JP5883217B2 - 六方晶系チタン酸バリウム粉末、その製造方法、誘電体磁器組成物および電子部品 - Google Patents
六方晶系チタン酸バリウム粉末、その製造方法、誘電体磁器組成物および電子部品 Download PDFInfo
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- JP5883217B2 JP5883217B2 JP2010222705A JP2010222705A JP5883217B2 JP 5883217 B2 JP5883217 B2 JP 5883217B2 JP 2010222705 A JP2010222705 A JP 2010222705A JP 2010222705 A JP2010222705 A JP 2010222705A JP 5883217 B2 JP5883217 B2 JP 5883217B2
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- barium titanate
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- hexagonal barium
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- C01G45/125—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3
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Description
一般式(Ba1−αMα)A(Ti1−βMnβ)BO3で表され、結晶構造が六方晶であるチタン酸バリウムを主成分として含むチタン酸バリウム粉末であって、
前記Mの12配位時の有効イオン半径が、12配位時のBa2+の有効イオン半径に対して、±20%以内であり、
前記A、B、αおよびβが、0.900≦(A/B)≦1.040、0.003≦α≦0.05、0.03≦β≦0.2の関係を満足することを特徴とする。
一般式(Ba1−αMα)A(Ti1−βMnβ)BO3で表され、結晶構造が六方晶であって、前記Mの12配位時の有効イオン半径が、12配位時のBa2+の有効イオン半径に対して±20%以内であり、前記A、B、αおよびβが、0.900≦(A/B)≦1.040、0.003≦α≦0.05、0.03≦β≦0.2の関係を満足する六方晶系チタン酸バリウムを主成分とし、該主成分100モルに対し、副成分として、
MgO、CaOおよびBaOからなる群から選ばれる少なくとも1つのアルカリ土類酸化物を、各酸化物換算で1〜3モル、かつ該アルカリ土類酸化物の合計量を9モル以下、
Mn3O4および/またはCr2O3と、CuOと、Al2O3とを、それぞれ、各金属元素換算で0.1〜1モル、
Y、La、Ce、Pr、Nd、Sm、Gd、Tb、Dy、HoおよびYbからなる群から選ばれる少なくとも1つの希土類元素の酸化物を、希土類元素換算の合計で0.1〜1モル、および
SiO2を含むガラス成分を、SiO2換算で0.1〜1モル含む。
上記のいずれかに記載の六方晶系チタン酸バリウム粉末を製造する方法であって、
チタン酸バリウムの原料、元素Mの原料およびMnの原料を準備する工程と、
前記チタン酸バリウムの原料、前記Mの原料および前記Mnの原料を熱処理する工程と、を有する。
図1に示すように、電子部品の代表例であ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。このコンデンサ素子本体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。コンデンサ素子本体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。
本実施形態に係る六方晶系チタン酸バリウム粉末は、六方晶構造を有するチタン酸バリウム(六方晶チタン酸バリウム)粉末を主成分としている。具体的には、本実施形態に係る六方晶系チタン酸バリウム粉末100質量%に対して、50質量%以上、好ましくは90質量%以上、より好ましくは95質量%以上含有されている。
次に、本実施形態に係る六方晶系チタン酸バリウム粉末を製造する方法について説明する。
副成分としては、
MgO、CaOおよびBaOからなる群から選ばれる少なくとも1つのアルカリ土類酸化物、
金属酸化物として、Mn3O4および/またはCr2O3と、CuOと、Al2O3と、
