JP5774824B2 - 圧電/電歪磁器組成物 - Google Patents
圧電/電歪磁器組成物 Download PDFInfo
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- JP5774824B2 JP5774824B2 JP2010142237A JP2010142237A JP5774824B2 JP 5774824 B2 JP5774824 B2 JP 5774824B2 JP 2010142237 A JP2010142237 A JP 2010142237A JP 2010142237 A JP2010142237 A JP 2010142237A JP 5774824 B2 JP5774824 B2 JP 5774824B2
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- electrostrictive
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
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- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
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- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 description 1
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- KYKNRZGSIGMXFH-ZVGUSBNCSA-M potassium bitartrate Chemical compound [K+].OC(=O)[C@H](O)[C@@H](O)C([O-])=O KYKNRZGSIGMXFH-ZVGUSBNCSA-M 0.000 description 1
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- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- LLVQEXSQFBTIRD-UHFFFAOYSA-M sodium;2,3,4-trihydroxy-4-oxobutanoate;hydrate Chemical compound O.[Na+].OC(=O)C(O)C(O)C([O-])=O LLVQEXSQFBTIRD-UHFFFAOYSA-M 0.000 description 1
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- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
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- 239000010937 tungsten Substances 0.000 description 1
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- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- 229910003454 ytterbium oxide Inorganic materials 0.000 description 1
- 229940075624 ytterbium oxide Drugs 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—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
- C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/80—Constructional details
- H10N30/85—Piezoelectric or electrostrictive active materials
- H10N30/853—Ceramic compositions
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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Description
第1実施形態は、圧電/電歪磁器組成物に関する。
第1実施形態の圧電/電歪磁器組成物は、第2実施形態〜第5実施形態に示すようにアクチュエータに好適に用いられる。ただし、第1実施形態の圧電/電歪磁器組成物の用途は、アクチュエータに限られない。例えば、第1実施形態の圧電/電歪磁器組成物は、センサ等の圧電/電歪素子にも用いられる。
