JP7128442B2 - 誘電体磁器組成物および積層セラミック電子部品 - Google Patents
誘電体磁器組成物および積層セラミック電子部品 Download PDFInfo
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- JP7128442B2 JP7128442B2 JP2018144529A JP2018144529A JP7128442B2 JP 7128442 B2 JP7128442 B2 JP 7128442B2 JP 2018144529 A JP2018144529 A JP 2018144529A JP 2018144529 A JP2018144529 A JP 2018144529A JP 7128442 B2 JP7128442 B2 JP 7128442B2
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Description
一般式ABO3(AはBa、SrおよびCaから選択される少なくとも1種、BはTi、ZrおよびHfから選択される少なくとも1種)で表される主成分と、希土類成分R(RはSc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Luから選ばれる少なくとも1種)とを含むコアシェル構造の誘電体粒子を含む誘電体磁器組成物であり、前記コアシェル構造のシェル部における平均希土類濃度Cが0.3atom%以上であり、前記誘電体粒子の最表面から10nm内側における希土類濃度と、前記誘電体粒子のコアシェル境界面から10nmシェル側における希土類濃度とから算出される希土類濃度勾配Sが、-0.010atom%/nm≦S≦0.009atom%/nmであることを特徴としている。
一般式ABO3(A、Bは前記と同じ)で表される主成分と、希土類成分R(Rは前記と同じ)とを含むコアシェル構造の誘電体粒子を含む誘電体磁器組成物であり、前記コアシェル構造のシェル部における平均希土類濃度Cが0.3atom%以上であり、前記誘電体粒子の最表面から10nm内側と、前記誘電体粒子のコアシェル境界面から10nmシェル側との間の領域における希土類濃度の標準偏差をσとしたときに、σ/C≦0.15であることを特徴としている。
<積層セラミックコンデンサ1>
図1に示すように、本発明の一実施形態に係る積層セラミックコンデンサ1は、誘電体層2と、内部電極層3とが交互に積層された構成のコンデンサ素子本体10を有する。この素子本体10の両端部には、素子本体10の内部で交互に配置された内部電極層3と各々導通する一対の外部電極4が形成してある。素子本体10の形状に特に制限はないが、通常、直方体状とされる。また、その寸法にも特に制限はなく、用途に応じて適当な寸法とすればよい。
誘電体層2は、本実施形態に係る誘電体磁器組成物から構成されている。該誘電体磁器組成物は、主成分として、一般式ABO3 (Aは、Ba、CaおよびSrからなる群から選ばれる少なくとも1つであり、Bは、Ti、ZrおよびHfからなる群から選ばれる少なくとも1つである)で表され、ペロブスカイト型結晶構造を有する化合物から成る主成分を含有する。さらに、副成分として、希土類成分R(RはSc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Luから選ばれる少なくとも1種)の酸化物を含有する。なお、酸素(O)量は、上記式の化学量論組成から若干偏倚してもよい。
図2には、図1の誘電体層の要部拡大断面図を示す。本実施形態の誘電体層は、ABO3が主成分である誘電体粒子により構成され、誘電体粒子には副成分の希土類元素が固溶している。すべての誘電体粒子が、いわゆるコアシェル構造の粒子21であることが好ましいが、完全固溶系の粒子20が含まれていても良い。なお、本実施形態では、誘電体磁器組成物におけるコアシェル構造の確認およびその組成分析については、誘電体層の断面観察により行う。切断面が誘電体粒子の表面近傍であると、シェル部のみしか観察されないことがある。本実施形態では、希土類濃度の測定は、明確にコアが観察できるコアシェル粒子21について行う。
