JP2009256140A - 誘電体粒子の製造方法 - Google Patents
誘電体粒子の製造方法 Download PDFInfo
- Publication number
- JP2009256140A JP2009256140A JP2008107693A JP2008107693A JP2009256140A JP 2009256140 A JP2009256140 A JP 2009256140A JP 2008107693 A JP2008107693 A JP 2008107693A JP 2008107693 A JP2008107693 A JP 2008107693A JP 2009256140 A JP2009256140 A JP 2009256140A
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- JP
- Japan
- Prior art keywords
- heat treatment
- barium titanate
- particles
- titanium dioxide
- treatment step
- 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
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- 239000002245 particle Substances 0.000 title claims abstract description 290
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 47
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 306
- 238000010438 heat treatment Methods 0.000 claims abstract description 262
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 188
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 188
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 137
- 239000011812 mixed powder Substances 0.000 claims abstract description 52
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 47
- 239000000843 powder Substances 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims description 42
- 230000008569 process Effects 0.000 claims description 24
- 229910052788 barium Inorganic materials 0.000 claims description 23
- 238000010304 firing Methods 0.000 claims description 19
- 238000004458 analytical method Methods 0.000 claims description 17
- 239000010936 titanium Substances 0.000 claims description 17
- 230000005540 biological transmission Effects 0.000 claims description 12
- 229910052719 titanium Inorganic materials 0.000 claims description 12
- 238000000634 powder X-ray diffraction Methods 0.000 claims description 9
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical group O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims description 2
- 239000003989 dielectric material Substances 0.000 abstract description 3
- 235000010215 titanium dioxide Nutrition 0.000 description 128
- 239000012071 phase Substances 0.000 description 55
- 239000002994 raw material Substances 0.000 description 46
- 238000006243 chemical reaction Methods 0.000 description 35
- 230000000052 comparative effect Effects 0.000 description 34
- 238000009826 distribution Methods 0.000 description 21
- 238000002441 X-ray diffraction Methods 0.000 description 17
- 239000007789 gas Substances 0.000 description 17
- 239000010419 fine particle Substances 0.000 description 14
