JP4678022B2 - 誘電体磁器組成物の製造方法 - Google Patents
誘電体磁器組成物の製造方法 Download PDFInfo
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- JP4678022B2 JP4678022B2 JP2007304577A JP2007304577A JP4678022B2 JP 4678022 B2 JP4678022 B2 JP 4678022B2 JP 2007304577 A JP2007304577 A JP 2007304577A JP 2007304577 A JP2007304577 A JP 2007304577A JP 4678022 B2 JP4678022 B2 JP 4678022B2
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
- C04B2235/786—Micrometer sized grains, i.e. from 1 to 100 micron
Description
第1に、内部電極の材料であるNiなどの卑金属の融点以上、あるいはそれに近い温度域となり、その結果、誘電体磁器組成物とともに同時焼成される卑金属粒子の溶融、球状化が進み、内部電極層のライン性が劣化する、すなわち内部電極層に途切れを発生するといった不都合を生じる要因ともなる。内部電極層のライン性が悪化すると、得られるコンデンサの比誘電率が低下し、結果的に静電容量の低下を招き、最終的には高容量化・薄層化に対応できない。
組成式〔(CaxSr1−x)O〕m〔(TiyZr1−y−zHfz)O2 〕(式中、x、y、z、mは、それぞれ0.5≦x≦1.0、0.01≦y≦0.10、0<z≦0.20、0.90≦m≦1.04である)である誘電体酸化物と、酸化マンガンと、酸化アルミニウムと、焼結助剤と、を有する誘電体磁器組成物を製造する方法であって、
SiO2 を主成分とし、さらにMO(ただし、Mは、Ba、Ca、Sr及びMgの少なくとも1種)を含む第1ガラス組成物と、
B2 O3 、Al2 O3 、ZnO及びSiO2 を含んで構成され、1.5μm以下の平均粒径を持つ第2ガラス組成物と、
を有する焼結助剤を用いて、誘電体磁器組成物を製造する方法が開示されている。
該誘電体酸化物100重量部に対し、焼結助剤を1〜10重量部混合する工程、および得られた混合物を焼成する工程を含む、誘電体磁器組成物の製造方法であって、
前記焼結助剤が、焼結助剤の全量100重量%中に、
酸化マンガン、炭酸マンガンまたはこれらの混合物を、MnO換算で30〜69重量%、
酸化アルミニウムを、Al2O3換算で1〜20重量%、
酸化ケイ素を、SiO2換算で30〜50重量%含んでなる、誘電体磁器組成物の製造方法。
該誘電体酸化物100重量部に対し、
焼結助剤を1〜10重量部および
酸化ナトリウム、炭酸ナトリウムまたはこれらの混合物を、Na2O換算で0.1〜0.5重量部の混合する工程、および
得られた混合物を焼成する工程を含む誘電体磁器組成物の製造方法であって、
前記焼結助剤が、焼結助剤の全量100重量%中に、
酸化マンガン、炭酸マンガンまたはこれらの混合物を、MnO換算で30〜69重量%、
酸化アルミニウムを、Al2O3換算で1〜20重量%、
酸化ケイ素を、SiO2換算で30〜50重量%含んでなる、誘電体磁器組成物の製造方法。
組成式〔(CaxSr1−x)O〕m〔(TiyZr1−y−zHfz)O2 〕にて示される。
yは、0.01≦y≦0.10、好ましくは0.02≦y≦0.07であり、
zは、0<z≦0.20、好ましくは0<z≦0.10であり、
mは、0.90≦m≦1.04、好ましくは1.005≦m≦1.035である。
まず、誘電体酸化物を製造するための出発原料として、平均粒径0.4μmのSrCO3、CaCO3、TiO2、ZrO2及びHfO2を準備した。
また、上記で得られた誘電体酸化物100重量部と、表1に示す配合の焼結助剤と、アクリル樹脂4.8重量部と、塩化メチレン40重量部と、酢酸エチル20重量部と、ミネラルスピリット6重量部と、アセトン4重量部とをボールミルで混合し、ペースト化し、誘電体層用ペーストを得た。なお、試料16〜30では、前記と同様の変更を行った。
