JP4064241B2 - 高品質チタン酸バリウム系パウダーの製造方法 - Google Patents
高品質チタン酸バリウム系パウダーの製造方法 Download PDFInfo
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- JP4064241B2 JP4064241B2 JP2002565899A JP2002565899A JP4064241B2 JP 4064241 B2 JP4064241 B2 JP 4064241B2 JP 2002565899 A JP2002565899 A JP 2002565899A JP 2002565899 A JP2002565899 A JP 2002565899A JP 4064241 B2 JP4064241 B2 JP 4064241B2
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- barium
- barium titanate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/468—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
- C01P2002/34—Three-dimensional structures perovskite-type (ABO3)
-
- 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
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- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
[反応式1] BaCl2 + TiCl4 + 2C2O4H2 + 5H2O → BaTiO(C2O4)2・4H2O + 6HC1
[反応式2] BaTiO(C2O4)2・4H2O → BaTiO(C2O4)2 + 4H2O
[反応式3] BaTiO(C2O4)2 + 1/2 O2 → BaCO3 +TiO2 +2CO2
[反応式4] BaCO3 + TiO2 → BaTiO3
既存のシュウ酸塩法で塩化バリウムと四塩化チタンの混合水溶液の滴加時の問題点は、滴加時点のシュウ酸溶液の最適濃度の低下によりバリウム対チタンの非化学量論組成を有するバリウムチタニルシュウ酸塩が生成するということである。しかし、本発明のノズル高速噴射時には、最適の化学量論組成を有するバリウムチタニルシュウ酸塩を高収率で製造することができ、これにより高温カ焼時、粒成長の均一な高品質のチタン酸バリウムパウダーを得ることができる。
1mol/l濃度のTiCl4水溶液1200lと1mol/l濃度のBaCl2水溶液1320lとを4M3グラス−ライン(Glass-lined)反応槽でよく混ぜて混合溶液を作った後、これを6M3反応器に予め作っておいた1mol/l濃度のシュウ酸水溶液2520lにフル−コン(Full-Con)タイプの一流体ノズルを用いて21l/minの速度で噴射して滴加した。この際、シュウ酸溶液を機械攪拌機で攪拌しながら噴射して、攪拌機の攪拌速度は150rpmに維持して、シュウ酸溶液の温度は90℃に維持した。そして、ノズル噴射の際、混合溶液供給ポンプとしてダイヤフラムポンプを使用した。このように2時間滴加して、1時間反応温度を維持した後、攪拌を維持したまま空冷させて1時間熟成した。その後、前記から製造されたバリウムチタニルシュウ酸塩スラリを遠心分離機により濾過し、洗滌液のpHが6以上になるように純粋で洗滌してバリウムチタニルシュウ酸塩結晶を得た。この際、収率は98%(Tiイオン基準)であり、Ba/Tiモル比は0.999であった。
二流体ノズルを使用したことを除いては、前記実施例1と同様の方法によりバリウムチタニルシュウ酸塩結晶を製造した。この際、収率は96%(Tiイオン基準)であり、反応器壁から採取したBTOのBa/Tiモル比は0.987、全体モル比は0.997であった。
1mol/l濃度のTiCl4水溶液1.2lと1mol/l濃度のBaCl2水溶液1.3lとを4l反応器でよく混ぜて混合溶液を作った後、これを6l反応器に予め作っておいた1mol/l濃度のシュウ酸水溶液2.5lに2時間滴下して添加(dropwise addition)した。この際、シュウ酸溶液の温度は90℃にして、滴加速度は21ml/minに調節した。滴加後、1時間反応温度を維持し、1時間攪拌を維持したまま空冷してバリウムチタニルシュウ酸塩沈殿を得た。前記実施例と同様の方法により沈殿を濾過、洗滌してバリウムチタニルシュウ酸塩結晶を得た。この際、収率は80%(Tiイオン基準)であり、Ba/Tiモル比は0.921であった。
Claims (12)
- 塩化バリウム(BaCl2)及び四塩化チタン(TiCl4)の混合水溶液を高速噴射ノズルによりシュウ酸(H2C2O4)水溶液に滴加して沈殿させた後、熟成させて、洗滌及び濾過してバリウムチタニルシュウ酸塩(BTO)結晶を得る段階;
前記得られたバリウムチタニルシュウ酸塩(BTO)結晶を1次粉砕し乾燥した後、熱分解させてチタン酸バリウム(BaTiO3)パウダーを形成する段階;及び
前記形成されたチタン酸バリウムパウダーを2次粉砕させる段階を含み、
前記ノズルのタイプが、一流体ノズル (single-fluid nozzle) であること
を特徴とするチタン酸バリウム系パウダーの製造方法。 - 前記ノズルの噴射速度が、0.01〜70l/minであることを特徴とする請求項1に記載のチタン酸バリウム系パウダーの製造方法。
- 前記一流体ノズルが、フル−コン(Full-Con)、ホロー−コン(Hollow-Con)及びフラット(Flat)の中から選択されることを特徴とする請求項1又は2に記載のチタン酸バリウム系パウダーの製造方法。
- 前記塩化バリウム水溶液及び塩化チタン水溶液の濃度が、0.2〜2.0mol/lであることを特徴とする請求項1に記載のチタン酸バリウム系パウダーの製造方法。
- 前記塩化バリウム(BaCl2)/四塩化チタン(TiCl4)のモル比が1〜1.5であることを特徴とする請求項1に記載のチタン酸バリウム系パウダーの製造方法。
- 前記シュウ酸(H2C2O4)水溶液の濃度が、0.2〜2.0mol/lであることを特徴とする請求項1に記載のチタン酸バリウム系パウダーの製造方法。
- 前記熟成が、1〜100時間行われることを特徴とする請求項1に記載のチタン酸バリウム系パウダーの製造方法。
