JP2005097112A - タングステン−銅複合酸化物粉末 - Google Patents
タングステン−銅複合酸化物粉末 Download PDFInfo
- Publication number
- JP2005097112A JP2005097112A JP2004310838A JP2004310838A JP2005097112A JP 2005097112 A JP2005097112 A JP 2005097112A JP 2004310838 A JP2004310838 A JP 2004310838A JP 2004310838 A JP2004310838 A JP 2004310838A JP 2005097112 A JP2005097112 A JP 2005097112A
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- JP
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- Prior art keywords
- copper
- tungsten
- composite oxide
- powder
- phase
- 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.)
- Granted
Links
- 239000000843 powder Substances 0.000 title claims abstract description 123
- 239000002131 composite material Substances 0.000 title claims abstract description 117
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 title description 6
- 239000010949 copper Substances 0.000 claims abstract description 292
- 229910052802 copper Inorganic materials 0.000 claims abstract description 153
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 152
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 115
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 103
- 239000010937 tungsten Substances 0.000 claims abstract description 96
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims abstract description 16
- OQFRENMCLHGPRB-UHFFFAOYSA-N copper;dioxido(dioxo)tungsten Chemical compound [Cu+2].[O-][W]([O-])(=O)=O OQFRENMCLHGPRB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 90
- 239000001257 hydrogen Substances 0.000 claims description 25
- 229910052739 hydrogen Inorganic materials 0.000 claims description 25
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 23
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- 229910001956 copper hydroxide Inorganic materials 0.000 claims description 2
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims description 2
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims description 2
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- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 description 5
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
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- GDXHBFHOEYVPED-UHFFFAOYSA-N 1-(2-butoxyethoxy)butane Chemical compound CCCCOCCOCCCC GDXHBFHOEYVPED-UHFFFAOYSA-N 0.000 description 1
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
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- ALKZAGKDWUSJED-UHFFFAOYSA-N dinuclear copper ion Chemical compound [Cu].[Cu] ALKZAGKDWUSJED-UHFFFAOYSA-N 0.000 description 1
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- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
