JP2013155071A - 誘電体セラミック材料及びそれに用いるペロブスカイト型複合酸化物粗粒子の製造方法 - Google Patents
誘電体セラミック材料及びそれに用いるペロブスカイト型複合酸化物粗粒子の製造方法 Download PDFInfo
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- JP2013155071A JP2013155071A JP2012016507A JP2012016507A JP2013155071A JP 2013155071 A JP2013155071 A JP 2013155071A JP 2012016507 A JP2012016507 A JP 2012016507A JP 2012016507 A JP2012016507 A JP 2012016507A JP 2013155071 A JP2013155071 A JP 2013155071A
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- perovskite
- dielectric
- ceramic material
- dielectric ceramic
- complex oxide
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Abstract
【解決手段】平均粒子径が8μm以上50μm以下でBET比表面積が0.3m2/g以上1.0m2/g以下であるペロブスカイト(ABO3)型複合酸化物粗粒子と、平均粒子径が0.7μm以上3μm以下でBET比表面積が0.6m2/g以上3m2/g以下であるペロブスカイト(ABO3)型複合酸化物微粒子とからなる誘電体セラミック材料である。
【選択図】図1
Description
従来、高誘電率材料としては、セラミック粉末を成形した後、これを焼成して得られるセラミック焼結体を用いているため、その寸法や形状は成形法により制約を受けた。また、焼結体は高硬度で脆性であるため、自由な加工が困難であり、任意の形状や複雑な形状を得るには困難を極めた。
特許文献1では、粒子径が比較的大きな多孔質のペロブスカイト型複合酸化物粒子を用いているため、ハンドリング性に問題が生じることはないが、樹脂中に充填できる量がせいぜい30体積%程度であり、得られる複合誘電体の誘電率が低いという問題があった。
即ち、本発明に係る誘電体セラミック材料は、平均粒子径が8μm以上50μm以下でBET比表面積が0.3m2/g以上1.0m2/g以下であるペロブスカイト(ABO3)型複合酸化物粗粒子と平均粒子径が0.7μm以上3μm以下でBET比表面積が0.6m2/g以上3m2/g以下であるペロブスカイト(ABO3)型複合酸化物微粒子とからなるものである。
ペロブスカイト型複合酸化物粗粒子の平均粒子径が8μm未満であると、焼成時に粒子同士の融着が進行して解砕を強力に行う必要を要し、ひいては結晶性低減や微細粒子を発生するなど不具合を生じ、一方、平均粒子径が50μm超であると、最大径が100μmを超え、樹脂との複合化において厚みに関する自由度を失い、用途が大幅に制限される。好ましくは、ペロブスカイト型複合酸化物粗粒子の平均粒子径は10μm〜30μmである。更に、ペロブスカイト型複合酸化物粗粒子のBET比表面積が0.3m2/g未満であると、樹脂複合時の誘電率を効率的に発現しにくくなり、一方、BET比表面積が1.0m2/g超であると、解砕時の粒子崩壊や微粒子発生を生じたり、樹脂への分散自体にも困難を生じる。好ましくは、ペロブスカイト型複合酸化物粗粒子のBET比表面積は0.4m2/g〜0.7m2/gである。
