WO2006038406A1 - 高純度ZrB2粉末及びその製造方法 - Google Patents
高純度ZrB2粉末及びその製造方法 Download PDFInfo
- Publication number
- WO2006038406A1 WO2006038406A1 PCT/JP2005/016214 JP2005016214W WO2006038406A1 WO 2006038406 A1 WO2006038406 A1 WO 2006038406A1 JP 2005016214 W JP2005016214 W JP 2005016214W WO 2006038406 A1 WO2006038406 A1 WO 2006038406A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- powder
- purity
- zrb
- zrb2
- single crystal
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/04—Metal borides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
- C30B13/16—Heating of the molten zone
- C30B13/20—Heating of the molten zone by induction, e.g. hot wire technique
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12014—All metal or with adjacent metals having metal particles
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
- Y10T428/12535—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.] with additional, spatially distinct nonmetal component
- Y10T428/12576—Boride, carbide or nitride component
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
Definitions
- the present invention relates to a high-purity ZrB powder having a purity of 99.9 wt% or more and a method for producing the same.
- ZrB zirconium diboride
- the crystal structure of ZrB is such that hexagonal network boron layers and zirconium metal layers overlap alternately.
- this single crystal substrate is generally manufactured by high frequency induction heating FZ method (floating zone melting method)! (See Patent Document 1).
- Patent Document 1 ZrB powder is mainly decomposed by thermal decomposition.
- Non-Patent Document 2 there is a paper on the production of high-purity ZrB powder (see Non-Patent Document 2).
- Non-Patent Document 1 The Institute of Electronics, Information and Communication Engineers, IEICE Technical Report, Shigeru Otani, “Current Status of ZrB2 Substrate Fabrication”, pages 17-19, vol.102, No.114 (2002)
- Non-Patent Document 2 China Building Materials Academy, Beijing 100024, China (China), H. ZHAO and 2 other authors PREPARATION OF ZIRCONIUM BORIDE POWDER ”page 5
- Patent Document 1 Japanese Patent Laid-Open No. 63-297273
- Patent Document 2 Japanese Patent Laid-Open No. 63-282165
- the present invention relates to the production of a ZrB single crystal substrate by the high frequency induction heating FZ method (floating zone melting method).
- the purity of the ZrB powder for sintering, which is required for manufacturing, is set to 99.9 wt% or higher.
- High-purity ZrB powder characterized by a purity of 99.9 wt% or more, excluding impurities of C and gas components
- a method for producing high-purity ZrB powder comprising a step of obtaining a powder.
- the high purity ZrB powder of the present invention and the production method thereof have a purity of 99.9 wt% or more.
- High-purity ZrB powder can be obtained, and this high-purity ZrB powder is sintered and sintered.
- a ZrB single crystal with melt force is produced by using the ligature (rod) by the FZ method (floating zone melting method).
- ZrB has a high melting point of 3220 ° C.
- impurities C, ZrC, HfC, TiC, etc.
- ZrB itself is primarily used for cutting tools and heat engine parts.
- the present situation is that improvement of purity has not been regarded as a problem.
- the contents of impurities Hf and Ti contained in the high-purity ZrB powder are adjusted.
- Respectively, can be less than 0.1 wt%.
- the contents of Fe, Cr, and Nb as impurities can each be 0.05 wt% or less, and the content of C as an impurity can be 0.1 wt% or less.
- the reduction of the C content is effective in reducing carbides such as ZrC, HfC, and TiC that can be achieved with only C.
- the FZ method floating zone melting method
- a dense and uniform sintered body can be obtained.
- Electron beam melting 'forging to produce ingots with a purity of 99.9 wt% or more.
- this is cut into chips, and the chips are hydrogenated to ZrH. This is pulverized, but Z
- rH is fragile and very easy to pulverize.
- Finely pulverized ZrH is dehydrogenated into Zr powder. According to this, a net of more than 99.9 wt%
- this Zr powder is oxidized at high temperature (heated to 500-900 ° C) and in an oxygen atmosphere to make ZrO fine powder. Then, this ZrO fine powder is mixed with B (boron) powder, and ZrO is mixed with B
- Zr powder having a purity of 99.99 wt% was obtained. Furthermore, this Zr powder is heated to 800 ° C and oxidized in an oxygen atmosphere to
- O is directly synthesized (reduced) with B, and 99.
- An ingot was manufactured by high-frequency induction heating FZ method (floating zone melting method). As a result, a large single crystal ingot with few impurities was obtained.
- the single crystal thus obtained is mirror-polished and etched to measure the size of the single crystal, and the number of pit defects and pores of 1 ⁇ m or more present in the crystal is measured. did.
