WO2021060375A1 - 三酸化モリブデン粉体及びその製造方法 - Google Patents

三酸化モリブデン粉体及びその製造方法 Download PDF

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Publication number
WO2021060375A1
WO2021060375A1 PCT/JP2020/036025 JP2020036025W WO2021060375A1 WO 2021060375 A1 WO2021060375 A1 WO 2021060375A1 JP 2020036025 W JP2020036025 W JP 2020036025W WO 2021060375 A1 WO2021060375 A1 WO 2021060375A1
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WIPO (PCT)
Prior art keywords
molybdenum trioxide
molybdenum
powder
moo
trioxide powder
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.)
Ceased
Application number
PCT/JP2020/036025
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English (en)
French (fr)
Japanese (ja)
Inventor
裕延 沖
佑介 狩野
建軍 袁
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
DIC Corp
Original Assignee
DIC Corp
Dainippon Ink and Chemicals Co Ltd
Priority date (The priority date 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 date listed.)
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Publication date
Application filed by DIC Corp, Dainippon Ink and Chemicals Co Ltd filed Critical DIC Corp
Priority to KR1020227008780A priority Critical patent/KR102813084B1/ko
Priority to JP2021548988A priority patent/JP7056807B2/ja
Priority to EP20867217.0A priority patent/EP4036061A4/en
Priority to US17/762,726 priority patent/US12497303B2/en
Priority to CN202080066677.9A priority patent/CN114430728A/zh
Publication of WO2021060375A1 publication Critical patent/WO2021060375A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/02—Oxides; Hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/06—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/74—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by peak-intensities or a ratio thereof only
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Definitions

