JP4932487B2 - 複合強誘電体を得るための方法 - Google Patents
複合強誘電体を得るための方法 Download PDFInfo
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- JP4932487B2 JP4932487B2 JP2006534784A JP2006534784A JP4932487B2 JP 4932487 B2 JP4932487 B2 JP 4932487B2 JP 2006534784 A JP2006534784 A JP 2006534784A JP 2006534784 A JP2006534784 A JP 2006534784A JP 4932487 B2 JP4932487 B2 JP 4932487B2
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- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims description 46
- 239000002245 particle Substances 0.000 claims abstract description 80
- 150000001875 compounds Chemical class 0.000 claims abstract description 20
- 239000003989 dielectric material Substances 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000012530 fluid Substances 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 150000004767 nitrides Chemical class 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims description 30
- 239000011248 coating agent Substances 0.000 claims description 25
- 238000005245 sintering Methods 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 6
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 229910013641 LiNbO 3 Inorganic materials 0.000 claims description 2
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 2
- 229910002367 SrTiO Inorganic materials 0.000 claims description 2
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- 150000001242 acetic acid derivatives Chemical class 0.000 claims description 2
- 125000005595 acetylacetonate group Chemical group 0.000 claims description 2
- 150000001298 alcohols Chemical group 0.000 claims description 2
- 150000004703 alkoxides Chemical class 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 125000002524 organometallic group Chemical group 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 229910002113 barium titanate Inorganic materials 0.000 abstract description 2
- 229910003334 KNbO3 Inorganic materials 0.000 abstract 1
- 229910003327 LiNbO3 Inorganic materials 0.000 abstract 1
- 229910003781 PbTiO3 Inorganic materials 0.000 abstract 1
- 229910002370 SrTiO3 Inorganic materials 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 33
- 239000000919 ceramic Substances 0.000 description 14
- 239000010410 layer Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 230000005684 electric field Effects 0.000 description 8
- 230000008021 deposition Effects 0.000 description 7
- 239000011247 coating layer Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000004626 scanning electron microscopy Methods 0.000 description 3
- XBIUWALDKXACEA-UHFFFAOYSA-N 3-[bis(2,4-dioxopentan-3-yl)alumanyl]pentane-2,4-dione Chemical compound CC(=O)C(C(C)=O)[Al](C(C(C)=O)C(C)=O)C(C(C)=O)C(C)=O XBIUWALDKXACEA-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000008542 thermal sensitivity Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000000864 Auger spectrum Methods 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004814 ceramic processing Methods 0.000 description 1
- 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 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000009036 growth inhibition Effects 0.000 description 1
- 238000002847 impedance measurement Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
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- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000011664 signaling Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 238000003826 uniaxial pressing Methods 0.000 description 1
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Description
‐E.F.Alberta,R.Guo and A.S.Bhalla,”Novel BST:MgTiO3 composites for frequency agile applications”,Ferroelectrics,2002,Vol.268,pp.169-174、この文献はBa1−xSrxTiO3(BST)をMgTiO3(MT)と混合し、混合物を焼結することにより得られる複合材について開示している;および
