JP2005306662A - 誘電体セラミックス粉末の製造方法及び複合誘電体材料の製造方法 - Google Patents
誘電体セラミックス粉末の製造方法及び複合誘電体材料の製造方法 Download PDFInfo
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Abstract
【課題】 粉砕法による粉末を用いた場合であっても、樹脂との混合物の流動性を確保することのできる誘電体セラミックス粉末の製造方法を提供する。
【解決手段】 原料組成物を第1温度に保持することにより第1焼成物を得る第1焼成工程と、第1焼成物を粉砕して第1粉砕物を得る第1粉砕工程と、第1粉砕物を第1温度よりも低い第2温度に保持することにより第2焼成物を得る第2焼成工程と、第2焼成物を粉砕して第2粉砕物を得る第2粉砕工程と、を備える誘電体セラミックス粉末の製造方法により、樹脂との混合物の流動性を確保するのはもちろん、優れた誘電特性の複合誘電体材料を得ることができる。
【選択図】なし
Description
本発明の誘電体セラミックス粉末の製造方法において、第2粉砕物を複合誘電体材料用のフィラーとして用いることができる。複合誘電体基板の厚さが薄い場合には、粒径の大きな粒子が存在すると表面粗度が粗くなるおそれがあるため、第2粉砕物の最大粒径を10μm以下にすることが好ましい。
また、本発明の誘電体セラミックス粉末の製造方法においては、第1粉砕工程及び第2粉砕工程を気流式粉砕機で行うことが所定の比表面積、格子歪を得る上で好ましい。
本発明の誘電体セラミックス粉末の製造方法は、第1焼成工程及び第2焼成工程と、少なくとも2つの焼成工程を備えている。第1焼成工程と第2焼成工程は以下説明するように保持温度が異なる。
第1焼成工程は、原料組成物同士の反応を十分に進行させるために、第2焼成工程よりも高い温度で焼成を行う。望ましい温度範囲は、1300〜1650℃である。1300℃未満では原料組成物同士の反応を十分に進行させることができないためであり、また、1650℃を超えると原料組成物が溶融するおそれがある。なお、この保持温度は、対象となるセラミックスの材質に応じて設定する必要がある。具体的な組成物に対する適切な温度範囲は後述する。第1焼成工程における保持時間は、0.5〜10時間の範囲とすることが好ましい。0.5時間未満では原料組成物同士の反応を十分に進行させることができないためであり、また10時間を超えてもそれ以上反応の進行を期待することができないためである。
原料粉末から構成される場合、原料組成物は、異なる組成を有する複数の化合物を含んでいる。例えば、チタン酸バリウムを得たい場合には、原料組成物は、所定量に秤量されたBaCO3粉末(原料粉末)とTiO2粉末(原料粉末)を含み、さらに副成分を含む場合がある。チタン酸バリウムの場合、第1焼成工程は、BaCO3粉末とTiO2粉末の反応を十分に進行させることを目的としている。
仮焼き物が原料組成物を構成する場合、仮焼き物に対して副成分を添加した後に粉砕し、得られた粉砕物を第1焼成工程に供することができる。仮焼き物は、異なる組成を有する複数の化合物からなる混合物を所定の温度に保持することにより得ることができる。
なお、本発明における比表面積は、密度の異なる粒子同士の比較を行うために下記式(1)に基づいて単位体積あたりの値に換算している。
SSA(m2/cm3)=SSA(m2/g)×ρ(g/cm3)…(1)
SSA(m2/g):BET法により測定した粒子の比表面積
ρ:比重ビンを用いて測定した粒子の密度
本発明における格子歪はHallの方法、つまり下記式(2)に基づいて求めるものとする。
βcosθ/λ=2η(sinθ/λ)+K/D…(2)
β:積分幅、
θ:回折線のブラッグ角、
η:格子歪、
D:結晶子サイズ、
K:Schrrer定数、
λ:X線波長(CuKα1、1.54056Å)
式(2)においてηは、図1に示すように粉末X線回折パターンからピーク位置(2θ)とピークの積分幅(β)を求め、さらに図2のグラフのようにプロットして得た直線の傾きを2で割って求める。
なお、本発明による格子歪の測定条件は下記の通りである。
装置:RINT2500(株式会社リガク製)
電流−電圧:50kV−300mA、
2θ:20〜80°、
スキャン速度:1°/min、
サンプリング間隔:0.002°、
発散スリット:1/2°、
散乱スリット:1/2°、
受光スリット:開放
さらに、Ba(Mg,Nb)O3系セラミックス、Ba(Mg,Ta)O3系セラミックス、Ba(Co,Mg,Nb)O3系セラミックス、Ba(Co,Mg,Ta)O3系セラミックスについて適用することもできる。