Y、La、Ce、Pr、Nd、Sm、Gd、Tb、Dy、HoおよびYbからなる群から選ばれる少なくとも1つの希土類元素の酸化物、および
SiO2を含むガラス成分が用いられる。
図1に示した、電子部品の代表例である積層セラミックコンデンサ1における誘電体層2の厚さは、特に限定されないが、一層あたり5μm以下であることが好ましく、より好ましくは3μm以下である。厚さの下限は、特に限定されないが、たとえば1μm程度である。本実施形態に係る誘電体磁器組成物によれば、層厚1μm以上で比誘電率が50以上を示す。誘電体層2の積層数は、特に限定されないが、200以上であることが好ましい。
コンデンサ試料に対し、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1kHz,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。
<六方晶系チタン酸バリウム粉末の調製>
まず、チタン酸バリウムの原料として、BaCO3(比表面積:25m2/g)およびTiO2(比表面積:50m2/g)を準備した。また、元素Mの原料として、La(OH)3(比表面積:10m2/g)、Mnの原料として、Mn3O4(比表面積:20m2/g)を準備した。
X線回折は、X線源としてCu−Kα線を用い、その測定条件は、電圧45kV、電流40mAで、2θ=20°〜90°の範囲を、走査速度4.0deg/min、積算時間30secであった。
Aサイト置換量αとBサイト置換量βとの比(α/β)を表4に示す値とした以外は、実験例1と同様にして、粉末を作製し、比表面積およびX線回折測定を行った。結果を表4〜6に示す。
元素Mの原料としてLa(OH)3の代わりに表7に示す元素の酸化物、炭酸塩、水酸化物を用いた以外は、実験例1と同様にして、粉末を作製し、比表面積およびX線回折測定を行った。結果を表7〜9に示す。
六方晶系チタン酸バリウム粉末および平均粒径0.1〜1.5μmの副成分原料粉末(MgO、CaO、BaO、Mn3O4、CuO、Al2O3、Y2O3、Dy2O3、Gd2O3、Ho2O3、Yb2O3、Tb2O3およびSiO2−ZnO−B2O3ガラス)を、焼成後の組成が下記の表10に示す組成となるように秤量した後、この原料に媒体として水を加えて5時間ボールミルで混合した。その後に、この混合物を乾燥させ、混合粉末を得た。
副成分の組成を、主成分100モルに対して、希土類を0.1モル、MgOを1.0モル、CaOを1.0モル、BaOを1.0モル、Mn3O4を0.1モル、CuOを0.1モル、Al2O3を0.1モル、ガラス成分を0.1モルとし、一般式における元素Mの種類、α、βおよびA/Bを表11に示す値とした以外は、実験例4と同様にして、コンデンサを作製し、上記の特性評価を行った。結果を表11に示す。
副成分の組成を、主成分100モルに対して、希土類を1.0モル、MgOを3.0モル、CaOを3.0モル、BaOを3.0モル、Mn3O4を1.0モル、CuOを1.0モル、Al2O3を1.0モル、ガラス成分を1.0モルとし、一般式における元素Mの種類、α、βおよびA/Bを表12に示す値とした以外は、実験例4と同様にして、コンデンサを作製し、上記の特性評価を行った。結果を表12に示す。
2…誘電体層
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(Ba1−αMα)A(Ti1−βMnβ)BO3で表され、結晶構造が六方晶であるチタン酸バリウムを含むチタン酸バリウム粉末であって、
前記Mの12配位時の有効イオン半径が、12配位時のBa2+の有効イオン半径に対して、±20%以内であり、
前記MがDy、Gd、Ho、Y、Er、Yb、La、CeおよびBiから選ばれる少なくとも1つであり、
前記A、B、αおよびβが、0.900≦(A/B)≦1.040、0.003≦α≦0.05、0.03≦β≦0.2の関係を満足し、
比表面積が2m 2 /g以上であり、
X線回折測定により得られるX線回折チャートにおいて、チタン酸バリウムに由来するピーク以外のピークが存在せず、六方晶チタン酸バリウム、正方晶チタン酸バリウムおよび立方晶チタン酸バリウムの最大ピーク強度の合計を100%として、六方晶チタン酸バリウムの最大ピーク強度が占める比率が50%以上であることを特徴とする電子部品の誘電体層用の六方晶系チタン酸バリウム粉末。 - 前記αと前記βとの比(α/β)が、(α/β)≦0.40の関係を満足する請求項1に記載の六方晶系チタン酸バリウム粉末。
