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WO2010079843A1 - Agrégat nanocristallin et son procédé de production - Google Patents

Agrégat nanocristallin et son procédé de production Download PDF

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Publication number
WO2010079843A1
WO2010079843A1 PCT/JP2010/050365 JP2010050365W WO2010079843A1 WO 2010079843 A1 WO2010079843 A1 WO 2010079843A1 JP 2010050365 W JP2010050365 W JP 2010050365W WO 2010079843 A1 WO2010079843 A1 WO 2010079843A1
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WO
WIPO (PCT)
Prior art keywords
producing
nanocrystal
solution
nanocrystal aggregate
aggregate
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/JP2010/050365
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English (en)
Japanese (ja)
Inventor
一実 加藤
鋒 党
誠 桑原
宏明 今井
智志 和田
肇 羽田
恵介 景山
幸恵 中野
利昌 鈴木
直仁 山田
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.)
NGK Insulators Ltd
Murata Manufacturing Co Ltd
National Institute of Advanced Industrial Science and Technology AIST
Taiyo Yuden Co Ltd
TDK Corp
Original Assignee
NGK Insulators Ltd
Murata Manufacturing Co Ltd
National Institute of Advanced Industrial Science and Technology AIST
Taiyo Yuden Co Ltd
TDK Corp
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Filing date
Publication date
Application filed by NGK Insulators Ltd, Murata Manufacturing Co Ltd, National Institute of Advanced Industrial Science and Technology AIST, Taiyo Yuden Co Ltd, TDK Corp filed Critical NGK Insulators Ltd
Publication of WO2010079843A1 publication Critical patent/WO2010079843A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C30B29/605—Products containing multiple oriented crystallites, e.g. columnar crystallites
    • 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
    • C30B28/00—Production of homogeneous polycrystalline material with defined structure
    • C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
    • 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
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides
    • C30B29/32—Titanates; Germanates; Molybdates; Tungstates
    • 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
    • C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
    • C30B30/06—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions using mechanical vibrations
    • 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
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions

Definitions

  • the present invention relates to a nanocrystal aggregate in which nanocrystals are aggregated, and a method for producing the same.
  • Ceramic electronic parts are being made smaller and higher performance, and various materials have been developed. In addition, harmless materials with low environmental impact and low-temperature manufacturing technology are required. Under such circumstances, a ceramic powder having a small particle size and a narrow particle size distribution that can be sintered at a low temperature is attracting attention as a material for electronic components.
  • This small particle size and narrow particle size distribution powder can be synthesized, for example, by an aqueous solution reaction under pressure (hydrothermal reaction) or a thermal decomposition reaction of sprayed droplets.
  • Patent Document 1 discloses a method for producing plate-like calcium hydroxide
  • Patent Document 2 discloses a colloidal particle precipitation / floating method and a processing apparatus using the method
  • Patent Document 3 discloses a method for producing a ceramic raw material powder. It is disclosed.
  • small particles having a particle size of submicron or less have a large surface ratio to the volume, and the surface is active, so that it is difficult to control the aggregation state. That is, the number of fine particles constituting the aggregated grains, the crystal orientation, and the size and shape of the entire aggregate cannot be adjusted. For this reason, the particle size and shape of the aggregated particles cannot be arbitrarily arranged. As a result, even if it is possible to synthesize particles having a small particle size on the order of nanometers, it is not possible to sinter dense ceramics at low temperatures by taking advantage of the characteristics.
  • An object of the present invention is to provide a nanocrystal aggregate in which nanocrystals are aggregated and a method for producing the same.
  • a nanocrystal aggregate can be obtained by irradiating a mixed solution containing metal ions with ultrasonic waves. That is, according to the present invention, the following nanocrystal aggregates and methods for producing the same are provided.
  • a method for producing a nanocrystal aggregate in which a nanocrystal aggregate in which nanocrystals are aggregated is produced by irradiating a mixed solution containing metal ions with ultrasonic waves.
  • the mixed solution containing the metal ions is obtained by dissolving or dispersing any one of an inorganic salt, an organic acid, and an organic metal compound in one of water, alcohol, and an organic solvent. Or the manufacturing method of the nanocrystal aggregate
  • nanocrystal aggregate By irradiating the mixed solution containing metal ions with ultrasonic waves, a nanocrystal aggregate can be produced, and the synthesis time for obtaining the nanocrystal can be shortened.
  • secondary particles in which primary particles (nanocrystals) are aligned in the same crystal orientation can be synthesized.
  • secondary agglomerated particles having a uniform particle size can be synthesized.
  • 3 is a flowchart showing a procedure for synthesizing barium titanate nanocrystals in Process 1. It is a flowchart which shows the synthetic
  • 4 is a flowchart showing a procedure for synthesizing barium titanate nanocrystals in Process 3. It is a SEM photograph of the powder synthesize
  • the method for producing a nanocrystal aggregate of the present invention is a method for producing a nanocrystal aggregate in which nanocrystals are aggregated by irradiating a mixed solution containing metal ions with ultrasonic waves.
  • the nanocrystal aggregate (sometimes referred to as an aggregate) produced by the method for producing a nanocrystal aggregate of the present invention is a collection of nanocrystals.
  • a nanocrystal is a single crystal particle having a particle size of several nanometers to several tens of nanometers.
  • the gathering of nanocrystals means a state in which a plurality of nanocrystals gather and are in contact with each other.
  • the nanocrystals are assembled with a specific crystal orientation.
  • “Aggregating in a specific crystal orientation” means a state in which a plurality of nanocrystals are gathered in the same crystal orientation and are in contact with each other.
  • the nanocrystals are aligned in a specific crystal orientation.
  • “Aligned to a specific crystal orientation” means a state in which they are aligned in the same crystal orientation.
  • the particle size of the nanocrystal aggregate of the present invention is 100 nanometers to 50 micrometers. Furthermore, the particle size distribution of the nanocrystal aggregate is within 30 nanometers centering on the particle size.
  • the form control method of barium titanate aggregates that is, the method of irradiating ultrasonic waves to a mixed solution of barium ions and titanium ions