‐Z.X.Xiong,X.J.Zhou,W.Z.Zen,K.Z.Baba-Khishi and S.T.Chen,”Development of ferroelectric ceramics with high dielectric constant and low dissipation factor for high-voltage capacitors”、この文献はMnSiO3、WO3、CeO2、Bi2(SnO3)3およびZnOでドープされたBaTiO3、BaZrO3およびBaSnO3から形成される複合材について開示している。
‐X.Liu,W.Y.Shin and W.H.Shih,”Effects of copper coating on the crystalline structure of the fine barium titanate particles”,Journal of the American Ceramic Society,1997,80(11),pp.2781-2788、この文献はBaTiO3粒子を銅層で被覆する技術について開示している;
‐T.M.Harkulich,J.Magder,M.S.Vukasovich and R.J.Lockhart,”Ferroelectrics of ultrafine particl size:II,grain growth inhibition studies”,Journal of the American Ceramic Society,1966,49(6),pp.295-9、この文献はBaTiO3粒子を酸化タンタル層で被覆する技術について開示している;
‐C.Huber,M.Treguer-Delapierre,C.Elissalde,F.Weill and M.Maglione,”New application of the core-shell concept to ferroelectric nanopowder”,Journal of Materials Chemistry,2003,13,pp.650-653、この文献はシリカ(SiO2)の層で被覆されたBa1−xSrxTiO3ナノスケール粒子について開示している;および
‐Z.Yue,X.Wang,L.Zhang and X.Yao,”Temperature stable Pb(Zn1/3Nb2/3)O3-based composite ceramics prepared by particle-coating method”,Journal of Materials Science Letters,1997,16(6),pp.1354-1356、この文献はSiO2‐B2O3の薄ガラス層で被覆されたPb(Zn1/3Nb2/3)O3ベースの複合セラミック粒子について開示している。
‐強誘電化合物の粒子を誘電体の層で被覆し、そして
‐被覆粒子を焼結することにより高密度複合材を形成する
工程からなり、
該被覆工程が、少なくとも1種の溶媒および誘電体の前駆物質を含有した流体と強誘電化合物の粒子を接触させることからなり、該流体が加圧下で維持されることで特徴付けられる、強誘電複合材を得るための方法を提供する。
rO2、HfO2、SnO2、SnO3およびTa2O5から選択されてよい。
‐26.5cm3の内部容積を有するデポジションリアクター1;
‐二酸化炭素CO2の形で溶媒を含有するシリンダー2:該シリンダーは供給ラインでリアクター1へ接続されている;
‐高圧ポンプ4で注入されるCO2の温度を調節して、リアクター1へ供給するためのクライオスタット3;
‐高圧ポンプ4;
‐デポジションリアクター1の周りに巻かれた加熱コイル5;
‐ヒーター5を調節するための調節器6;
‐デポジションリアクター1で圧力を測定するための圧力センサー7;
‐リアクターで圧力の過度に大きな上昇時に圧力を放出しうるラプチャーディスクの形の安全装置8;および
‐リアクター1を減圧するためのバルブ9
‐球状アルミナ粒子からなるI型粒子の集団;および
‐アルミナ被覆BST粒子からなるII型粒子の集団
を含んでなる(図3Aおよび3Bでみられる)クリーン乾燥粉末からなる。
‐リアクター中の圧力;
‐被覆温度;
‐前駆物質濃度;
‐リアクター中の滞留時間;
‐超臨界溶媒の性質;および
‐補助溶媒の添加
‐焼結圧力;
‐焼結温度;および
‐焼結時間
‐最大誘電率のシフトなしに、誘電率ピークの広域化、ひいては複合材の感熱性の低下;
‐低い誘電損失tanδ;
‐初期アルミナ被覆BST粉末の、数ギガヘルツの周波数までの電気的性質、特に強誘電および非直線性の保存;および
‐周波数非依存性チューナビリティ(実質的に100ヘルツ〜1ギガヘルツの周波数)および複合材に印加される電場に非依存性の誘電損失係数tanδ
Claims (14)
- ‐強誘電化合物の粒子を誘電化合物の層で被覆し、それにより被覆粒子のみならず、誘電化合物のみから形成されたナノ構造粒子をもたらし、そして
‐被覆粒子およびナノ構造粒子を焼結することにより、被覆粒子間で形成された隙間にナノ構造粒子が分配されてなる高密度複合材を形成する
工程からなり、
該被覆工程が、少なくとも1種の溶媒および誘電化合物の前駆物質を含有した流体と強誘電化合物の粒子を接触させることからなり、該流体が超臨界温度および圧力条件下で維持されることで特徴付けられる、強誘電複合材を得るための方法。 - 強誘電化合物粒子を合成する先行工程を更に含み、この合成が加圧下で行われる、請求項1に記載の方法。
- 粒子の合成が10℃以上の温度で行われる、請求項2に記載の方法。
- 合成が超臨界温度および圧力条件下で行われる、請求項2または3に記載の方法。
- 強誘電化合物が、次の材料:PbTiO3、PZT、PMN、LiNbO3、KNbO3、KTN、BaTiO3およびBaTiO3‐SrTiO3から選択される、請求項1〜4のいずれか一項に記載の方法。
- 強誘電化合物がBaxSr1−xTiO3 (0<x<1)またはBaTiO3である、請求項1〜5のいずれか一項に記載の方法。
- 誘電化合物が酸化物または窒化物から選択される、請求項1〜6のいずれか一項に記載の方法。
- 誘電化合物が、次の酸化物:Al2O3、SiO2、TiO2、MgTiO3、ZrO2、HfO2、SnO2、SnO3およびTa2O5から選択される、請求項7に記載の方法。
- 誘電化合物の前駆物質が、塩類、金属および有機金属錯体の群から選択される、請求項1〜8のいずれか一項に記載の方法。
- 誘電化合物の前駆物質が、アセテート類、アセチルアセトネート類またはアルコキシド類の群から選択される、請求項1〜8のいずれか一項に記載の方法。
- 溶媒がCO2またはNH3を含んでなる、請求項1〜10のいずれか一項に記載の方法。
- 溶媒が、アルコール類、水またはそれらの混合液から選択される、請求項1〜11のいずれか一項に記載の方法。
- 誘電化合物のマトリックスと、
前記マトリックス中における被覆された強誘電化合物粒子とを含んでなる複合材であって、
前記誘電化合物マトリックスがAl 2 O 3 の粒子から形成されており、強誘電粒子がBa x Sr 1−x TiO 3 (0<x<1)から形成され、Al 2 O 3 の粒子が前記被覆された強誘電化合物粒子で形成された隙間に分配されてなる、高密度複合材。 - 強誘電粒子がBa 0.6 Sr 0.4 TiO3から形成されている、請求項13に記載の材料。
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US8441965B2 (en) * | 2010-08-05 | 2013-05-14 | Apple Inc. | Methods and apparatus for reducing data transmission overhead |
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FR2861088B1 (fr) | 2006-01-20 |
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EP1812619B1 (fr) | 2010-09-22 |
EP1812619A2 (fr) | 2007-08-01 |
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