルコニウムのインゴットを得る工程4,
を有し,得られる炭化ジルコニウムのインゴットの大きさが50mm以上であり,密度が5.7g/cm3以上であり,ビッカース硬度が1500以上であることを特徴とする。
(工程1)
工程1は,酸化ジルコニウムと炭素とを混合して混合物を得る。本発明では,前記混合物中の酸化ジルコニウムに対する炭素の質量比率は15〜20質量%に設定する。
(工程2)
工程2では,前記工程1で調製した混合物を造粒して造粒物を得る。
(工程3)
工程3では,前記工程2で得た造粒物をアルゴンプラズマにより溶融する。
(工程4)
工程4では,工程3で得た溶融物を徐冷して炭化ジルコニウムのインゴットを得る。
本発明の炭化ジルコニウム粉末の製造方法は,上記インゴットの製造方法により得られた炭化ジルコニウムのインゴットを粉砕することを特徴とする。前記の通り,本発明のインゴットは従来品と比較して高密度及び高硬度であるため,当該インゴットを粉砕することにより得られる本発明の炭化ジルコニウム粉末も高密度及び高硬度の特性を有する。
酸化ジルコニウム粉末として純度99.5質量%,平均粒子径3μm(第一稀元素化学工業株式会社製)を用いた。また,炭素粉末としてファインパウダーSGP(SECカーボン株式会社製)を用いた。
造粒物を20kg使用し,また印加時間を電力110kwhで2時間とする以外は実施例1と同じ方法で炭化ジルコニウムのインゴットを得た。
酸化ジルコニウム粉末84kg,炭素粉末12kgを実施例1と同様に造粒処理し,造粒物を得た(C/ZrO2混合比率:14.3%)。
酸化ジルコニウム粉末84kg,炭素粉末18kgを実施例1と同様に造粒処理し,造粒体を得た(C/ZrO2混合比率:21.4%)。
酸化ジルコニウム粉末84kg,炭素粉末14.6kgを実施例1と同様に造粒処理し,造粒体を得た(C/ZrO2混合比率:17.4%)。
酸化ジルコニウム粉末84kg,炭素粉末14.6kgを造粒処理せず(C/ZrO2混合比率:17.4%),電融工程に供した。電融は実施例1と同条件とした。
Claims (3)
- 下記工程を有し,得られる炭化ジルコニウムのインゴットの大きさが50mm以上であり,密度が5.7g/cm3以上であり,ビッカース硬度が1500以上であることを特徴とする炭化ジルコニウムのインゴットの製造方法:
(1)酸化ジルコニウムと炭素とを混合して混合物を得る工程であって,前記混合物中の酸化ジルコニウムに対する炭素の質量比率が15〜20質量%である工程1,
(2)前記混合物を造粒して造粒物を得る工程2,
(3)アーク式電融炉をアルゴンガスで満たしてプラズマを発生させることにより当該炉内を炭化ジルコニウムの融点以上の温度に保持することにより,前記造粒物を溶融して溶融物を得る工程3,
(4)前記溶融物を徐冷して炭化ジルコニウムのインゴットを得る工程4。 - 得られる炭化ジルコニウムのインゴットの大きさが80mm以上であり,密度が6.0g/cm3以上であり,ビッカース硬度が2000以上である,請求項1に記載の製造方法。
- 請求項1又は2に記載の製造方法により得られる炭化ジルコニウムのインゴットを粉砕することを特徴とする炭化ジルコニウム粉末の製造方法。
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JP2013196717A JP5896968B2 (ja) | 2013-09-24 | 2013-09-24 | 炭化ジルコニウムのインゴット及び粉末の製造方法 |
US15/022,612 US20160229698A1 (en) | 2013-09-24 | 2014-07-04 | Method for producing ingot and powder of zirconium carbide |
EP14847888.6A EP3029009A4 (en) | 2013-09-24 | 2014-07-04 | Method for producing ingot and powder of zirconium carbide |
CN201480050498.0A CN105555737A (zh) | 2013-09-24 | 2014-07-04 | 碳化锆的锭及粉末的制造方法 |
PCT/JP2014/067879 WO2015045547A1 (ja) | 2013-09-24 | 2014-07-04 | 炭化ジルコニウムのインゴット及び粉末の製造方法 |
KR1020167006295A KR20160060039A (ko) | 2013-09-24 | 2014-07-04 | 탄화 지르코늄 잉곳 및 분말의 제조방법 |
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