  • the mixed solution containing metal ions is obtained by dissolving and dispersing an inorganic salt, an organic acid, and an organometallic compound in any of water, alcohol, and an organic solvent.
  • Inorganic salts include chlorides, nitrates, sulfates and the like.
  • Examples of the organic acid include acetate and formate.
  • Examples of organometallic compounds include metal alkoxides.
  • a colloidal dispersion solution containing one or more metal ions can be used as the mixed solution.
  • the colloid dispersion solution include titanate colloid and titanium hydroxide colloid.
  • the frequency of ultrasonic waves in the reaction step by ultrasonic irradiation is preferably 10 kHz to 1000 kHz, and more preferably 20 kHz to 100 kHz. If it is less than 10 kHz, it is difficult to obtain an irradiation effect. On the other hand, if it exceeds 1000 kHz, heat is generated, which is not appropriate.
  • barium titanate aggregate as a nanocrystal aggregate
  • an alkaline solution in which sodium hydroxide is added to a mixed aqueous solution consisting of an aqueous barium chloride solution and an aqueous titanium chloride solution can be used as the mixed solution containing metal ions. It does not exclude mixed solutions containing ions other than.
  • a sol solution formed by hydrolysis of a metal alkoxide such as titanium tetraisopropoxide can be used as the colloid dispersion solution, but other colloids are included. It does not exclude the solution.
  • the ultrasonic irradiation is performed at 80 ° C. to 100 ° C. If the reaction temperature is too low, the solubility of metal ions is lowered and segregation occurs, so that the target crystal cannot be synthesized.
  • FIGS. 1A to 1B taking as an example the case of producing a barium titanate aggregate.
  • distilled water is prepared and bubbled with Ar gas to exclude carbon dioxide in the air.
  • a BaCl 2 solution containing Ba ions is prepared at room temperature.
  • a TiCl 4 solution containing Ti ions is prepared. It is preferable that the Ba ions contained in the BaCl 2 solution and the Ti ions contained in the TiCl 4 solution be produced in the same number.
  • the pH is adjusted by mixing these solutions with an aqueous NaOH solution or the like.
  • the pH is preferably 13 to 14, and more preferably 14.
  • ultrasonic irradiation is performed at 50 to 200 W / cm 2 .
  • the temperature of the solution is preferably 80 to 100 ° C.
  • the produced powder is centrifuged, washed with ion-exchanged distilled water, and dried in a vacuum dryer.
  • distilled water is prepared and bubbled with Ar gas.
  • a BaCl 2 solution containing Ba ions is prepared at room temperature.
  • a TiCl 4 solution containing the same number of Ti ions as Ba ions is prepared and added to the BaCl 2 solution.
  • pH is adjusted by adding NaOH aqueous solution etc. to this solution and mixing.
  • ultrasonic irradiation is performed at 50 to 200 W / cm 2 .
  • the produced powder is centrifuged, washed with ion-exchanged distilled water, and dried in a vacuum dryer.
  • distilled water is prepared and bubbled with Ar gas.
  • a BaCl 2 solution containing Ba ions is prepared at room temperature.
  • pH is adjusted by adding NaOH aqueous solution etc. to this solution and mixing.
  • a TiCl 4 solution containing the same number of Ti ions as Ba ions is prepared and added to the BaCl 2 solution.
  • ultrasonic irradiation is performed at 50 to 200 W / cm 2 .
  • the produced powder is centrifuged, washed with ion-exchanged distilled water, and dried in a vacuum dryer.
  • nanocrystal aggregate in which nanocrystals are aligned in the same crystal orientation can be produced.
  • Titanium chloride manufactured by Wako Pure Chemical Industries
  • barium chloride manufactured by Wako Pure Chemical Industries
  • sodium hydroxide were used.
  • a horn type ultrasonic irradiation device manufactured by Branson, Sonifier D450 type was used, and the frequency was 20 kHz and the output was 150 W / cm 2 .
  • Process 1 of the nanoparticle synthesis procedure is shown in FIG. 1A, process 2 in FIG. 1B, and process 3 in FIG. 1C.
  • Process 1, Process 2, and Process 3 were applied.
  • ⁇ Process 1> As shown in FIG. 1A, 50 ml of distilled water was prepared and bubbled with Ar gas for 30 minutes. Using this, a BaCl 2 solution containing 0.1 M (mol / L) and 0.05 M Ba ions was prepared at room temperature. Similarly, a TiCl 4 solution containing 0.1 M (mol / L) and 0.05 M Ti ions was prepared. And these solutions and NaOH aqueous solution (5N) were mixed, and it was set to pH14 at room temperature. Next, ultrasonic irradiation was performed at 80 ° C. in air at 150 W / cm 2 . The produced powder was centrifuged twice, washed twice with ion-exchanged distilled water, and dried in a vacuum dryer at 100 ° C. for 2 hours.
  • Table 1 shows the process of the prepared sample, the solution concentration (concentration of Ba ion and Ti ion), and the ultrasonic irradiation time.