また、ペロブスカイト型複合酸化物微粒子の平均粒子径が0.7μm未満であると、粒子自身の結晶性も低く、誘電率向上に対して不利となり、一方、平均粒子径が3μm超であると、粗粒子間に存在して分散性を向上させる上で妨げとなる。好ましくは、ペロブスカイト型複合酸化物微粒子の平均粒子径は1μm〜2μmである。更に、ペロブスカイト型複合酸化物微粒子のBET比表面積が0.6m2/g未満であると、樹脂複合時に効率の良い誘電率向上が困難になり、一方、BET比表面積が3m2/g超であると、樹脂への分散性が悪くなり、複合体の機械的強度を低減させるなど不具合を生じ易くなる。好ましくは、ペロブスカイト型複合酸化物微粒子のBET比表面積は0.8m2/g〜2m2/gである。
なお、本発明における平均粒子径とは、レーザー光散乱法により求められる値である。
中でも、ペロブスカイト型複合酸化物粗粒子については、固相法を利用して製造することが工業的観点から望ましい。ペロブスカイト型複合酸化物粗粒子を製造する具体的な方法は、Ba、Ca、Mg及びSrからなる群から選択される少なくとも1種の元素を含む炭酸塩と、Ti及びZrからなる群から選択される少なくとも1種の元素を含む酸化物と、分散媒とを含むスラリーを調製し、このスラリーをスプレードライ法で乾燥させて造粒粉を得、この造粒粉を焼成すればよい。造粒粉の焼成温度を1000℃〜1400℃の範囲で調整することで、0.3m2/g〜1.0m2/gのBET比表面積を有するペロブスカイト型複合酸化物粗粒子を得ることができる。
また、メディアミルによる処理は、スラリー中の固形分の平均粒子径が0.8μm以下、好ましくは0.1μm〜0.6μmで、最大粒子径が3μm以下となるように行うことが、粒子間の空隙の状態を制御しながら、上記範囲の平均粒子径とBET比表面積のものを容易に得ることができ、また、誘電特性にも優れたペロブスカイト型複合酸化物粗粒子が得られる観点から好ましい。
メディアミルとしては、ビーズミル、ボールミル、ペイントシェーカー、アトライタ、サンドミル等を用いることができる。特にビーズミルを用いることが好ましい。その場合、運転条件やビーズの種類及び大きさは、装置のサイズや処理量、使用する原料の種類に応じて適切に選択すればよい。
本発明における複合誘電体は、後述する高分子材料に上述した誘電体セラミック材料を好ましくは30体積%〜60体積%、より好ましくは40体積%〜55体積%充填することができる。誘電体セラミック材料を充填率が低過ぎると、高い誘電率が得られず、一方、充填率が高過ぎると、機械的特性及び電気絶縁性の低下が懸念される。しかし、本発明の誘電体セラミック材料は、特許文献2よりも低い充填率で同程度の誘電率を達成することができる(後述する実施例を参照)。
熱硬化性樹脂としては、例えば、エポキシ樹脂、フェノール樹脂、ポリイミド樹脂、メラミン樹脂、シアネート樹脂類、ビスマレイミド類、ビスマレイミド類とジアミンとの付加重合物、多官能性シアン酸エステル樹脂、二重結合付加ポリフェニレンオキサイド樹脂、不飽和ポリエステル樹脂、ポリビニルベンジルエーテル樹脂、ポリブタジエン樹脂、フマレート樹脂等の公知のものが挙げられる。これらの熱硬化性樹脂は、1種単独で使用してもよいし、2種以上を組み合わせて使用してもよい。これら熱硬化性樹脂の中でも、耐熱性、加工性、価格等のバランスからエポキシ樹脂及びポリビニルベンジルエーテル樹脂が好ましい。
エポキシ樹脂硬化剤の配合量は、エポキシ樹脂に対して、当量比で好ましくは0.1〜10、より好ましくは0.7〜1.3の範囲である。
また、硬化の調整のために、ハイドロキノン、ベンゾキノン、銅塩等を配合してもよい。