  • the present invention includes the following aspects.
  • It is composed of an aggregate of primary particles containing a ⁇ crystal structure of molybdenum trioxide, and the content ratio of MoO 3 measured by fluorescent X-ray (XRF) is 99.6% or more, and the average grain of the primary particles is 99.6% or more.
  • Molybdenum trioxide powder having a diameter of 1 ⁇ m or less.
  • the internal pressure in the firing furnace is not particularly limited and may be positive pressure or reduced pressure. However, from the viewpoint of preferably discharging the molybdenum oxide precursor compound from the firing furnace to the cooling pipe, firing is performed under reduced pressure. It is preferable that this is done in.
  • the specific degree of decompression is preferably ⁇ 5000 to ⁇ 10 Pa, more preferably ⁇ 2000 to ⁇ 20 Pa, and even more preferably ⁇ 1000 to ⁇ 50 Pa. When the degree of decompression is ⁇ 5000 Pa or more, high airtightness and mechanical strength of the firing furnace are not excessively required, and the manufacturing cost can be reduced, which is preferable. On the other hand, when the degree of depressurization is ⁇ 10 Pa or less, clogging of the molybdenum oxide precursor compound at the discharge port of the firing furnace can be prevented, which is preferable.
  • the cooling of the molybdenum trioxide vapor is preferably performed in an air atmosphere.
  • Molybdenum trioxide vapor is cooled in an air atmosphere, by the molybdenum trioxide powder, can be greater than the ratio (I / II) of 1.1, in molybdenum trioxide powder, a MoO 3 Beta crystals are easy to obtain.
  • the powder obtained by cooling the molybdenum trioxide vapor may be fired again at a temperature of 100 ° C. to 320 ° C.
  • the wide area X-ray absorption fine structure (EXAFS) was measured using the molybdenum trioxide powder of Example 1.
  • the extended X-ray absorption fine structure (EXAFS) spectrum of the K-edge of molybdenum is shown in FIG. In the radial distribution function obtained from this spectrum, the ratio (I / II) of the peak intensity I due to Mo-O to the peak intensity II due to Mo-Mo was 2.0.
  • molybdenum trioxide powder of Example 2 was crystal structure analysis by X-ray diffraction (XRD), the peak attributable to ⁇ crystal peaks and MoO 3 attributable to ⁇ crystal of MoO 3 was observed, other No peak was observed.
  • XRD X-ray diffraction
  • Example 3 A molybdenum trioxide powder was produced in the same manner as in Example 1 except that the firing temperature of 1100 ° C. in Example 1 was changed to a firing temperature of 1500 ° C. After firing, 1.0 kg of aluminum oxide, which is a blue powder, and 0.95 kg of molybdenum trioxide powder recovered by the recovery machine 4 were taken out from the sheath.
  • the recovered molybdenum trioxide powder of Example 3 had an average particle size of 120 nm as primary particles, and the content ratio (purity) of molybdenum trioxide (MoO 3) was 99. It was confirmed that it was 6%.
  • Example 5 1 g of the molybdenum trioxide powder of Example 1 was placed in a crucible and fired again at 300 ° C. for 4 hours to obtain the molybdenum trioxide powder of Example 5.
  • the molybdenum trioxide powder of Example 5 has an average particle size of primary particles of 130 nm, and the content ratio (purity) of molybdenum trioxide (MoO 3) is 99.7% as measured by fluorescent X-ray (XRF). It was confirmed that.
  • molybdenum trioxide powder of Example 5 were crystal structure analysis by X-ray diffraction (XRD), the peak attributable to ⁇ crystal peaks and MoO 3 attributable to ⁇ crystal of MoO 3 was observed, other No peak was observed. Next, when the peak intensity ratio ( ⁇ (011) / ⁇ (021)) of the (011) plane of the ⁇ crystal and the (021) plane of the ⁇ crystal was determined, ⁇ (011) / ⁇ (021) was 1.7. there were.
  • molybdenum trioxide powder of Example 7 was crystal structure analysis by X-ray diffraction (XRD), the peak attributable to ⁇ crystal peaks and MoO 3 attributable to ⁇ crystal of MoO 3 was observed, other No peak was observed.
  • XRD X-ray diffraction
  • Example 2 A mixture of 1 kg of transition aluminum oxide (manufactured by Wako Pure Chemical Industries, Ltd., activated alumina, average particle size 45 ⁇ m) and 1 kg of molybdenum trioxide (manufactured by Taiyo Mining Co., Ltd.) in Example 1 is mixed with transition aluminum oxide (sum). Same as in Example 1 except that the mixture was changed to a mixture of 3.0 kg of activated alumina, average particle size 45 ⁇ m) manufactured by Kojunyaku Kogyo Co., Ltd. and 1.0 kg of molybdenum trioxide (manufactured by Taiyo Mining Co., Ltd.). , Molybdenum trioxide powder was produced.
  • molybdenum trioxide powder of Comparative Example 2 was crystal structure analysis by X-ray diffraction (XRD), the peak attributable to ⁇ crystal peaks and MoO 3 attributable to ⁇ crystal of MoO 3 was observed, other No peak was observed. Next, when the peak intensity ratio ( ⁇ (011) / ⁇ (021)) of the (011) plane of the ⁇ crystal and the (021) plane of the ⁇ crystal was determined, ⁇ (011) / ⁇ (021) was 5.0. there were.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Fuel Cell (AREA)
PCT/JP2020/036025 2019-09-24 2020-09-24 三酸化モリブデン粉体及びその製造方法 Ceased WO2021060375A1 (ja)

Priority Applications (5)

Application Number Priority Date Filing Date Title
KR1020227008780A KR102813084B1 (ko) 2019-09-24 2020-09-24 삼산화몰리브덴 분체 및 그 제조 방법
JP2021548988A JP7056807B2 (ja) 2019-09-24 2020-09-24 三酸化モリブデン粉体及びその製造方法
EP20867217.0A EP4036061A4 (en) 2019-09-24 2020-09-24 MOLYBDENUM TRIOXIDE POWDER AND METHOD FOR THE PRODUCTION THEREOF
US17/762,726 US12497303B2 (en) 2019-09-24 2020-09-24 Molybdenum trioxide powder and method for producing same
CN202080066677.9A CN114430728A (zh) 2019-09-24 2020-09-24 三氧化钼粉体及其制造方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2019-172915 2019-09-24
JP2019172915 2019-09-24

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WO2021060375A1 true WO2021060375A1 (ja) 2021-04-01

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US (1) US12497303B2 (https=)
EP (1) EP4036061A4 (https=)
JP (1) JP7056807B2 (https=)
KR (1) KR102813084B1 (https=)
CN (1) CN114430728A (https=)
TW (1) TWI815040B (https=)
WO (1) WO2021060375A1 (https=)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115321598A (zh) * 2022-09-23 2022-11-11 西安稀有金属材料研究院有限公司 低成本、高分散、高孔隙和高纯超细三氧化钼的制备方法
JP7188664B1 (ja) * 2021-03-24 2022-12-13 Dic株式会社 三酸化モリブデン粉体及びその製造方法
JPWO2023013244A1 (https=) * 2021-08-04 2023-02-09
JPWO2024058260A1 (https=) * 2022-09-15 2024-03-21