内部電極層3に含有される導電材は特に限定されないが、本実施形態では、NiまたはNi合金が好ましい。Ni合金としては、Mn,Cr,CoおよびAlから選択される1種以上の元素とNiとの合金が好ましく、合金中のNi含有量は95重量%以上であることが好ましい。なお、NiまたはNi合金中には、P等の各種微量成分が0.1重量%程度以下含まれていてもよい。内部電極層3の厚さは用途等に応じて適宜決定すればよい。
外部電極4に含有される導電材は特に限定されないが、本発明では安価なNi,Cuや、これらの合金を用いることができる。外部電極4の厚さは用途等に応じて適宜決定すればよい。
本実施形態の積層セラミックコンデンサ1は、従来の積層セラミックコンデンサと同様に、ペーストを用いた通常の印刷法やシート法によりグリーンチップを作製し、これを焼成した後、外部電極を印刷または転写して焼成することにより製造される。以下、製造方法について具体的に説明する。
下記の例において得られたコンデンサ試料の誘電体層を観察し、コアシェル粒子と判断された粒子について、該粒子の粒子径を測定し、平均粒子径を求める。また、シェル部における希土類濃度を測定し、希土類濃度勾配S、および希土類濃度の平均C、標準偏差σを求める。これらの詳細を以下に記載する。また、得られたコンデンサ試料について、絶縁比抵抗および高温負荷寿命の測定を、それぞれ下記に示す方法により行った。
コンデンサ試料を誘電体層に対して垂直な面で切断した。この切断面について、透過型電子顕微鏡(TEM)に付属のEDS装置を用いて、面分析を行い、希土類元素のマッピングデータを得た。また、同時にSi濃度等を測定し、粒界相や偏析相の輪郭を確定する。
コンデンサ試料を中心まで研磨し、その研磨面を焼成温度よりも100℃低い温度でサーマルエッチング処理した。処理後の研磨面を、電界放出型電子顕微鏡(FE-SEM)により観察し、2次電子像によるSEM写真を撮影した。このSEM写真をソフトウェアにより画像処理を行い、誘電体粒子の境界を判別し、各誘電体粒子の面積を算出した。そして、算出された誘電体粒子の面積を円相当径に換算して1.27倍した値を誘電体粒子径とした。この測定を2000個の誘電体粒子について行い、そのメジアン径を誘電体平均粒子径とした。
コンデンサ試料に対し、絶縁抵抗計(アドバンテスト社製R8340A)を用いて、20℃において50Vの直流電圧を、コンデンサ試料に10秒間印加し、印加後50秒放置した後の絶縁抵抗IRを測定した。測定した絶縁抵抗と、電極面積と層間厚みから絶縁比抵抗ρを計算した。本実施例では、1.0×1011Ω・m以上を良好とし、1.0×1012Ω・m以上を優良とし、1.0×1011Ω・m未満を不良とした。
コンデンサ試料に対し、175℃にて、25V/μmの電界下で直流電圧の印加状態に保持し、寿命時間を測定することにより、高温負荷寿命を評価した。本実施例においては、印加開始から絶縁抵抗が一桁落ちるまでの時間を寿命と定義した。また、本実施例では、上記の評価を20個のコンデンサ試料について行い、その平均値を高温負荷寿命とした。評価基準は50時間以上を良好とし、100時間以上を優良とした。
主成分原料に対し、X線回折装置(ブルカー社製X線回折装置 D8 ADVANCE)を用いてX線回折を測定し、その結果をリードベルド解析により単位結晶格子のa軸とc軸の長さを同定した。結晶性は単位格子のa軸とc軸の比(c/a)によって判定できる。
本実施形態では、c/aが1.010以上を高結晶性(H)とし、1.009以下を低結晶性(L)とし、両者の中間の結晶性(c/a:1.009超、1.010未満)を有するものを中結晶性(M)とした。
<主成分原料>
BaTiO3粉末(平均粒子径0.17μm、結晶性H)
BaTiO3粉末(平均粒子径0.17μm、結晶性M)
BaTiO3粉末(平均粒子径0.17μm、結晶性L)
BaTiO3粉末(平均粒子径0.12μm、結晶性L)