複合誘電体ペーストを基材上に塗布した後、乾燥することによりフィルム状に成形することができる。基材としては、例えば、表面に剥離処理がなされたプラスチックフィルムを用いることができる。剥離処理が施されたプラスチックフィルム上に塗布してフィルム状に成形した場合、一般には成形後、フィルムから基材を剥離して用いることが好ましい。基材として用いることができるプラスチックフィルムとしては、ポリエチレンテレフタレート(PET)フィルム、ポリエチレンフィルム、ポリプロピレンフィルム、ポリエステルフィルム、ポリイミドフィルム、アラミド、カプトン、ポリメチルペンテン等のフィルムを挙げることができる。また、基材として用いるプラスチックフィルムの厚みとしては、1μm〜100μmであることが好ましく、さらに好ましくは1μm〜40μmである。また、基材表面上に施す離型処理としては、シリコーン、ワックス、フッ素樹脂等を表面に塗布する離型処理が好ましく用いられる。
押出成形した誘電体フィルムは、上記の基材上に押し出されるように成形されてもよい。また、基材として、金属箔を用いる場合、金属箔としては、銅、アルミニウム、真鍮、ニッケル、鉄等を材料とする箔の他、これらの合金の箔、複合箔等を用いることができる。金属箔には、必要時に応じて表面粗面化の処理や、接着剤の塗布等の処理を施しておいてもよい。
<製造例1:ペロブスカイト型複合酸化物粗粒子(BaCaTiZr系)>
容器に水を仕込み、撹拌しながら粉末濃度が20〜30重量%となるよう、また所定の複合酸化物組成となるよう炭酸バリウム、炭酸カルシウム、酸化チタン及び酸化ジルコニウムを仕込み、1時間以上撹拌してスラリーを得た。このスラリーをビーズミルにて、レーザー光散乱法で求めた固形分の平均粒子径が0.47μm、粒度分布の最大径が3μm以下となるよう処理した。このスラリーを、スプレーバッグドライヤーを用いて造粒乾燥処理し、球状の造粒粉とした。なお、球状の造粒粉はレーザー光散乱法で求められる平均粒子径が33.4μmであった。スプレーバッグドライヤーのスラリー射出仕様は100mmφのディスクで20,000rpmとし、乾燥室温度は105℃とした。得られた造粒粉を気孔率20%以上のアルミナ系容器に仕込み、1225℃で20時間焼成を行った。得られた焼成体をコーヒーミルで解砕し、目開き100μmの篩を通して、球状の複合ペロブスカイト粒子を得た。得られた複合ペロブスカイト粒子は、22.5μmの平均粒子径(D50)、0.62m2/gのBET比表面積及び1.003のA/B比((BaO+CaO)/(TiO2+ZrO2)のモル比)を有するBa(0.981)Ca(0.020)Ti(0.848)Zr(0.150)O3であった。なお、複合ペロブスカイト粒子の平均粒子径はレーザー光散乱法で求めた。
焼成温度を1250℃に変更した以外は製造例1と同様にして球状の複合ペロブスカイト粒子を得た。得られた複合ペロブスカイト粒子は、21.5μmの平均粒子径(D50)、0.85m2/gのBET比表面積及び1.000のA/B比((BaO+CaO)/(TiO2+ZrO2)のモル比)を有するBa(0.980)Ca(0.020)Ti(0.849)Zr(0.151)O3あった。なお、複合ペロブスカイト粒子の平均粒子径はレーザー光散乱法で求めた。
容器に水を仕込み、所定量の分散剤(花王株式会社製ポイズ2100)を添加し、撹拌しながら粉末濃度が20〜30重量%となるよう、また所定の複合酸化物組成となるようチタン酸バリウム前駆体、炭酸バリウム、炭酸カルシウム及び酸化ジルコニウムを仕込み、1時間以上撹拌してスラリーを得た。このスラリーをビーズミルにて、レーザー光散乱法で求めた固形分の平均粒子径が0.54μm、粒度分布の最大径が3μm以下となるよう処理した。このスラリーを、スプレーバッグドライヤーを用いて造粒乾燥処理し、球状の造粒粉とした。なお、球状の造粒粉はレーザー光散乱法で求められる平均粒子径が30.3μmであった。スプレーバッグドライヤーのスラリー射出仕様は100mmφのディスクで20,000rpmとし、乾燥室温度は105℃とした。得られた造粒粉を気孔率20%以上のアルミナ系容器に仕込み、1175℃で20時間焼成を行った。得られた焼成体をコーヒーミルで解砕し、目開き100μmの篩を通して、球状の複合ペロブスカイト粒子を得た。得られた複合ペロブスカイト粒子は、21.4μmの平均粒子径(D50)、0.62m2/gのBET比表面積及び1.001のA/B比((BaO+CaO)/(TiO2+ZrO2)のモル比)を有するBa(0.980)Ca(0.020)Ti(0.851)Zr(0.149)O3であった。