本発明に適用する誘電体セラミックスは、複合ペロブスカイト系セラミックスが好ましく、その中でも(Ba,Sr)系セラミックス、(Ba,Ca)系セラミックス、(Sr,Ca)TiO3系セラミックス又は(Ba,Sr,Ca)TiO3系セラミックスであることが好ましい。他の組成に比べて、高い誘電率(ε)を得ることができるからである。この好ましい誘電体セラミックスについては、副成分として、A(ただし、AはMn、Crから選ばれる1種または2種の元素)の酸化物、X(ただし、XはV、Nb、W、Ta及びMoから選択される1種又は2種以上の元素)の酸化物、Rの酸化物(ただし、RはSc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb及びLuから選択される1種又は2種以上の元素)SiO2 、MO(ただし、MはBa、Ca、Sr及びMgから選択される1種又は2種以上の元素)、Li2 O、B2 O3及びMSiO3から選択される1種又は2種以上の化合物を含有することができる。
1250〜1450℃:チタン酸バリウム系セラミックス、チタン酸ストロンチウム系セラミックス、チタン酸カルシウム系セラミックス、チタン酸鉛系セラミックス、チタン酸ビスマス系セラミックス、チタン酸バリウム−錫系セラミックス、鉛−カルシウム系セラミックス、Ba−希土類元素−Ti系セラミックス(Ba−Nd−Ti系セラミックス、Ba−Sm−Ti系セラミックス)、二酸化チタン系セラミックス、(Ba,Sr)系セラミックス、(Ba,Ca)系セラミックス、(Sr,Ca)TiO3系セラミックス、(Ba,Sr,Ca)TiO3系セラミックス
1500〜1650℃:アルミナ系セラミックス、Ba(Mg,Nb)O3系セラミックス、Ba(Mg,Ta)O3系セラミックス、Ba(Co,Mg,Nb)O3系セラミックス、Ba(Co,Mg,Ta)O3系セラミックス
以上のようにして得た誘電体セラミック粉末を、有機樹脂材料と混合することで複合誘電体材料が得られるが、本発明による複合誘電体材料は、以下のような製造方法に従うことが好ましい。まず、誘電体セラミック粉末と有機樹脂材料を所定量ずつ秤量して混合する。混合は、例えば、混練機等を使用しての乾式混合によっても行えるが、ボールミル、攪拌機等を使用して、トルエン、キシレン等の有機溶剤中で充分に混合するのが好ましい。この混合時には、後述する可撓性付与材、カップリング剤、及び反応開始剤を添加しても良い。このようにして得られたスラリーを例えば60〜150℃で乾燥し、誘電体セラミック粉末と有機樹脂材料の混合物からなる複合誘電体材料の前駆体を得る。この前駆体を用いて例えば100〜300℃で所望の形状にプレス成形する。この際、前駆体はシート形状のままでもよいし、粉末状としてもよい。さらに、有機樹脂材料に熱硬化性樹脂を用いる場合には、この成形物を例えば100〜250℃の温度で硬化処理する。この硬化に際しては、後述する補強材を存在させてもよい。
複合誘電体材料中の補強材の含有量は、10〜30wt%の範囲であることが好ましい。より好ましくは15〜25wt%である。
SrCO3粉末、CaCO3粉末及びTiO2粉末を、焼成後に表1に示す主成分となるように秤量し、湿式ボールミルにて16時間だけ混合、粉砕した。次いで、混合された原料粉末を1200℃で2時間保持する仮焼きを行った。
次に、得られた仮焼き物(一部については表1に示す副成分を添加)を湿式ボールミルにて16時間だけ粉砕した。得られた粉砕粉末を表1に示す条件の第1焼成を行った後に、目開き1mmのメッシュを通過するまで乳鉢を用いて粗粉砕し、次いで気流式粉砕機で微粉砕(第1粉砕)を行って第1粉砕物を得た。
次に、第1粉砕物を表1に示す条件の第2焼成を行った後に、目開き1mmのメッシュを通過するまで乳鉢を用いて粗粉砕し、次いで気流式粉砕機で微粉砕(第2粉砕)を行って第2粉砕物を得た。
次に、いくつかの第2粉砕物については、表1に示す条件の第3焼成を行った後に、目開き1mmのメッシュを通過するまで乳鉢を用いて粗粉砕し、次いで気流式粉砕機で微粉砕(第3粉砕)を行って第3粉砕物を得た。
第1焼成を1200℃の温度で行う(試料No.1〜3)か又は第1焼成の温度が1400℃であっても第2焼成を1200℃(試料No.5、6)で行うと、得られる誘電体セラミックス粉末は、比表面積が9m2/cm3以下、格子歪が0.2以下という所望の特性を得ることができる。これに対して、焼成を1400℃の温度による第1焼成のみとすると、比表面積が9m2/cm3を超え、かつ格子歪も0.2を超えてしまう。そのために、最低溶融粘度が750Pa・sまで達してしまう。
比表面積、格子歪が所望の特性が得られている試料No.1〜3と試料No.5とを比較すると、1400℃で第1焼成を行った後に1200℃で第2焼成を行った試料No.5、6の方が、複合誘電体材料としてのQ値及び誘電率の温度特性(τε)が優れていることがわかる。
Claims (7)
- 原料組成物を第1温度に保持することにより第1焼成物を得る第1焼成工程と、
前記第1焼成物を粉砕して第1粉砕物を得る第1粉砕工程と、
前記第1粉砕物を前記第1温度よりも低い第2温度に保持することにより第2焼成物を得る第2焼成工程と、
前記第2焼成物を粉砕して第2粉砕物を得る第2粉砕工程と、