- 230000000694 effects Effects 0.000 description 13
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 12
- 150000001553 barium compounds Chemical class 0.000 description 11
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 11
- 239000010410 layer Substances 0.000 description 11
- 239000000047 product Substances 0.000 description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- 229910010413 TiO 2 Inorganic materials 0.000 description 10
- 229910001422 barium ion Inorganic materials 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- 239000003985 ceramic capacitor Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 238000010298 pulverizing process Methods 0.000 description 7
- 230000009257 reactivity Effects 0.000 description 7
- 238000003746 solid phase reaction Methods 0.000 description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 6
- 239000000460 chlorine Substances 0.000 description 6
- 229910052801 chlorine Inorganic materials 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- 239000001569 carbon dioxide Substances 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 238000013507 mapping Methods 0.000 description 5
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 5
- 230000007704 transition Effects 0.000 description 5
- 238000004438 BET method Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 230000001186 cumulative effect Effects 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 238000005755 formation reaction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000012808 vapor phase Substances 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 3
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- WKBPZYKAUNRMKP-UHFFFAOYSA-N 1-[2-(2,4-dichlorophenyl)pentyl]1,2,4-triazole Chemical compound C=1C=C(Cl)C=C(Cl)C=1C(CCC)CN1C=NC=N1 WKBPZYKAUNRMKP-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000000790 scattering method Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000003991 Rietveld refinement Methods 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004455 differential thermal analysis Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- IBIKHMZPHNKTHM-RDTXWAMCSA-N merck compound 25 Chemical compound C1C[C@@H](C(O)=O)[C@H](O)CN1C(C1=C(F)C=CC=C11)=NN1C(=O)C1=C(Cl)C=CC=C1C1CC1 IBIKHMZPHNKTHM-RDTXWAMCSA-N 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000851 scanning transmission electron micrograph Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
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- 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