なお、ここで使用したチタン酸バリウム前駆体は、蓚酸塩法チタン酸バリウム合成の出発原料となる蓚酸バリウムチタニルを脱蓚酸し、さらに気流粉砕を行って得られたものである。この、チタン酸バリウム前駆体は、2.8μmの平均粒子径(D50)及び7.7m2/gのBET比表面積を有するものであった。
また、複合ペロブスカイト粒子及びチタン酸バリウム前駆体の平均粒子径はレーザー光散乱法で求めた。
焼成温度を1200℃に変更した以外は製造例3と同様にして球状の複合ペロブスカイト粒子を得た。得られた複合ペロブスカイト粒子は、20.4μmの平均粒子径(D50)、0.49m2/gのBET比表面積及び1.001のA/B比((BaO+CaO)/(TiO2+ZrO2)のモル比)を有するBa(0.980)Ca(0.020)Ti(0.851)Zr(0.149)O3であった。なお、複合ペロブスカイト粒子の平均粒子径はレーザー光散乱法で求めた。
容器に水を仕込み、所定量の分散剤(花王株式会社製ポイズ2100)を添加し、撹拌しながら粉末濃度が20〜30重量%となるよう、チタン酸バリウム前駆体を仕込み、1時間以上撹拌してスラリーを得た。このスラリーをビーズミルにて、レーザー光散乱法で求められる固形分の平均粒子径が0.51μm、粒度分布の最大径が3μm以下となるよう処理した。このスラリーを、スプレーバッグドライヤーを用いて造粒乾燥処理し、球状の造粒粉とした。なお、球状の造粒粉はレーザー光散乱法で求められる平均粒子径が32.9μmであった。スプレーバッグドライヤーのスラリー射出仕様は100mmφのディスクで20,000rpmとし、乾燥室温度は105℃とした。得られた造粒粉を気孔率20%以上のアルミナ系容器に仕込み、1100℃で20時間焼成を行った。得られた焼成体をコーヒーミルで解砕し、目開き100μmの篩を通して、球状のチタン酸バリウム粒子を得た。得られたチタン酸バリウム粒子は、19.2μmの平均粒子径(D50)、0.62m2/gのBET比表面積及び0.999のA/B比(BaO/TiO2のモル比)を有するものであった。
なお、ここで使用したチタン酸バリウム前駆体は、蓚酸塩法チタン酸バリウム合成の出発原料となる蓚酸バリウムチタニルを脱蓚酸し、さらに気流粉砕を行って得られたものである。この、チタン酸バリウム前駆体は、2.8μmの平均粒子径(D50)及び7.7m2/gのBET比表面積を有するものであった。
また、球状のチタン酸バリウム粒子及びチタン酸バリウム前駆体の平均粒子径はレーザー光散乱法で求めた。
焼成温度を1150℃に変更した以外は製造例5と同様にして球状のチタン酸バリウム粒子を得た。得られたチタン酸バリウム粒子は、15.3μmの平均粒子径(D50)、0.40m2/gのBET比表面積及び0.999のA/B比(BaO/TiO2のモル比)を有するものであった。なお、チタン酸バリウム粒子の平均粒子径はレーザー光散乱法で求めた。
焼成温度を1000℃に変更した以外は製造例5と同様にして球状のチタン酸バリウム粒子を得た。得られたチタン酸バリウム粒子は、18.9μmの平均粒子径(D50)、0.96m2/gのBET比表面積及び1.001のA/B比(BaO/TiO2のモル比)を有するものであった。なお,チタン酸バリウム粒子の平均粒子径はレーザー光散乱法で求めた。