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CN114833349B (zh) * 2022-07-04 2023-01-31 成都虹波实业股份有限公司 一种低钾大粒度钼粉的制造方法

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JPH01208330A (ja) * 1988-02-12 1989-08-22 Sumitomo Metal Mining Co Ltd 超微粉三酸化モリブデンの製造方法及びその製造装置
JP2004339054A (ja) * 2003-05-15 2004-12-02 Cyprus Amax Minerals Co 酸化モリブデンのナノ粒子を製造するための方法及び装置
CN104495932A (zh) * 2014-11-27 2015-04-08 新疆大学 一种固相化学反应合成纳米三氧化钼的方法
JP2019172915A (ja) 2018-03-29 2019-10-10 住友ベークライト株式会社 電子装置の製造に用いられる仮接着フィルム、電子パッケージ製造用サポート基板および電子パッケージの製造方法

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JP2004339054A (ja) * 2003-05-15 2004-12-02 Cyprus Amax Minerals Co 酸化モリブデンのナノ粒子を製造するための方法及び装置
CN104495932A (zh) * 2014-11-27 2015-04-08 新疆大学 一种固相化学反应合成纳米三氧化钼的方法
JP2019172915A (ja) 2018-03-29 2019-10-10 住友ベークライト株式会社 電子装置の製造に用いられる仮接着フィルム、電子パッケージ製造用サポート基板および電子パッケージの製造方法

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Title
See also references of EP4036061A4
WANG, LU ET AL.: "Preparation of Ultrafine beta -Mo03 from Industrial Grade Mo03 Powder by the Method of Sublimation", THE JOURNAL OF PHYSICAL CHEMISTRY C, vol. 120, no. 35, 8 September 2016 (2016-09-08), pages 19821 - 19829, XP055809407 *

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7188664B1 (ja) * 2021-03-24 2022-12-13 Dic株式会社 三酸化モリブデン粉体及びその製造方法
JPWO2023013244A1 (https=) * 2021-08-04 2023-02-09
WO2023013244A1 (ja) * 2021-08-04 2023-02-09 三井金属鉱業株式会社 モリブデン酸溶液およびその製造方法、酸化モリブデン粉末およびその製造方法
JP7338093B2 (ja) 2021-08-04 2023-09-04 三井金属鉱業株式会社 モリブデン酸溶液およびその製造方法、酸化モリブデン粉末およびその製造方法
KR20240039170A (ko) * 2021-08-04 2024-03-26 미쓰이금속광업주식회사 몰리브덴산 용액 및 그 제조 방법, 산화몰리브덴 분말 및 그 제조 방법
KR102723282B1 (ko) 2021-08-04 2024-10-31 미쓰이금속광업주식회사 몰리브덴산 용액 및 그 제조 방법, 산화몰리브덴 분말 및 그 제조 방법
JPWO2024058260A1 (https=) * 2022-09-15 2024-03-21
WO2024058260A1 (ja) * 2022-09-15 2024-03-21 Dic株式会社 複合体、触媒インク、及び複合体の製造方法
JP7605374B2 (ja) 2022-09-15 2024-12-24 Dic株式会社 複合体、触媒インク、及び複合体の製造方法
CN115321598A (zh) * 2022-09-23 2022-11-11 西安稀有金属材料研究院有限公司 低成本、高分散、高孔隙和高纯超细三氧化钼的制备方法
CN115321598B (zh) * 2022-09-23 2023-10-20 西安稀有金属材料研究院有限公司 低成本、高分散、高孔隙和高纯超细三氧化钼的制备方法

Also Published As

Publication number Publication date
EP4036061A1 (en) 2022-08-03
EP4036061A4 (en) 2023-11-08
US12497303B2 (en) 2025-12-16
US20220340443A1 (en) 2022-10-27
CN114430728A (zh) 2022-05-03
JPWO2021060375A1 (https=) 2021-04-01
JP7056807B2 (ja) 2022-04-19
KR20220070436A (ko) 2022-05-31
KR102813084B1 (ko) 2025-05-28
TWI815040B (zh) 2023-09-11
TW202116683A (zh) 2021-05-01

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