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- B82—NANOTECHNOLOGY
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Abstract
【解決手段】
ルチル化率が30%以下、比表面積が20m2/g以上の二酸化チタン粒子と炭酸バリウム粒子を混合し混合粉末を準備する工程と、該混合粉末を熱処理し、二酸化チタン粒子表面に平均厚み3nm以上の連続したチタン酸バリウム相を15重量%以上生成させる第1熱処理工程、および800〜1000℃にて熱処理を行う第2熱処理工程を含む誘電体材料の製造方法。
【選択図】 なし
Description
ルチル化率が30%以下、BET比表面積が20m2/g以上の二酸化チタン粒子を準備する工程、
BET比表面積が10m2/g以上の炭酸バリウム粒子を準備する工程、
二酸化チタン粒子と炭酸バリウム粒子とを混合し混合粉末を準備する工程、
該混合粉末を熱処理し、二酸化チタン粒子表面にチタン酸バリウム相を生成させる第1熱処理工程、および
第1熱処理工程後に、800〜1000℃にて熱処理を行う第2熱処理工程を含み、
第1熱処理工程における熱処理温度が、第2熱処理工程の熱処理温度よりも低く、第1熱処理工程後の混合粉末の15重量%以上がチタン酸バリウムとなり、二酸化チタン粒子表面に平均厚み3nm以上のチタン酸バリウム相を生成させるのに充分な時間反応させる、誘電体粒子の製造方法。
(比表面積)
原料である二酸化チタン粒子の比表面積をBET法により求めた。具体的には、NOVA2200(高速比表面積計)を用い、紛量1g、窒素ガス、1点法 脱気条件300℃で15分保持、の条件で測定した。
原料として用いた二酸化チタン粒子10mgを1100℃で水蒸気蒸留し、分解物を0.09%の過酸化水素5mlに捕集し、イオンクロマトグラフィーにより塩素量を定量した。
プラズマ発光分析法により塩素以外の不純物量を評価した。
原料として使用した二酸化チタン粒子のX線回折分析によりルチル化率を求めた。具体的には、BRUKER AXS社製、全自動多目的X線回折装置 D8 ADVANCEを用いて、Cu−Kα、40kV、40mA、2θ:20〜120degで測定し、1次元高速検出器LynxEye、発散スリット0.5deg、散乱スリット0.5degを用いた。また、スキャン:0.01〜0.02deg、スキャンスピード:0.3〜0.8s/divでスキャンした。解析には、Rietveld解析ソフト(Topas(BrukerAXS社製))を用いた。
レーザー回折散乱法を用いて原料の二酸化チタンの粒径を評価した。レーザー回折粒度分布計はMT3000(日機装(株)マイクロトラック粒度分布計)を用い、純水溶液中に分散材を0.4重量%添加して、超音波分散をしたものを用いて、累積粒度分布の微粒側からの累積10%、累積50%および累積90%の粒径を算出した。
[混合粉末の調製]
比表面積が30m2/gの炭酸バリウム粒子と、二酸化チタン粒子(TiO2(A))とをBa/Ti比が0.997となるように秤量し、ジルコニア(ZrO2)2mm径のメディアを用いた容量50リットルのボールミルにより72時間湿式混合し、その後、スプレードライにより乾燥して、混合粉末を得た。湿式混合は、スラリー濃度を40重量%とし、ポリカルボン酸塩系の分散剤を0.5重量%添加する条件で行った。ここで二酸化チタン粒子は比表面積が大きい微粒子であるため、原料の混合は十分行う必要がある。
電気炉(バッチ炉)により大気圧力中、大気雰囲気で、昇温速度3.3℃/分(200℃/時間)にて、室温から表2に示す第1熱処理温度(T0=600℃)まで混合粉末を昇温した。その後、熱処理温度にて2時間保持し、3.3℃/分(200℃/時間)で降温した。二酸化チタン原料がTiO2(A)を用い第1熱処理温度(T0)が600℃、保持時間2時間である実施例を実施例1Aとする。またTiO2(B)を使用したものを実施例1Bとする。第1熱処理をバッチ炉で実施した場合は、混合粉末100g〜250gをアルミナ製容器に充填し、反応時に発生するCO2ガス濃度を15モル%以下となるように、大気フローを実施した条件での熱処理とした。
上記した二酸化チタン粒子の場合と同様の条件で測定した。結果をRietveld解析ソフト(Topas(BrukerAXS社製))を用いて解析し、チタン酸バリウムの重量濃度を算出した。
透過電子顕微鏡(日立社製HD−2000)を用い、倍率20〜60万倍、加速電圧200.0kVでTEM像を得て、またEDS(エネルギー分散型X線分光装置)による組成マッピングし、バックグラウンドを除去し、二酸化チタンのピークとチタン酸バリウムのピークを分離し、二酸化チタン粒子表面のチタン酸バリウム相を同定した。二酸化チタン表面のチタン酸バリウム相の平均厚みは、STEM像およびZコントラスト像の60万倍の画像より算出した。また、全二酸化チタン粒子のうち、表面に平均厚み4nm以上のチタン酸バリウム相が形成された二酸化チタン粒子の割合の算出では20万倍の倍率において、6画像の視野で50個以上の二酸化チタン粒子(断面形状が観察できるもの)を用いて集計した。ここで表面に平均厚み4nm以上のチタン酸バリウム相が形成された二酸化チタン粒子とは、粒子断面像で連続的に被覆されているものである。連続的に被覆とは、Zコントラスト像で、3nm以上のチタン酸バリウム相が、断面の外周部の90%以上が連続的である状態とした。
第1熱処理工程を実施せず、それ以外は実施例1と同様の操作を行ったものを比較例1とする。原料の二酸化チタンがTiO2(A)の場合は比較例1A、TiO2(B)の場合は比較例1Bとしている。比較例1では第1熱処理工程を実施していないが、湿式粉砕後のスプレードライヤー乾燥条件の最高温度が250℃であるため、表や図においては便宜上熱処理温度を250℃で処理したものとして列挙するものとした。