蓚酸バリウムチタニルを脱蓚酸した後、気孔率20%以上のムライト製容器に仕込み、950℃で20時間の焼成を行なった。焼成粉末に対し気流粉砕を行い、平均粒子径0.75μm、BET比表面積2.0m2/gのチタン酸バリウムを得た。このチタン酸バリウムを同様にムライト製容器に仕込み、1100℃で20時間の焼成を行なった。焼成粉末に対し気流粉砕を行い、球状のチタン酸バリウム粒子を得た。得られたチタン酸バリウム粒子は、1.9μmの平均粒子径(D50)、0.90m2/gのBET比表面積及び1.001のA/B比(BaO/TiO2のモル比)を有するものであった。なお、球状のチタン酸バリウム粒子の平均粒子径はレーザー光散乱法で求めた。
表1に示すような重量割合で、上記製造例で得られたペロブスカイト型複合酸化物粗粒子及びペロブスカイト型複合酸化物微粒子を市販のミキサーで混合し、実施例1〜7の誘電体セラミック材料を得た。
なお、ここで使用したエポキシ樹脂は、99重量%の熱硬化性エポキシ樹脂(三菱化学株式会社製、商品名:JER(登録商標)828EL、分子量約370、比重1.17、25℃での公称粘度120〜150P)と、1重量%のイミダゾール系硬化促進剤(四国化成工業株式会社製、商品名:2E4MZ)とからなるものである。
Claims (9)
- 平均粒子径が8μm以上50μm以下でBET比表面積が0.3m2/g以上1.0m2/g以下であるペロブスカイト(ABO3)型複合酸化物粗粒子と平均粒子径が0.7μm以上3μm以下でBET比表面積が0.6m2/g以上3m2/g以下であるペロブスカイト(ABO3)型複合酸化物微粒子とからなることを特徴とする誘電体セラミック材料。
- 前記ペロブスカイト型複合酸化物粗粒子が、Ba、Ca、Mg及びSrからなる群から選択される少なくとも1種の元素を含む炭酸塩と、Ti及びZrからなる群から選択される少なくとも1種の元素を含む酸化物と、分散媒とを含むスラリーを調製し、このスラリーをスプレードライ法で乾燥させて造粒粉を得、この造粒粉を焼成して得られたもの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材料。
- 前記スラリーが、チタン酸バリウム前駆体を更に含むことを特徴とする請求項2に記載の誘電体セラミック材料。
- 前記ペロブスカイト型複合酸化物粗粒子の配合割合が、10重量%以上70重量%以下であり且つ前記ペロブスカイト型複合酸化物微粒子の配合割合が、30重量%以上90重量%以下であることを特徴とする請求項1〜3の何れか一項に記載の誘電体セラミック材料。
- 前記ペロブスカイト型複合酸化物微粒子が、Aサイト元素がBa、Ca、Mg及びSrからなる群から選択される少なくとも1種であり且つBサイト元素がTi及びZrからなる群から選択される少なくとも1種であるABO3型複合酸化物からなることを特徴とする請求項1〜4の何れか一項に記載の誘電体セラミック材料。
- 前記ペロブスカイト型複合酸化物粗粒子が、焼結助剤を含有しないことを特徴とする請求項1〜5の何れか一項に記載の誘電体セラミック材料。
- 複合誘電体の無機充填材として用いられることを特徴とする請求項1〜6の何れか一項に記載の誘電体セラミック材料。
- Ba、Ca、Mg及びSrからなる群から選択される少なくとも1種の元素を含む炭酸塩と、Ti及びZrからなる群から選択される少なくとも1種の元素を含む酸化物と、分散媒とを含むスラリーを調製する工程、
前記スラリーをスプレードライ法で乾燥させて造粒粉を得る工程、及び
前記造粒粉の焼成温度を1000℃以上1400℃以下の範囲で調整し、BET比表面積が0.3m2/g以上1.0m2/g以下である焼成体を得る工程
を有することを特徴とするペロブスカイト型複合酸化物粗粒子の製造方法。 - 前記スラリーが、チタン酸バリウム前駆体を更に含むことを特徴とする請求項8に記載のペロブスカイト型複合酸化物粗粒子の製造方法。
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