  • the crystal phase and crystallinity of the particles of the prepared sample were evaluated using an X-ray powder diffraction method (XRD, acceleration voltage 40 kV, current 20 mA). Further, the microstructure was observed using a scanning electron microscope (SEM, acceleration voltage 10 kV) and a transmission electron microscope (TEM, acceleration voltage 300 kV). The crystallinity of each particle was analyzed by electron diffraction (restricted field method, nanobeam diffraction). The chemical composition of the particles and the supernatant solution was evaluated by ICP emission analysis.
  • XRD X-ray powder diffraction method
  • SEM scanning electron microscope
  • TEM transmission electron microscope
  • BaCO 3 was the main phase regardless of the solution concentration and the ultrasonic irradiation time.
  • FIG. 2 shows scanning micrographs of particles synthesized under the raw material solution mixing method (processes 1, 2, 3), solution concentration (0.1 M, 0.05 M), and ultrasonic irradiation time of 20 minutes.
  • the product obtained from the high-concentration (0.1 M) solution has aggregated primary particles having a small particle size to form pseudospherical secondary particles having a relatively uniform particle size. I understood.
  • the product obtained from the low-concentration (0.05 M) solution in Process 2 had a characteristic structure in which secondary particles having an angular shape were assembled.
  • FIGS. 3A, 3B, and 3C transmission electron micrographs of the barium titanate particles synthesized for the processes 1 and 2 using a high-concentration (0.1M) solution under the condition of ultrasonic irradiation time of 40 minutes are shown in FIGS. 3A, 3B, and 3C.
  • 3A shows process 1, solution concentration 0.1M
  • FIG. 3B shows process 1, solution concentration 0.05M
  • FIG. 3C shows process 2, solution concentration 0.1M.
  • the particle size of the secondary particles was 250 nm to 400 nm, and had a relatively quasi-spherical shape. Further, according to observation with a high-resolution transmission electron microscope, it was found that the particle size of the primary particles (nanocrystal) was 5 nm to 10 nm and was indefinite. Furthermore, lattice fringes were observed in the primary particles, which revealed that they were barium titanate nanocrystals.
  • 4A to 6B show the electron diffraction results of the barium titanate particles synthesized in Processes 1 and 2 using a high-concentration (0.1 M) solution under the condition of ultrasonic irradiation time of 40 minutes.
  • 4A and 4B are electron diffraction patterns (process 1, solution concentration 0.1 M) of powder synthesized with an ultrasonic irradiation time of 40 minutes, and SAED in FIG. 4A is a limited field of view and electron diffraction pattern
  • FIG. 1-6 are the nanobeam irradiation position and the nanobeam diffraction pattern.
  • 5A and 5B are electron diffraction patterns (process 1, solution concentration 0.05 M) of powder synthesized with an ultrasonic irradiation time of 40 minutes.
  • SAED in FIG. 5A is a limited field of view and electron diffraction pattern
  • FIG. 1-6 are the nanobeam irradiation position and the nanobeam diffraction pattern.
  • 6A and 6B are electron diffraction patterns (process 2, solution concentration 0.1 M) of the powder synthesized with an ultrasonic irradiation time of 40 minutes.
  • SAED in FIG. 6A is a limited field of view and electron diffraction pattern
  • FIG. 1-6 are the nanobeam irradiation position and the nanobeam diffraction pattern.
  • Secondary particles (aggregates of barium titanate nanocrystal primary particles) synthesized from an electron beam diffraction pattern (SAED in FIGS. 4A to 6B) obtained by combining a single secondary particle with a limited field stop ( ⁇ 150 nm) are: It turned out that all show the pattern similar to a barium titanate single crystal according to a zone axis. From this result, it was suggested that the secondary particles synthesized by ultrasonic irradiation had high crystallinity, and the primary particles (barium titanate nanocrystals) constituting the secondary particles were aligned in the same direction.
  • the electron beam diffraction pattern of the secondary particles with the nanobeam diffraction pattern (nanobeam diameter 1 nm) of the primary particles constituting the secondary particles (1-6 in FIGS. 4B, 5B, and 6B). It was clarified that the primary particles have the same crystal orientation and that the orientation coincides with the crystal orientation of the entire secondary particles.
  • the present invention can be used as a method for producing a nanocrystal aggregate having a uniform crystal orientation.
  • the nanocrystal aggregate of the present invention can be used for dielectric materials, piezoelectric materials, and the like.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