- the results are shown in Table 1.
- an ingot having a purity of 99.9 wt% or more was produced by e-beam melting and forging.
- this Zr powder is heated to 800 ° C and oxidized in an oxygen atmosphere to
- this ZrO fine powder is mixed with B (boron) having a low C content and 99 wt% purity.
- ZrO is directly synthesized (reduced) by B, and 99.9 wt% or more excluding C and gas components
- Table 1 shows the content of each impurity produced in Example 2.
- the single crystal thus obtained is mirror-polished and etched to measure the size of the single crystal, and the number of pit defects and pores of 1 ⁇ m or more present in the crystal is measured. did.
- the results are shown in Table 1.
- High-Hf content! 2N level Zr sponge raw material is used for electron beam melting.
- the ingot was manufactured by forging and having a purity of 99.9 wt%.
- this Zr powder is heated to 800 ° C and oxidized in an oxygen atmosphere to
- O is synthesized directly (reduced) by B, and 99.9 wt% level pure without C and gas components
- An ingot was manufactured by high-frequency induction heating FZ method (floating zone melting method). As a result, a large single crystal ingot with few impurities was obtained.
- the single crystal thus obtained is mirror-polished and etched to measure the size of the single crystal, and the number of pit defects and pores of 1 ⁇ m or more present in the crystal is measured. did.
- the results are shown in Table 1.
- Table 1 shows the abundance.
- the single crystal thus obtained was mirror-polished and etched to measure the size of the single crystal, and the number of pit defects and the number of pores of 1 IX m or more present in the crystal was measured. .
- the results are shown in Table 1.
- Zr scrap with a high Hf content and a purity of 95 wt% is hydrogenated to ZrH.
- this Zr powder is heated to 800 ° C and oxidized in an oxygen atmosphere to
- this ZrO fine powder is mixed with B (boron) having a purity of 95 wt%, and ZrO
- Table 2 shows the content of each impurity produced in Comparative Example 1.
- An ingot was produced by high-frequency induction heating FZ method (floating zone melting method), but the crystal became fine, and it was difficult to obtain a single crystal ingot. In addition, there were so many defects and pores that measurement was impossible.
- FZ method floating zone melting method
- a Zr sponge having a purity of 99.9 wt% with a slightly higher C and Hf content was used for hydrogenation and further dehydrogenation to obtain a Zr powder having a purity of 99.9 wt%. This was mixed with 95% pure B powder and synthesized directly to obtain ZrB powder. Content of each impurity produced in Comparative Example 3
- the ingot was manufactured by high-frequency induction heating FZ method (floating zone melting method), but the crystal became fine, and it was powerful that a large single crystal ingot could not be obtained. At this point, the defect density and pore density were finally measured, but they were 4 x 10 7 pieces Zcm 2 and 53 pieces, respectively.
- a Zr sponge having a purity of 99.9 wt% with a low Hf content was hydrogenated, further dehydrogenated, and oxidized to obtain a ZrO powder having a purity of 99.9 wt%.
- the ingot was manufactured by high-frequency induction heating FZ method (floating zone melting method), but the crystal became fine, and it was powerful that a large single crystal ingot could not be obtained.
- the defect density and the pore density could be measured, but they were 6 ⁇ 10 5 pieces Zcm 2 and 15 pieces, respectively.