混合粉末を実施例1Bと同様にして調製した。
[第1熱処理工程]
ロータリーキルン(RK炉と略)により大気雰囲気で、第1熱処理温度600℃にて0.3時間混合粉末の熱処理を行った。処理時間0.3時間は、ロータリーキルンの保温部に対し、粉末の平均滞留時間を処理時間としたものである。原料の二酸化チタンがTiO2(B)でRK炉600℃にて0.3時間で第1熱処理工程を行ったものを実施例4Bとする。第1熱処理工程の熱処理温度を650℃に変更した以外は、実施例4Bと同様の操作を行ったものを実施例5B、第1熱処理工程の熱処理温度を700℃に変更した以外は、実施例4Bと同様の操作を行ったものを実施例6Bとする。
実施例1〜6、比較例1〜3の第1熱処理工程を経た粉末に対し、第2熱処理工程を実施した。第1熱処理工程の後、一旦室温まで下げ、その粉末を分けてバッチ炉(B炉)において第2熱処理工程での温度を900〜1000℃、保持時間を2〜12時間の条件で行った。第2熱処理工程では、大気圧力中、大気雰囲気中で行い、昇温速度3.3℃/分(200℃/時間)、降温速度3.3℃/分(200℃/時間)とし、粉末5〜50gをアルミナ製容器に充填し熱処理を行った。表3、表4に代表的な結果を示す。
BET平均粒径=6(理論密度/比表面積)×1000
理論密度は、5.7g/cm3とした
結果を表5に示す。
チタン酸バリウムの誘電特性評価のため、以下のように試料を準備した。本発明の実施例(1B−1,1A−2,1B−2,3B−2,4B−2,6B−1)および比較例(1B−3)で得られたチタン酸バリウム粒子に、バインダとしてPVA(ポリビニルアルコール樹脂)を10重量%添加し、加圧成型することにより、直径12.5mm、厚さ約0.6mmの円板状の試料を得た。次に、得られた円板状の試料の脱バインダ処理として、400℃、保持時間4時間、空気中での熱処理を行った。その後、焼成温度T2が1250℃の条件で熱処理を行った。雰囲気:大気中、保持時間:2時間、昇温速度3.3℃/minの条件とした。
Claims (11)
- ルチル化率が30%以下、BET比表面積が20m2/g以上の二酸化チタン粒子を準備する工程、
BET比表面積が10m2/g以上の炭酸バリウム粒子を準備する工程、
二酸化チタン粒子と炭酸バリウム粒子とを混合し混合粉末を準備する工程、
該混合粉末を熱処理し、二酸化チタン粒子表面にチタン酸バリウム相を生成させる第1熱処理工程、および
第1熱処理工程後に、800〜1000℃にて熱処理を行う第2熱処理工程を含み、
第1熱処理工程における熱処理温度が、第2熱処理工程の熱処理温度よりも低く、第1熱処理工程後の混合粉末の15重量%以上がチタン酸バリウムとなり、二酸化チタン粒子表面に平均厚み3nm以上のチタン酸バリウム相を生成させるのに充分な時間反応させる、誘電体粒子の製造方法。 - 第1熱処理工程が、全二酸化チタン粒子の75%以上において、該二酸化チタン粒子表面に連続的に平均厚み4nm以上のチタン酸バリウム相を生成させる工程であり、混合粉末中の20重量%以上がチタン酸バリウムとなる請求項1に記載の製造方法。
- 第2熱処理工程の熱処理温度が850〜950℃であり、生成するチタン酸バリウム粒子のc/a値が1.008以上である請求項1または2に記載の製造方法。
- 第2熱処理工程の熱処理温度が850〜950℃であり、生成するチタン酸バリウム粒子は、X線CuKα線の粉末X線回折における(200)面と(002)面のピーク点の中間点におけるX線強度(Ib)と(200)面の回折線強度I(200)の比(I(200)/Ib)が4以上である請求項1〜3のいずれかに記載の製造方法。
- 第1熱処理工程を、1×103Pa以上1.0133×105Pa以下の圧力中、大気雰囲気中575〜650℃にて行い、混合粉末中の25重量%以上55重量%以下がチタン酸バリウムとなる請求項1に記載の製造方法。
- 第1熱処理工程を、粉体を流動焼成する焼成炉中で、1×103Pa以上1.0133×105Pa以下の圧力中、、大気雰囲気中600〜700℃にて行い、混合粉末中の20重量%以上75重量%以下がチタン酸バリウムとなる請求項1に記載の製造方法。
- 第1熱処理工程において、雰囲気中のCO2ガス濃度を15モル%以下に制御する請求項5または6に記載の製造方法。
- 第1熱処理工程後に、550℃以下まで冷却する工程を含み、その後第2熱処理工程を行う請求項5または6に記載の製造方法。
- 第1熱処理工程を、1×103Pa以下の圧力中で450〜600℃にて行う請求項1に記載の製造方法。
- 第1熱処理工程における生成物を粉末X線回折分析することにより、チタン酸バリウム相の重量濃度の評価を行い、第1熱処理工程の進行を確認する工程を含む請求項1に記載の製造方法。
- 第1熱処理工程における生成物を透過電子顕微鏡分析により観察し、二酸化チタン粒子表面のチタン酸バリウム相の確認を行い、第1熱処理工程の進行を確認する工程を含む請求項1に記載の製造方法。
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Also Published As
Publication number | Publication date |
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US20090264276A1 (en) | 2009-10-22 |
CN101565317B (zh) | 2012-12-12 |
CN101565317A (zh) | 2009-10-28 |
JP4525788B2 (ja) | 2010-08-18 |
TW201003692A (en) | 2010-01-16 |
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