La présente invention est un agrégat nanocristallin qui est un agrégat de nanocristaux. L'invention concerne également un procédé pour produire un tel agrégat. Une solution mixte ou une dispersion colloïdale contenant un ou plusieurs types d'ions métalliques est irradiée avec des ondes ultrasonores afin de produire un agrégat nanocristallin dans lequel des grains monocristallins dont la taille est comprise entre 1 et 20 nanomètres sont alignés/agrégés de sorte que les nanocristaux aient une orientation cristalline prédéterminée, et la dimension des grains de l'agrégat est ajustée pour être comprise entre 100 nanomètres et 50 micromètres.
PCT/JP2010/050365 2009-01-07 2010-01-07 Agrégat nanocristallin et son procédé de production Ceased WO2010079843A1 (fr)

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JP2009001934A JP5488957B2 (ja) 2009-01-07 2009-01-07 ナノクリスタル集合体、およびその製造方法

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012188335A (ja) * 2011-03-14 2012-10-04 National Institute Of Advanced Industrial Science & Technology ナノ結晶の配列方法、ナノ結晶膜の作製方法、ナノ結晶膜被覆基板及びその製造方法
WO2013010066A1 (fr) * 2011-07-14 2013-01-17 Covaris, Inc. Systèmes et procédés de fabrication de compositions nanocristallines au moyen d'énergie acoustique focalisée
WO2016060042A1 (fr) * 2014-10-17 2016-04-21 国立研究開発法人産業技術総合研究所 Procédé d'alignement de nanocristaux, procédé de production d'une structure nanocristalline, substrat formant structure nanocristalline et son procédé de production
CN117881642A (zh) * 2021-08-31 2024-04-12 国立研究开发法人产业技术综合研究所 钙钛矿型陶瓷成型体和其制造方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001152213A (ja) * 1999-11-24 2001-06-05 Japan Science & Technology Corp 金属超微粒子とその製造方法
KR20030012222A (ko) * 2001-07-31 2003-02-12 삼성정밀화학 주식회사 티탄산바륨의 제조방법
JP2007031799A (ja) * 2005-07-28 2007-02-08 Toda Kogyo Corp 金属ナノ粒子の製造方法
JP2008037064A (ja) * 2006-08-10 2008-02-21 Murata Mfg Co Ltd 配向性セラミックスの製造方法
JP2008133162A (ja) * 2006-11-29 2008-06-12 Kyocera Corp チタン酸バリウム粉末およびその製法、ならびに誘電体磁器

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001152213A (ja) * 1999-11-24 2001-06-05 Japan Science & Technology Corp 金属超微粒子とその製造方法
KR20030012222A (ko) * 2001-07-31 2003-02-12 삼성정밀화학 주식회사 티탄산바륨의 제조방법
JP2007031799A (ja) * 2005-07-28 2007-02-08 Toda Kogyo Corp 金属ナノ粒子の製造方法
JP2008037064A (ja) * 2006-08-10 2008-02-21 Murata Mfg Co Ltd 配向性セラミックスの製造方法
JP2008133162A (ja) * 2006-11-29 2008-06-12 Kyocera Corp チタン酸バリウム粉末およびその製法、ならびに誘電体磁器

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012188335A (ja) * 2011-03-14 2012-10-04 National Institute Of Advanced Industrial Science & Technology ナノ結晶の配列方法、ナノ結晶膜の作製方法、ナノ結晶膜被覆基板及びその製造方法
WO2013010066A1 (fr) * 2011-07-14 2013-01-17 Covaris, Inc. Systèmes et procédés de fabrication de compositions nanocristallines au moyen d'énergie acoustique focalisée
CN103958744A (zh) * 2011-07-14 2014-07-30 科瓦里斯股份有限公司 用于使用聚焦声制备纳米晶体组合物的系统和方法
CN103958744B (zh) * 2011-07-14 2016-08-31 科瓦里斯股份有限公司 用于使用聚焦声制备纳米晶体组合物的系统和方法
WO2016060042A1 (fr) * 2014-10-17 2016-04-21 国立研究開発法人産業技術総合研究所 Procédé d'alignement de nanocristaux, procédé de production d'une structure nanocristalline, substrat formant structure nanocristalline et son procédé de production
JPWO2016060042A1 (ja) * 2014-10-17 2017-07-27 国立研究開発法人産業技術総合研究所 ナノ結晶の配列方法、ナノ結晶構造体の作製方法、ナノ結晶構造体形成基板及びナノ結晶構造体形成基板の製造方法
US10766785B2 (en) 2014-10-17 2020-09-08 National Institute Of Advanced Industrial Science And Technology Method of arranging nanocrystals, method of producing nanocrystal structure, nanocrystal structure formation substrate, and method of manufacturing nanocrystal structure formation substrate
CN117881642A (zh) * 2021-08-31 2024-04-12 国立研究开发法人产业技术综合研究所 钙钛矿型陶瓷成型体和其制造方法

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