- 前記バリウムチタニルシュウ酸塩(BTO)結晶を1次粉砕する際、添加剤を用いて、Ba、Ti、またはBa及びTiを他の元素で置換することを特徴とする請求項1に記載のチタン酸バリウム系パウダーの製造方法。
- 前記Baの置換元素が、Mg、Ca、Sr及びPbの中から選択される1種以上であることを特徴とする請求項8に記載のチタン酸バリウム系パウダーの製造方法。
- 前記Tiの置換元素が、Zr,Hf及びSnの中から選択される1種以上であることを特徴とする請求項8に記載のチタン酸バリウム系パウダーの製造方法。
- 前記添加剤が、置換元素の塩化物及び硝酸塩から選択されることを特徴とする請求項8乃至10のいずれか一つの項に記載のチタン酸バリウム系パウダーの製造方法。
- 前記熱分解の加熱速度が0.5〜10℃/minであり、維持温度が700〜1200℃であることを特徴とする請求項1に記載のチタン酸バリウム系パウダーの製造方法。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR10-2001-0009066A KR100414832B1 (ko) | 2001-02-22 | 2001-02-22 | 고품질 티탄산바륨계 파우더의 제조방법 |
PCT/KR2002/000165 WO2002066377A1 (en) | 2001-02-22 | 2002-02-05 | Method for preparing high quality barium-titanate based powder |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2004521850A JP2004521850A (ja) | 2004-07-22 |
JP4064241B2 true JP4064241B2 (ja) | 2008-03-19 |
Family
ID=19706141
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2002565899A Expired - Lifetime JP4064241B2 (ja) | 2001-02-22 | 2002-02-05 | 高品質チタン酸バリウム系パウダーの製造方法 |
Country Status (7)
Country | Link |
---|---|
US (1) | US20040115122A1 (ja) |
EP (1) | EP1362008A1 (ja) |
JP (1) | JP4064241B2 (ja) |
KR (1) | KR100414832B1 (ja) |
CN (1) | CN1234613C (ja) |
TW (1) | TW558470B (ja) |
WO (1) | WO2002066377A1 (ja) |
Families Citing this family (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
TW527321B (en) * | 2000-08-09 | 2003-04-11 | Samsung Electro Mech | A method for producing barium titanate based powders by oxalate process |
KR100434883B1 (ko) * | 2001-08-14 | 2004-06-07 | 삼성전기주식회사 | 티탄산바륨계 파우더의 제조방법 |
KR100503857B1 (ko) * | 2002-11-01 | 2005-07-25 | (주)아해 | 무기산으로 제조한 사염화티타늄 수용액과 염화바륨수용액으로부터 나노크기의 결정성 티탄산바륨 분말을제조하는 방법 |
JP5025100B2 (ja) * | 2005-06-27 | 2012-09-12 | 京セラ株式会社 | チタン酸バリウム粉末の製造方法 |
CN101537494B (zh) * | 2009-04-29 | 2010-07-28 | 北京科技大学 | 一种镍颗粒分散锆钛酸钡钙压电复合材料的制备方法 |
KR101606932B1 (ko) * | 2009-04-29 | 2016-03-28 | 삼성전기주식회사 | 옥살레이트 공정에 의한 티탄산바륨 분말의 제조방법 및 그 방법에 의하여 제조된 티탄산바륨 분말 |
US9242922B2 (en) * | 2011-04-01 | 2016-01-26 | M. Technique Co., Ltd. | Method for producing barium titanyl salt and barium titanate |
CN102242400B (zh) * | 2011-06-29 | 2013-06-05 | 浙江大学 | 一种制备单晶CaTiO3枝晶的方法 |
JP5879078B2 (ja) | 2011-09-15 | 2016-03-08 | 日本化学工業株式会社 | シュウ酸バリウムチタニルの製造方法及びチタン酸バリウムの製造方法 |
CN108675785A (zh) * | 2012-11-30 | 2018-10-19 | 三星电机株式会社 | 制造钛酸钡的方法和通过该方法制造的钛酸钡 |
KR101770701B1 (ko) | 2012-12-21 | 2017-09-06 | 삼성전자주식회사 | 티탄산 바륨을 포함한 이산화탄소 흡착제, 이를 포함한 이산화탄소 포집 모듈, 및 이를 이용한 이산화탄소 분리 방법 |
KR102376545B1 (ko) * | 2017-08-01 | 2022-03-21 | 삼성디스플레이 주식회사 | 플렉시블 디스플레이 윈도우 |
Family Cites Families (19)
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US2985506A (en) * | 1957-12-06 | 1961-05-23 | Vita Sam Di | Method of producing barium titanate |
US3529978A (en) * | 1969-09-23 | 1970-09-22 | Globe Union Inc | General purpose batio3 ceramic dielectric compositions |
SE451114B (sv) * | 1981-11-13 | 1987-09-07 | Fluidcarbon International Ab | Sett for forstoftning av partikelhaltiga dispersioner och losningar |