得られた円盤状サンプルとコンデンササンプルを用いて、磁器特性(焼結密度、結晶粒径)、電気特性(絶縁抵抗IR、比誘電率ε)およびクラック発生率を下記の方法で評価した。結果を表4に示す。
焼結密度は、円盤状サンプルの寸法と質量とから算出した。焼結密度は、好ましくは4.5g/cm3 以上を良好とした。なお、焼結密度の値は、円盤状サンプル数n=10個を用いて測定した値の平均値から求めた。
誘電体層を構成する誘電体粒子(グレイン)の平均結晶粒径は、コンデンサのサンプルのSEM写真を用いるコード法により算出した。本実施例では、誘電体粒子の形状を便宜的に球と仮定して粒径を算出する。具体的には、まず、誘電体層の微細構造を示すSEM写真を用い、このSEM写真上に任意の直線を引き、この線が隣接する誘電体粒子同士の間に存在する粒界と交錯する点(交点)の数を求める。次に、求められた交点数から単位長さ当たりの粒界との交点の数PLを計算する。次に、得られたPLの値を用いて、コード長さL3を算出する。コード長さL3は1/PLで求められる。次に、得られたL3の値に1.5を乗じたL3×1.5により、誘電体粒子の平均結晶粒径を算出した。なお、用いたSEM写真の視野は23μm×30μmとし、1サンプルにつき5〜6枚の写真を用いて、それぞれの粒径を算出し、これらの平均値を平均結晶粒径とした。
絶縁抵抗IRは、次のようにして評価した。コンデンササンプルに対し、絶縁抵抗計(アドバンテスト社製R8340A)を用いて、25℃においてDC50Vをコンデンササンプルに60秒間印加した後の絶縁抵抗IR(単位はΩ)を測定した。絶縁抵抗IRは、1×1011Ω以上を良好とする。なお、絶縁抵抗IRの値は、コンデンササンプル数n=10個を用いて測定した値の平均値から求めた。
コンデンサの試料に対し、基準温度20℃において、デジタルLCRメータ(横河電機(株)製 YHP4274A)にて、周波数120Hz,入力信号レベル(測定電圧)0.5Vrms/μmの条件下で、静電容量Cを測定した。そして、得られた静電容量、積層セラミックコンデンサの誘電体厚みおよび内部電極同士の重なり面積から、比誘電率(単位なし)を算出した。比誘電率は、高いほど好ましい。
クラック発生率は次のように評価した。
Claims (2)
- 組成式〔(CaxSr1−x)O〕m〔(TiyZr1−y−zHfz)O2 〕(式中、x、y、z、mは、それぞれ0.5≦x≦1.0、0.01≦y≦0.10、0<z≦0.20、0.90≦m≦1.04である)で示される誘電体酸化物を調製する工程、
該誘電体酸化物100重量部に対し、焼結助剤を1〜5重量部混合する工程、および得られた混合物を焼成する工程を含む、誘電体磁器組成物の製造方法であって、
前記焼結助剤が、焼結助剤の全量100重量%中に、
酸化マンガン、炭酸マンガンまたはこれらの混合物を、MnO換算で45〜63重量%、
酸化アルミニウムを、Al2O3換算で2〜15重量%、
酸化ケイ素を、SiO2換算で35〜40重量%含んでなり、且つガラス成分を含まない誘電体磁器組成物の製造方法。 - 組成式〔(CaxSr1−x)O〕m〔(TiyZr1−y−zHfz)O2 〕(式中、x、y、z、mは、それぞれ0.5≦x≦1.0、0.01≦y≦0.10、0<z≦0.20、0.90≦m≦1.04である)で示される誘電体酸化物を調製する工程、
該誘電体酸化物100重量部に対し、
焼結助剤を1〜5重量部および
酸化ナトリウム、炭酸ナトリウムまたはこれらの混合物を、Na2O換算で0.1〜0.5重量部の混合する工程、および
得られた混合物を焼成する工程を含む誘電体磁器組成物の製造方法であって、
前記焼結助剤が、焼結助剤の全量100重量%中に、
酸化マンガン、炭酸マンガンまたはこれらの混合物を、MnO換算で45〜63重量%、
酸化アルミニウムを、Al2O3換算で2〜15重量%、
酸化ケイ素を、SiO2換算で35〜40重量%含んでなり、且つガラス成分を含まない誘電体磁器組成物の製造方法。
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