BaTiO3粉末(平均粒子径0.28μm、結晶性M)
なお、上記原料はいずれもBa/Ti=1.004とした。
<副成分原料>
Dy2O3(平均粒子径0.05μm、0.10μmの2種)
Gd2O3(平均粒子径0.05μm)
Tb2O3(平均粒子径0.05μm)
Y2O3(平均粒子径0.05μm)
Ho2O3(平均粒子径0.05μm)
Yb2O3(平均粒子径0.05μm)
チタン酸バリウムの原料紛体として、表1に記載の平均粒子径および結晶性を有するBaTiO3粉末(Ba/Ti=1.004)を準備した。
試料番号6では、平均粒子径が0.12μmのBaTiO3粉末を用い、試料番号7では、平均粒子径が0.28μmのBaTiO3粉末を使用した以外は、試料番号2と同様にして誘電体層用ペーストを調製した。
試料番号8では、Dy2O3粉末に代えてGd2O3粉末を用い、試料番号9ではTb2O3粉末を用い、試料番号10ではY2O3粉末を用い、試料番号11ではHo2O3粉末を用いた以外は、試料番号2と同様にして誘電体層用ペーストを調製した。
希土類化合物として、BaTiO3100モルに対し、試料番号12では1.0モルのDy2O3粉末(平均粒子径0.05μm)と0.3モルのHo2O3粉末とを用い、試料番号13では1.0モルのDy2O3粉末(平均粒子径0.05μm)と0.3モルのHo2O3粉末と0.2モルのYb2O3粉末とを用い、試料番号14では1.0モルのDy2O3粉末(平均粒子径0.05μm)と0.3モルのTb2O3粉末と0.2モルのYb2O3粉末とを用いた以外は、試料番号2と同様にして誘電体層用ペーストを調製した。
2…誘電体層
20…固溶粒子
21…コアシェル粒子
21a…主相(コア)
21b…拡散相(シェル)
3…内部電極層
4…外部電極
10…コンデンサ素子本体
Claims (4)
- 一般式ABO3(AはBa、SrおよびCaから選択される少なくとも1種、BはTi、ZrおよびHfから選択される少なくとも1種)で表される主成分と、希土類成分R(RはSc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Luから選ばれる少なくとも1種)とを含み、希土類元素濃度が0.2atom%未満のコア部と、希土類元素濃度が0.2atom%以上のシェル部を有するコアシェル構造の誘電体粒子を含む誘電体磁器組成物であり、前記コアシェル構造のシェル部における平均希土類濃度Cが0.4atom%以上であり、前記誘電体粒子の最表面から10nm内側における希土類濃度と、前記誘電体粒子のコアシェル境界面から10nmシェル側における希土類濃度とから算出される希土類濃度勾配Sが、-0.010atom%/nm≦S≦0.009atom%/nmである誘電体磁器組成物。
- 一般式ABO3(AはBa、SrおよびCaから選択される少なくとも1種、BはTi、ZrおよびHfから選択される少なくとも1種)で表される主成分と、希土類成分R(RはSc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Luから選ばれる少なくとも1種)とを含み、希土類元素濃度が0.2atom%未満のコア部と、希土類元素濃度が0.2atom%以上のシェル部を有するコアシェル構造の誘電体粒子を含む誘電体磁器組成物であり、前記コアシェル構造のシェル部における平均希土類濃度Cが0.4atom%以上であり、前記誘電体粒子の最表面から10nm内側と、前記誘電体粒子のコアシェル境界面から10nmシェル側との間の領域における希土類濃度の標準偏差をσとしたときに、σ/C≦0.15である誘電体磁器組成物。
- 前記誘電体粒子の平均粒子径が0.16~0.26μmである請求項1または2に記載の誘電体磁器組成物。
- 内部電極層と誘電体層とが交互に積層された積層体を有する積層セラミック電子部品であって、
前記誘電体層が、請求項1~3の何れかに記載の誘電体磁器組成物から構成される、積層セラミック電子部品。
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