JPS5936919A (ja) * | 1982-08-25 | 1984-02-29 | 三菱鉱業セメント株式会社 | 磁器コンデンサ |
JPS61146710A (ja) * | 1984-12-19 | 1986-07-04 | Central Glass Co Ltd | 高純度チタン酸バリウム微粒子の製造方法 |
JPS62154680A (ja) * | 1985-12-27 | 1987-07-09 | Toyo Soda Mfg Co Ltd | アクチユエ−タ−用BaTiO↓3系磁器 |
US4764493A (en) * | 1986-06-16 | 1988-08-16 | Corning Glass Works | Method for the production of mono-size powders of barium titanate |
DE3635532A1 (de) * | 1986-10-18 | 1988-04-28 | Philips Patentverwaltung | Verfahren zur herstellung von bariumtitanat batio(pfeil abwaerts)3(pfeil abwaerts) |
DD267480A1 (de) * | 1987-11-30 | 1989-05-03 | Univ Schiller Jena | Verfahren zur herstellung von titanaten |
JPH0388719A (ja) * | 1989-08-30 | 1991-04-15 | Tdk Corp | シュウ酸チタニルバリウム粒子の製造方法 |
US5219811A (en) * | 1989-08-31 | 1993-06-15 | Central Glass Company, Limited | Powder composition for sintering into modified barium titanate semiconductive ceramic |
JPH03103323A (ja) * | 1989-09-14 | 1991-04-30 | Tdk Corp | シュウ酸チタニルバリウム粒子の製造方法 |
KR960014909B1 (ko) * | 1993-06-08 | 1996-10-21 | 쌍용양회공업 주식회사 | 티탄산 바륨의 제조 방법 |
IT1270828B (it) * | 1993-09-03 | 1997-05-13 | Chon Int Co Ltd | Processo per la sintesi di polveri ceramiche cristalline di composti di perovskite |
KR19980013821A (ko) * | 1996-08-03 | 1998-05-15 | 구자홍 | 액정 디스플레이의 자동 밝기 조절장치 |
US5783165A (en) * | 1997-01-08 | 1998-07-21 | Ferro Corporation | Method of making barium titanate |
US6660680B1 (en) * | 1997-02-24 | 2003-12-09 | Superior Micropowders, Llc | Electrocatalyst powders, methods for producing powders and devices fabricated from same |
US6251816B1 (en) * | 1998-12-31 | 2001-06-26 | Mra Laboratories, Inc. | Capacitor and dielectric ceramic powder based upon a barium borate and zinc silicate dual-component sintering flux |
KR100360118B1 (ko) * | 1999-07-05 | 2002-11-04 | 삼성전기주식회사 | 옥살레이트법에 의한 티탄산바륨계 산화물 분말 제조방법 |
-
2001
- 2001-02-22 KR KR10-2001-0009066A patent/KR100414832B1/ko active IP Right Grant
-
2002
- 2002-02-05 US US10/468,468 patent/US20040115122A1/en not_active Abandoned
- 2002-02-05 WO PCT/KR2002/000165 patent/WO2002066377A1/en not_active Application Discontinuation
- 2002-02-05 CN CNB02806805XA patent/CN1234613C/zh not_active Expired - Lifetime
- 2002-02-05 JP JP2002565899A patent/JP4064241B2/ja not_active Expired - Lifetime
- 2002-02-05 EP EP02700822A patent/EP1362008A1/en not_active Withdrawn
- 2002-02-22 TW TW091103229A patent/TW558470B/zh not_active IP Right Cessation
Also Published As
Publication number | Publication date |
---|---|
JP2004521850A (ja) | 2004-07-22 |
TW558470B (en) | 2003-10-21 |
CN1234613C (zh) | 2006-01-04 |
CN1498192A (zh) | 2004-05-19 |
US20040115122A1 (en) | 2004-06-17 |
WO2002066377A1 (en) | 2002-08-29 |
KR100414832B1 (ko) | 2004-01-13 |
EP1362008A1 (en) | 2003-11-19 |
KR20020068792A (ko) | 2002-08-28 |
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