- C04B41/5133—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal with a composition mainly composed of one or more of the refractory metals
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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- C04B41/88—Metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
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- C22C1/04—Making non-ferrous alloys by powder metallurgy
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- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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- H—ELECTRICITY
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Abstract
【解決手段】 タングステン酸銅相及び三酸化タングステン相を有する個々の粒子を含み、三酸化タングステン相は主に個々の粒子の表面に存在するW−Cu複合酸化物粉末を提供する。タングステン被覆銅複合粉末をプレスしかつ焼結して銅ブリードアウトを経験しないでW相及びCu相の均一な分布を有するW−Cuプソイドアロイ品にしても或はエレクトロニクス産業用セラミック金属被覆において使用してもよい。
【選択図】 なし
Description
これより、W−Cuプソイドアロイを液相焼結する間、焼結品におけるW及びCu相の均質な分布をもたらしながら、銅ブリードアウトを生じさせないことが有利である。
発明の別の目的は、高い電気的及び熱的伝導性を有するW−Cuプソイドアロイを作製するのに用いることができるW−Cu複合粉末を製造するにある。
発明のそれ以上の目的は、銅ブリードアウト無しで理論的な密度近くにプレス及び焼結することができるW−Cu複合粉末を製造するにある。
発明のなおそれ以上の目的は、高い寸法調節度を有する焼結品を製造するのに用いることができるW−Cu複合粉末を製造するにある。
発明の別の目的に従えば、タングステン酸銅相及び三酸化タングステン相を有する個々の粒子を含み、三酸化タングステン相は主に個々の粒子の表面に存在するW−Cu複合酸化物粉末を提供する。
発明のなおそれ以上の目的に従えば、タングステン領域及び銅領域を有するミクロ構造断面を有し、タングステン領域のサイズが約5μmよりも小さくかつ銅領域のサイズが約10μmよりも小さいW−Cuプソイドアロイを提供する。
いくつかの要因が、サブミクロンW−Cu粉末システムの固体状態(1083℃−銅の融点よりも低い)及び液相(銅の融点よりも高い)焼結挙動に影響を与える。圧縮した超耐熱性金属粉末は、固体状態焼結の間(液相の不存在において)相当のミクロ構造的変化及び収縮を受ける。サブミクロン粒径粉末は、超耐熱性金属の融点(Tm)よりもずっと低い温度(T)において有効に再結晶化しかつ焼結する(数1)。
組成CuWO4+0.958WO3を有するW−Cu複合酸化物粉末を、(1)Cu2O+沈殿させたAPT(角張った粒子形態学)及び(2)Cu2O+スプレー乾燥させたAMT(球形の粒子形態学)から合成した。APT及びAMTの両方の粉末を複合酸化物粒子凝集物に転化させ、これらはAPT及びAMTの出発粒子と同形であった。複合酸化物を合成する間に、亜酸化銅の粒子は全く消失した。Cu2Oの出発形態学が複合酸化物粉末の形態学に及ぼす作用を確認することは可能でなかった。W−Cu複合酸化物の各々の粒子を形成する小さい、大部分サブミクロンのグレインは、WO3グレインが固体状態反応についての拡散境界を概略することを示唆する。反応機構は、酸化銅の可動性分子が拡散してWO3グレインの中に入ることからなると考えられる。W−Cu複合酸化物形態学を、合成において用いるタングステン酸アンモニウムの形態学を変えることによって制御することができることを、酸化物の水素還元の速度論及び共還元される(co−reduced)W−Cu複合粉末の形態学に影響を与えるのに用いることができる。
上記のW−Cu複合酸化物混合物、CuWO4+nWO3(式中、n>0)から造った共還元されたW−Cu複合粉末は、新しく還元されたタングステン粉末の色の特徴である灰色を示す。銅の存在する徴候は観測されない。これは、銅相がタングステン相によって実質的に被包されているW−Cuプソイドアロイ粒子の形成に一致する。
W−Cu複合粉末の大きな表面積は、粉末コンパクトにおける酸素含量を増大させる。タングステン−銅界面上の表面酸化物は、連続したW−Cu構造を有する稠密なプソイドアロイを製造する際に有意の問題を提起する。酸素飽和された銅は、1100°〜1200℃でタングステンを湿潤させないことが立証された。酸素の存在しない銅もまた、タングステン−銅界面上のWO3又は[WO2(OH)2]の形態の表面酸化物を有するタングステンを湿潤させない。W−Cu粉末コンパクトから酸素を除くことは、プソイドアロイを製造する際に根本的な問題を提起する。この問題は、銅の「水素病」及び酸素へのタングステンの高い親和性によって複雑にされる。
未粉砕のD50 − 6.4〜12.6μm
ロッド粉砕したD50− 1.8〜2.6μm
BET −0.55〜0.75m2/g
O2 − 800〜1300ppm。
前に解凝集しない還元されたままの粉末をプレスして上記の通りの丸いサンプルにした。焼結サイクルは、450、850、950、1100℃及びその銅含量をベースにしたアロイ稠密化温度(表10)の内の一つにおける1時間の期間の等温保持からなるものであった:
セラミック金属被覆はエレクトロニクスにおいて最も重要かつ精密な作業の内の一つである。それは、金属層を強くかつ空密の両方であるセラミック対金属接合によってセラミック表面上に形成することからなる。金属被覆したセラミック表面は、エレクトロニック技術においてセラミック対金属及びセラミック対セラミック接続のために並びに配線導体層(路)のために使用される。金属被覆したセラミックは、金属被覆用ペーストを焼結又は未焼結のセラミック基材(ほとんどアルミナ又はベリリア)に塗布しかつペーストを焼成して接着性金属被覆領域を生じることによって製造する。ペーストを「未加工の」(未焼結の)セラミックと共に共焼成することは、それがセラミックを予備焼成することを排除しかつ一層良好な品質の金属被覆を生じるので、経済的に有利である。数多くのペースト配合物及び金属被覆技術が、米国特許第3,620,799号、同4,493,789号及び同4,799,958号に開示された。
Claims (14)
- タングステン酸銅相及び三酸化タングステン相を有する個々の粒子を含み、三酸化タングステン相は主に個々の粒子の表面に存在するW−Cu複合酸化物粉末。
- タングステン酸アンモニウムと銅の酸化物又は水酸化物とを反応させることによって造られる請求項1の複合酸化物粉末。
- メタタングステン酸アンモニウムと亜酸化銅とを反応させることによって造られる請求項2の複合酸化物粉末。
- 個々の粒子がタングステン酸アンモニウムに関して同形である請求項2の複合酸化物粉末。
- 粒径が5〜25μである請求項1の複合酸化物粉末。
- 組成CuWO4+nWO3(式中、n>0)を有する請求項1の複合酸化物粉末。
- nが0.035〜15である請求項6の複合酸化物粉末。
- CuWO4相及びWO3相を含むW−Cu複合酸化物粉末であって、X線回折によって測定する通りのWO3相対CuWO4相の比が、W−Cu複合酸化物粉末と同じ相の割合を有するCuWO4相とWO3相との機械的ブレンドのX線回折によって測定する通りの相の比に比べて大きいW−Cu複合酸化物粉末。
- 請求項8の複合酸化物粉末を還元させてタングステン被覆銅複合酸化物粉末を形成することを含むタングステン被覆銅複合粉末の製造方法。
- 複合酸化物粉末を水素中700°〜850℃において還元させてタングステン被覆銅複合粉末を形成する請求項9の方法。
- タングステン被覆銅複合粉末を形成する時間が1〜2時間である請求項10の方法。
- 水素を速度20〜300cm/秒で流す請求項10の方法。
- タングステン被覆銅粉末を、還元させた後に、窒素中で不動態化させる請求項9の方法。
- タングステン被覆銅粉末を粉砕しかつスプレー乾燥させて流動性粉末を形成する請求項9の方法。
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Cited By (5)
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JP2013076163A (ja) * | 2011-09-15 | 2013-04-25 | Mitsubishi Materials Corp | スパッタリングターゲットおよびその製造方法 |
CN104445414A (zh) * | 2014-11-02 | 2015-03-25 | 河北联合大学 | 两种纳米钨酸铜抗菌粉体的制备新方法 |
CN104671283A (zh) * | 2014-12-29 | 2015-06-03 | 河北联合大学 | 超声波法及超声-熔盐法合成钼酸铜纳米片抗菌粉体 |
JP2020015020A (ja) * | 2018-07-27 | 2020-01-30 | 国立研究開発法人物質・材料研究機構 | 触媒、触媒の製造方法、触媒担持担体、分解方法、水素の製造方法、及び、担体 |
JP7093549B2 (ja) | 2018-07-27 | 2022-06-30 | 国立研究開発法人物質・材料研究機構 | 触媒、触媒の製造方法、触媒担持担体、分解方法、水素の製造方法、及び、担体 |
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CA2190550C (en) | 2008-09-16 |
EP0774315B1 (en) | 2004-07-21 |
HUP9603166A3 (en) | 1999-07-28 |
CN1329956A (zh) | 2002-01-09 |
CN1160773A (zh) | 1997-10-01 |
JPH09143501A (ja) | 1997-06-03 |
US5956560A (en) | 1999-09-21 |
EP0774315A2 (en) | 1997-05-21 |
DE69635911T2 (de) | 2006-08-17 |
DE69635911D1 (de) | 2006-05-11 |
CN1329955A (zh) | 2002-01-09 |
JP3766486B2 (ja) | 2006-04-12 |
EP1118403A2 (en) | 2001-07-25 |
EP1118403A3 (en) | 2005-01-05 |
CN1068909C (zh) | 2001-07-25 |
EP1118403B1 (en) | 2006-03-15 |
CA2190550A1 (en) | 1997-05-18 |
CN1192837C (zh) | 2005-03-16 |
DE69632941T2 (de) | 2004-12-16 |
EP0774315A3 (en) | 1998-07-08 |
JP4181105B2 (ja) | 2008-11-12 |
HU221509B (en) | 2002-10-28 |
DE69632941D1 (de) | 2004-08-26 |
CN1191904C (zh) | 2005-03-09 |
HU9603166D0 (en) | 1997-01-28 |
US6103392A (en) | 2000-08-15 |
HUP9603166A2 (en) | 1997-07-28 |
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