を備えることを特徴とする誘電体セラミックス粉末の製造方法。 - 前記第1焼成工程における前記第1温度は1300〜1650℃、前記第2焼成工程における前記第2温度は1100〜1300℃であることを特徴とする請求項1に記載の誘電体セラミックス粉末の製造方法。
- 前記第2粉砕工程により得られる前記第2粉砕物は、最大粒径が10μm以下であることを特徴とする請求項1又は2に記載の誘電体セラミックス粉末の製造方法。
- 前記第1粉砕工程及び前記第2粉砕工程は、気流式粉砕機を用いて行うことを特徴とする請求項1〜3のいずれかに記載の誘電体セラミックス粉末の製造方法。
- 前記誘電体セラミックス粉末が複合ペロブスカイト系セラミックスであることを特徴とする請求項1〜4のいずれかに記載の誘電体セラミックス粉末の製造方法。
- 前記複合ペロブスカイト系セラミックスが、(Ba,Sr)系セラミックス、(Ba,Ca)系セラミックス、(Sr,Ca)TiO3系セラミックス又は(Ba,Sr,Ca)TiO3系セラミックスであることを特徴とする請求項5に記載の誘電体セラミックス粉末の製造方法。
- 誘電体セラミックス粉末と、前記誘電体セラミックス粉末を保持する有機樹脂材料とを含む複合誘電体材料の製造方法であって、
前記誘電体セラミックス粉末は、
原料組成物を第1温度に保持することにより第1焼成物を得る第1焼成工程と、
前記第1焼成物を粉砕して第1粉砕物を得る第1粉砕工程と、
前記第1粉砕物を前記第1温度よりも低い第2温度に保持することにより第2焼成物を得る第2焼成工程と、
前記第2焼成物を粉砕して第2粉砕物を得る第2粉砕工程と、を経ることにより作製されることを特徴とする複合誘電体材料の製造方法。
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US11/110,652 US20050237695A1 (en) | 2004-04-21 | 2005-04-20 | Method for producing dielectric ceramic powder and method for producing composite dielectric material |
TW094112580A TWI304055B (en) | 2004-04-21 | 2005-04-20 | Method for producing dielectric ceramic powder and method for producing composite dielectric material |
KR1020050032838A KR100634915B1 (ko) | 2004-04-21 | 2005-04-20 | 복합유전체재료의 제조방법 |
CNB2005100666507A CN1323052C (zh) | 2004-04-21 | 2005-04-21 | 电介质陶瓷粉末的制造方法和复合电介质材料的制造方法 |
EP05008752A EP1589065A1 (en) | 2004-04-21 | 2005-04-21 | Method for producing dielectric ceramic powder and method for producing composite dielectric material |
KR1020060073883A KR100642148B1 (ko) | 2004-04-21 | 2006-08-04 | 유전체 세라믹분말의 제조방법 |
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JP2008260674A (ja) * | 2007-03-20 | 2008-10-30 | Ngk Insulators Ltd | 圧電/電歪磁器組成物の製造方法 |
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JP2007161835A (ja) * | 2005-12-13 | 2007-06-28 | Toray Ind Inc | 誘電性樹脂組成物およびそれから得られる成形品 |
JP2008260674A (ja) * | 2007-03-20 | 2008-10-30 | Ngk Insulators Ltd | 圧電/電歪磁器組成物の製造方法 |
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US20050237695A1 (en) | 2005-10-27 |
KR100642148B1 (ko) | 2006-11-10 |
CN1690015A (zh) | 2005-11-02 |
KR20060047287A (ko) | 2006-05-18 |
EP1589065A1 (en) | 2005-10-26 |
TWI304055B (en) | 2008-12-11 |
CN1323052C (zh) | 2007-06-27 |
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