- 一般式(Ba1−αMα)A(Ti1−βMnβ)BO3で表され、結晶構造が六方晶であって、前記Mの12配位時の有効イオン半径が、12配位時のBa2+の有効イオン半径に対して±20%以内であり、前記MがDy、Gd、Ho、Y、Er、Yb、La、CeおよびBiから選ばれる少なくとも1つであり、前記A、B、αおよびβが、0.900≦(A/B)≦1.040、0.003≦α≦0.05、0.03≦β≦0.2の関係を満足し、比表面積が2m 2 /g以上であり、X線回折測定により得られるX線回折チャートにおいて、チタン酸バリウムに由来するピーク以外のピークが存在せず、六方晶チタン酸バリウム、正方晶チタン酸バリウムおよび立方晶チタン酸バリウムの最大ピーク強度の合計を100%として、六方晶チタン酸バリウムの最大ピーク強度が占める比率が50%以上である六方晶系チタン酸バリウムを主成分とし、該主成分100モルに対し、副成分として、
MgO、CaOおよびBaOからなる群から選ばれる少なくとも1つのアルカリ土類酸化物を、各酸化物換算で1〜3モル、かつ該アルカリ土類酸化物の合計量を9モル以下、
Mn3O4およびCr2O3の何れか一つ以上と、CuOと、Al2O3とを、それぞれ、各金属元素換算で0.1〜1モル、
Y、La、Ce、Pr、Nd、Sm、Gd、Tb、Dy、HoおよびYbからなる群から選ばれる少なくとも1つの希土類元素の酸化物を、希土類元素換算の合計で0.1〜1モル、および
SiO2を含むガラス成分を、SiO2換算で0.1〜1モル含む誘電体磁器組成物。 - 請求項3に記載の誘電体磁器組成物で構成してある誘電体層と、内部電極層を有する電子部品。
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JP3941871B2 (ja) * | 2003-08-01 | 2007-07-04 | 独立行政法人 宇宙航空研究開発機構 | 無容器凝固法によるバリウムチタン酸化物セラミックス材料の製造方法 |
JP4013226B2 (ja) * | 2004-01-29 | 2007-11-28 | 独立行政法人 宇宙航空研究開発機構 | 無容器凝固法によるバリウムチタン酸化物単結晶材料片の製造方法 |
WO2006018928A1 (ja) * | 2004-08-19 | 2006-02-23 | Murata Manufacturing Co., Ltd | 誘電体セラミック、及び積層セラミックコンデンサ |
JP2008162828A (ja) * | 2006-12-27 | 2008-07-17 | Japan Science & Technology Agency | 電子・光学用チタン酸バリウム−カルシウム単結晶体材料及び多結晶体材料とその製造方法 |
TW200835821A (en) * | 2007-02-16 | 2008-09-01 | Univ Nat Taiwan | Barium titanate single crystal and the preparation method thereof |
JP5094572B2 (ja) * | 2008-03-26 | 2012-12-12 | 京セラ株式会社 | 積層セラミックコンデンサ |
WO2009136443A1 (ja) * | 2008-05-09 | 2009-11-12 | 独立行政法人宇宙航空研究開発機構 | 誘電体磁器組成物 |
JP5779860B2 (ja) * | 2009-11-06 | 2015-09-16 | Tdk株式会社 | 六方晶系チタン酸バリウム粉末、その製造方法、誘電体磁器組成物および電子部品 |
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DE102010050553B4 (de) | 2017-11-23 |
CN102060521A (zh) | 2011-05-18 |
US20110110018A1 (en) | 2011-05-12 |
JP2011116629A (ja) | 2011-06-16 |
CN102060521B (zh) | 2014-02-05 |
DE102010050553A1 (de) | 2011-05-12 |
KR101313054B1 (ko) | 2013-09-30 |
US8373968B2 (en) | 2013-02-12 |
KR20110050390A (ko) | 2011-05-13 |
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