JP2011116630A - 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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- JP2011116630A JP2011116630A JP2010222708A JP2010222708A JP2011116630A JP 2011116630 A JP2011116630 A JP 2011116630A JP 2010222708 A JP2010222708 A JP 2010222708A JP 2010222708 A JP2010222708 A JP 2010222708A JP 2011116630 A JP2011116630 A JP 2011116630A
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- Prior art keywords
- barium titanate
- hexagonal
- mol
- ceramic composition
- dielectric
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- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 120
- 239000000203 mixture Substances 0.000 title claims abstract description 48
- 239000000919 ceramic Substances 0.000 title claims abstract description 33
- 239000000843 powder Substances 0.000 title claims description 72
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 13
- 239000011521 glass Substances 0.000 claims abstract description 12
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims description 32
- 239000013078 crystal Substances 0.000 claims description 25
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 12
- 238000009826 distribution Methods 0.000 claims description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 8
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 6
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 6
- 229910052689 Holmium Inorganic materials 0.000 claims description 6
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 6
- 239000003989 dielectric material Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- 229910052771 Terbium Inorganic materials 0.000 claims description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims description 5
- 229910052779 Neodymium Inorganic materials 0.000 claims description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 4
- 229910052772 Samarium Inorganic materials 0.000 claims description 4
- 238000009413 insulation Methods 0.000 abstract description 11
- 239000010410 layer Substances 0.000 description 68
- 238000010304 firing Methods 0.000 description 20
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- 239000003985 ceramic capacitor Substances 0.000 description 19
- 238000000034 method Methods 0.000 description 19
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- 239000010936 titanium Substances 0.000 description 15
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 11
- 238000010438 heat treatment Methods 0.000 description 11
- 239000001301 oxygen Substances 0.000 description 11
- 229910052760 oxygen Inorganic materials 0.000 description 11
- 238000002441 X-ray diffraction Methods 0.000 description 10
- 238000000137 annealing Methods 0.000 description 10
- 239000004020 conductor Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 10
- 238000006467 substitution reaction Methods 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000001816 cooling Methods 0.000 description 9
- 230000036961 partial effect Effects 0.000 description 9
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 8
- 238000010298 pulverizing process Methods 0.000 description 8
- 230000009466 transformation Effects 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 description 5
- 229910010413 TiO 2 Inorganic materials 0.000 description 5
- 229910052788 barium Inorganic materials 0.000 description 5
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 5
- 239000002270 dispersing agent Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 238000011282 treatment Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 238000004438 BET method Methods 0.000 description 4
- 229920002799 BoPET Polymers 0.000 description 4
- 229910000990 Ni alloy Inorganic materials 0.000 description 4
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- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000010953 base metal Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000002003 electrode paste Substances 0.000 description 4
- 229910052748 manganese Inorganic materials 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 150000002902 organometallic compounds Chemical class 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000001856 Ethyl cellulose Substances 0.000 description 3
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 229920001249 ethyl cellulose Polymers 0.000 description 3
- 235000019325 ethyl cellulose Nutrition 0.000 description 3
- 150000004679 hydroxides Chemical class 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
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- 230000008569 process Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000004925 Acrylic resin Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 230000000670 limiting effect Effects 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 150000003891 oxalate salts Chemical class 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000010405 reoxidation reaction Methods 0.000 description 2
- 238000005488 sandblasting Methods 0.000 description 2
- 239000003232 water-soluble binding agent Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000012447 hatching Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- -1 or various oxides Chemical class 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000015096 spirit Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- 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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- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
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Abstract
【解決手段】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、M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、A、B、αおよびβが、1.000<A/B≦1.040、0≦α<0.003、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等のアルカリ土類酸化物、Mn3O4および/またはCr2O3と、CuOと、Al2O3と、希土類元素酸化物と、SiO2を含むガラス成分とを特定量含んでなる誘電体磁器組成物。
【選択図】なし
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、1.000<(A/B)≦1.040、0≦α<0.003、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、1.000<(A/B)≦1.040、0≦α<0.003、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2〜5モル、かつ該アルカリ土類酸化物の合計量を15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0.5〜2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1〜5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、
少なくとも、チタン酸バリウムの原料および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および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1MHz,入力信号レベル(測定電圧)1Vrms/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。
温度25℃において、周波数1MHz、電圧(実効値)1Vの交流でQメータにより測定した。
<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、Mnの原料として、Mn3O4(比表面積:20m2/g)、元素Mの原料として、La(OH)3(比表面積:10m2/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。
元素Mの原料としてLa(OH)3の代わりに表4に示す元素の酸化物、炭酸塩、水酸化物を用いた以外は、実施例2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。
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7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1.0モル、MgOを1.0モル、CaOを1.0モル、BaOを1.0モル、Mn3O4を0.5モル、CuOを0.5モル、Al2O3を0.5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8に示す値とした以外は、実験例3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8に示す。
副成分の組成を、主成分100モルに対して、希土類を5.0モル、MgOを5.0モル、CaOを5.0モル、BaOを5.0モル、Mn3O4を2.0モル、CuOを2.0モル、Al2O3を2.0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9に示す値とした以外は、実験例3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9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 (5)
- 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、1.000<(A/B)≦1.040、0≦α<0.003、0.03≦β≦0.2の関係を満足することを特徴とする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A、B、αおよびβが、1.000<(A/B)≦1.040、0≦α<0.003、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2〜5モル、かつ該アルカリ土類酸化物の合計量を15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0.5〜2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1〜5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。
- 請求項1または2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、
少なくとも、チタン酸バリウムの原料および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および前記Mnの原料を熱処理する工程と、を有する六方晶系チタン酸バリウム粉末の製造方法。
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WO2013074577A1 (en) * | 2011-11-16 | 2013-05-23 | Stuart Martin A | High energy density storage device |
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