JP6039762B2 - 圧電磁器組成物 - Google Patents
圧電磁器組成物 Download PDFInfo
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- JP6039762B2 JP6039762B2 JP2015142187A JP2015142187A JP6039762B2 JP 6039762 B2 JP6039762 B2 JP 6039762B2 JP 2015142187 A JP2015142187 A JP 2015142187A JP 2015142187 A JP2015142187 A JP 2015142187A JP 6039762 B2 JP6039762 B2 JP 6039762B2
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- piezoelectric
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- piezoelectric ceramic
- perovskite
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- 239000000203 mixture Substances 0.000 title claims description 105
- 239000000919 ceramic Substances 0.000 title claims description 60
- 239000002245 particle Substances 0.000 claims description 21
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 15
- 239000004020 conductor Substances 0.000 description 18
- 230000005684 electric field Effects 0.000 description 11
- 238000000034 method Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 239000003513 alkali Substances 0.000 description 8
- 230000007423 decrease Effects 0.000 description 8
- 229910001316 Ag alloy Inorganic materials 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 238000010304 firing Methods 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 3
- 238000009766 low-temperature sintering Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 229910052763 palladium Inorganic materials 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 238000007650 screen-printing Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910001252 Pd alloy Inorganic materials 0.000 description 2
- 229910001260 Pt alloy Inorganic materials 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 238000007606 doctor blade method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000027734 detection of oxygen Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009837 dry grinding Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Description
(Pba・Rex){Zrb・Tic・(Ni1/3Nb2/3)d・(Zn1/3Nb2/3)e}O3 ・・・(1)
式中、Reは、La及び/又はNdであり、a〜e、xは次の要件を満たす。
0.95≦a≦1.05
0≦x≦0.05
0.35≦b≦0.45
0.35≦c≦0.45
0<d≦0.10
0.07≦e≦0.20
b+c+d+e=1
前記圧電磁器層は、前記ペロブスカイト組成物の焼結体からなる結晶粒子の粒界ないしは粒界三重点に、SiおよびKを含有する結晶ないしは非結晶質が存在していることが好ましい。
(LilNamK1−l−m)n(Nb1−oTao)O3 ・・・(2)
式中、l〜oは、次の要件を満たす。
0.04<l≦0.1
0≦m≦1
0.95≦n≦1.05
0≦o≦1
(Pba・Rex){Zrb・Tic・(Ni1/3Nb2/3)d・(Zn1/3Nb2/3)e}O3 ・・・(1)
式中、Reは、La及び/又はNdであり、a〜e、xは次の要件を満たす。
0.95≦a≦1.05
0≦x≦0.05
0.35≦b≦0.45
0.35≦c≦0.45
0<d≦0.10
0.07≦e≦0.20
b+c+d+e=1
また、本発明において、上記圧電磁器組成物は、更にCo成分を含有させてもよい。Co成分を含有させることで、圧電特性、誘電特性を所望の特性に微調整することができる。
Co成分の含有量は、ペロブスカイト組成物100質量部に対し、酸化物換算で0〜1質量%が好ましい。
次に、このペロブスカイト組成物と、表1に示す割合で秤量したAg2Oをポットミル内にジルコニアビーズ、イオン交換水と共に入れ、15時間湿式解砕し、得られた懸濁液をバットに移し、乾燥器内に入れ、150℃で乾燥させ、圧電磁器組成物を得た。
次に、各圧電磁器組成物にポリビニルブチラールを少量混合し、加圧プレス機を用い、圧力1.5MPaで圧縮成型し、直径8mm、厚さ0.5mmの円板形の試料を得た。
次に、この試料を電気炉内に入れ、大気雰囲気下において900℃〜1050℃で2時間焼成し、その後この試料を電気炉から取り出し、試料の両面にフリットレスAgペーストを印刷し、大気雰囲気下において700℃で焼き付け、これを外部電極とした。
この外部電極が取り付けられた円板形試料について、40℃〜400℃の間で誘電率εの温度依存性を測定し、キュリー温度Tcを求めた。また、TFアナライザーを用い、25℃、1Hz,3kV/mmの条件で各試料のヒステリシスを測定し、抗電界を算出した。次に、この外部電極付きの試料に、150℃の下で、1.5kV/mmの電圧を15分間印加し、試料を分極させた。次に、この分極させた試料の圧電定数Krを測定したところ、表1に示す通りであった。圧電定数Krの測定は、電子情報技術産業協会規格(JEITA EM−4501)にのっとり、インピーダンス測定を行い、算出した。結果を表2に示す。
次に、未焼成内部導体層が形成された各グリーンシートを11枚積層し、同じシートでペーストが印刷されていないシートを所定の厚みに積層したカバーシートを上下に挟み共に圧着して未焼成積層体を製造した。
次に、この未焼成積層体を電気炉内に入れ、大気雰囲気下において900℃で2時間焼成して積層体を製造した。得られた積層体について、TEM画像を撮影し、ペロブスカイト組成物の焼結体中の空隙にAgが偏析しているどうか確認した。また、EDS(エネルギー分散X線分光法)により、酸素の検出の有無を確認した。
また、ReにNdを用いた試料1Bでも同様な結果が得られた。試料1A、1Bが本発明の圧電磁器組成物にあたる。
Claims (2)
- 下式(1)で表わされるチタン酸ジルコン酸塩系ペロブスカイト組成物と、前記チタン酸ジルコン酸塩系ペロブスカイト組成物の焼結体中の空隙に偏析しているAgとを含有し、
前記Agは、酸化物換算で、前記チタン酸ジルコン酸塩系ペロブスカイト組成物100質量部に対し0.05〜0.3質量部含有することを特徴とする圧電磁器組成物。
(Pba・Rex){Zrb・Tic・(Ni1/3Nb2/3)d・(Zn1/3Nb2/3)e}O3 ・・・(1)
式中、Reは、La及び/又はNdであり、a〜e、xは次の要件を満たす。
0.95≦a≦1.05
0≦x≦0.05
0.35≦b≦0.45
0.35≦c≦0.45
0<d≦0.10
0.07≦e≦0.20
b+c+d+e=1 - 前記Agの最大粒子径が3μm以下である請求項1に記載の圧電磁器組成物。
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