- the purity of the ZrB powder for sintering can be 99.9 wt% or more.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2006539192A JP4685023B2 (ja) | 2004-10-07 | 2005-09-05 | 高純度ZrB2粉末及びその製造方法 |
US11/576,577 US8585995B2 (en) | 2004-10-07 | 2005-09-05 | High purity ZrB2 powder and manufacturing method thereof |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2004-294873 | 2004-10-07 | ||
JP2004294873 | 2004-10-07 |
Publications (1)
Publication Number | Publication Date |
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WO2006038406A1 true WO2006038406A1 (ja) | 2006-04-13 |
Family
ID=36142489
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2005/016214 WO2006038406A1 (ja) | 2004-10-07 | 2005-09-05 | 高純度ZrB2粉末及びその製造方法 |
Country Status (4)
Country | Link |
---|---|
US (1) | US8585995B2 (ja) |
JP (3) | JP4685023B2 (ja) |
TW (1) | TWI265159B (ja) |
WO (1) | WO2006038406A1 (ja) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2011063486A (ja) * | 2009-09-18 | 2011-03-31 | Sumitomo Osaka Cement Co Ltd | 高純度金属ホウ化物粒子の製造方法及びその方法により得られた高純度金属ホウ化物粒子 |
CN102050628A (zh) * | 2011-01-04 | 2011-05-11 | 上海大学 | 一种制备超细二硼化锆粉体的方法 |
JP2012131674A (ja) * | 2010-12-24 | 2012-07-12 | National Institute For Materials Science | 二ホウ化ジルコニウム粉末及びその合成方法 |
CN105197954A (zh) * | 2015-09-29 | 2015-12-30 | 山东理工大学 | 棒状硼化锆粉体的合成方法 |
Families Citing this family (4)
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CN102417188B (zh) * | 2011-08-30 | 2013-10-16 | 中国科学院上海硅酸盐研究所 | 一种低氧含量亚微米级过渡金属硼化物粉体的制备方法 |
CN105084901A (zh) * | 2015-06-29 | 2015-11-25 | 中国矿业大学 | 一种制备硼化锆(ZrB2)陶瓷先驱体的新方法 |
CN105645422B (zh) * | 2016-01-06 | 2018-06-15 | 昆明理工大学 | 一种液相法制备球形超细硼化锆粉体的工艺 |
CN108585889B (zh) * | 2018-04-28 | 2021-04-16 | 武汉科技大学 | 一种棒状硼化锆-片状碳化硅单晶复合粉体及其制备方法 |
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JPH07277734A (ja) * | 1994-04-08 | 1995-10-24 | Tosoh Corp | ホウ化ジルコニウム系多孔体 |
JP2004203666A (ja) * | 2002-12-25 | 2004-07-22 | Kyocera Corp | ZrB2単結晶及びその製造方法並びに半導体薄膜用基板 |
JP2005145787A (ja) * | 2003-11-18 | 2005-06-09 | Kyocera Corp | 半導体育成用基板および半導体装置 |
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JPS627673A (ja) * | 1985-06-19 | 1987-01-14 | 旭硝子株式会社 | ZrB↓2系焼結体 |
JPS6395113A (ja) * | 1986-10-13 | 1988-04-26 | Kawasaki Steel Corp | 金属硼化物を主成分とする微粉末の製造方法 |
JPS63282165A (ja) * | 1987-05-11 | 1988-11-18 | Matsushita Electric Ind Co Ltd | 酸化ジルコニウムとホウ化物を含む混合粉末及びそれらを含む複合焼結体の製造方法 |
JPS63297273A (ja) * | 1987-05-29 | 1988-12-05 | Ube Ind Ltd | ZrB↓2焼結体の製造方法 |
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-
2005
- 2005-09-05 WO PCT/JP2005/016214 patent/WO2006038406A1/ja active Application Filing
- 2005-09-05 JP JP2006539192A patent/JP4685023B2/ja not_active Expired - Fee Related
- 2005-09-05 US US11/576,577 patent/US8585995B2/en active Active
- 2005-09-16 TW TW094132010A patent/TWI265159B/zh not_active IP Right Cessation
-
2011
- 2011-01-04 JP JP2011000037A patent/JP2011088819A/ja active Pending
-
2013
- 2013-06-25 JP JP2013132633A patent/JP2013216574A/ja active Pending
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JPH07277734A (ja) * | 1994-04-08 | 1995-10-24 | Tosoh Corp | ホウ化ジルコニウム系多孔体 |
JP2004203666A (ja) * | 2002-12-25 | 2004-07-22 | Kyocera Corp | ZrB2単結晶及びその製造方法並びに半導体薄膜用基板 |
JP2005145787A (ja) * | 2003-11-18 | 2005-06-09 | Kyocera Corp | 半導体育成用基板および半導体装置 |
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Title |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2011063486A (ja) * | 2009-09-18 | 2011-03-31 | Sumitomo Osaka Cement Co Ltd | 高純度金属ホウ化物粒子の製造方法及びその方法により得られた高純度金属ホウ化物粒子 |
JP2012131674A (ja) * | 2010-12-24 | 2012-07-12 | National Institute For Materials Science | 二ホウ化ジルコニウム粉末及びその合成方法 |
CN102050628A (zh) * | 2011-01-04 | 2011-05-11 | 上海大学 | 一种制备超细二硼化锆粉体的方法 |
CN105197954A (zh) * | 2015-09-29 | 2015-12-30 | 山东理工大学 | 棒状硼化锆粉体的合成方法 |
Also Published As
Publication number | Publication date |
---|---|
US8585995B2 (en) | 2013-11-19 |
TWI265159B (en) | 2006-11-01 |
JP2013216574A (ja) | 2013-10-24 |
JP2011088819A (ja) | 2011-05-06 |
JP4685023B2 (ja) | 2011-05-18 |
JPWO2006038406A1 (ja) | 2008-05-15 |
US20080075648A1 (en) | 2008-03-27 |
TW200611885A (en) | 2006-04-16 |
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