第1実施形態の圧電/電歪磁器組成物は、Aサイト元素としてリチウム(Li),ナトリウム(Na)及びカリウム(K)を含み、Bサイト元素としてニオブ(Nb)及びアンチモン(Sb)を含み、Bサイト元素の総原子数に対するAサイト元素の総原子数の比が1より大きく、Bサイト元素の総原子数に占めるSbの原子数が1mol%以上10mol%以下であるペロブスカイト型酸化物に、バリウム(Ba),ストロンチウム(Sr),カルシウム(Ca),ランタン(La),セリウム(Ce),ネオジム(Nd),サマリウム(Sm),ジスプロシウム(Dy),ホルミウム(Ho)及びイッテルビウム(Yb)からなる群より選択される一種類以上の元素(以下では、「選択元素」という)の化合物と、マンガン(Mn)の化合物と、を含有させた圧電/電歪磁器組成物である。ペロブスカイト型酸化物に、Aサイト元素として銀(Ag)等の1価元素をさらに含有させてもよいし、Bサイト元素としてタンタル(Ta),バナジウム(V)等の5価元素をさらに含有させてもよい。
圧電/電歪磁器組成物の第1の成分は、組成が一般式{Liy(Na1-xKx)1-y}a(Nb1-z-wTazSbw)O3で表されるペロブスカイト型酸化物であることが望ましい。a,x,y,z及びwは、それぞれ、1<a≦1.05,0.30≦x≦0.70,0.02≦y≦0.10,0≦z≦0.5及び0.01≦w≦0.1を満たすことが望ましい。
圧電/電歪磁器組成物の第2の成分は、Ba,Sr,Ca,La,Ce,Nd,Sm,Dy,Ho及びYbからなる群より選択される一種類以上の選択元素の化合物である。
圧電/電歪磁器組成物の第3の成分は、Mnの化合物である。
ニオブ酸アルカリ系のペロブスカイト型酸化物及びその変性物は、一般的に言って、高温から低温に向かって立方晶、正方晶、斜方晶の順に逐次相転移するが、第1実施形態の圧電/電歪磁器組成物では、相転移温度TOTが室温の近傍となるように組成を選択することが望ましい。相転移温度TOTが室温の近傍にあれば、高電界印加時の電界誘起歪が大きくなるからである。
第1実施形態の圧電/電歪磁器組成物では、結晶相が正方晶であって、その格子歪がある程度小さくなるように組成を選択することが望ましい。
第1実施形態の圧電/電歪磁器組成物の原料粉末の製造にあたっては、ペロブスカイト型酸化物の構成元素(Li,Na,K,Nb,Ta,Sb等)の素原料の粉末に分散媒が加えられ、分散媒が加えられた素原料の粉末が乳鉢混合、ボールミル等のポットミル、ビーズミル、ハンマーミル、ジェットミル等で混合される。ペロブスカイト型酸化物の構成元素の素原料としては、酸化物又は仮焼過程において酸化物となる炭酸塩、酒石酸塩等の化合物が用いられる。分散媒としては、エタノール、トルエン、アセトン等の有機溶剤が用いられる。
[1]20〜2000℃/時間の昇温速度で室温から第1の仮焼温度の600〜1300℃まで昇温し第1の仮焼温度を保持する第1の段階;
の終了後すぐに20〜2000℃/時間の降温速度で室温まで降温する1段階の仮焼スケジュールにより混合原料が仮焼される。
[1]室温から第1の仮焼温度の600〜800℃まで昇温し第1の仮焼温度を保持する第1の段階;及び
[2]第1の仮焼温度から第2の仮焼温度の800〜1300℃まで昇温し第2の仮焼温度を保持する第2の段階;
の終了後に室温まで降温する2段階の仮焼スケジュールにより混合原料が仮焼される。
[1]室温から第1の仮焼温度の900〜1300℃まで500℃/時間以上の昇温速度で昇温し第1の仮焼温度を保持する第1の段階;及び
[2]第1の仮焼温度から第2の仮焼温度の600〜900℃まで200℃/時間以上の降温速度で降温し第2の仮焼温度を保持する第2の段階;
の終了後に室温まで降温する2段階の仮焼スケジュールにより混合原料が仮焼される。
第1実施形態の圧電/電歪磁器組成物の焼結体の製造にあたっては、まず、プレス成形、テープ成形、鋳込み成形等により原料粉末が成形される。
[1]20〜2000℃/時間の昇温速度で室温から第1の焼成温度の600〜1300℃まで昇温し第1の焼成温度を保持する第1の段階;
の終了後すぐに20〜2000℃/時間の降温速度で室温まで降温する1段階の焼成スケジュールにより原料粉末の成形体が仮焼される。
[1]室温から第1の焼成温度の600〜800℃まで昇温し第1の焼成温度を保持する第1の段階;及び
[2]第1の焼成温度から第2の焼成温度の800〜1300℃まで昇温し第2の焼成温度を保持する第2の段階;
の終了後に室温まで降温する2段階の焼成スケジュールにより原料粉末の成形体が仮焼される。
[1]室温から第1の焼成温度の900〜1300℃まで500℃/時間以上の昇温速度で昇温し第1の焼成温度を保持する第1の段階;及び
[2]第1の焼成温度から第2の焼成温度の600〜900℃まで200℃/時間以上の降温速度で降温し第2の焼成温度を保持する第2の段階;
の終了後に室温まで降温する2段階の焼成スケジュールにより原料粉末の成形体が仮焼される。
第2実施形態は、第1実施形態の圧電/電歪磁器組成物を用いた単層型の圧電/電歪アクチュエータ1に関する。
図1は、第2実施形態の圧電/電歪アクチュエータ1の模式図である。図1は、圧電/電歪アクチュエータ1の断面図である。
圧電/電歪体膜122は、第1実施形態の圧電/電歪磁器組成物の焼結体である。
電極膜121,123の材質は、白金、パラジウム、ロジウム、金若しくは銀等の金属又はこれらの合金である。中でも、焼成時の耐熱性が高い点で白金又は白金を主成分とする合金が好ましい。また、焼成温度によっては、銀−パラジウム等の合金も好適に用いられる。
基体11の材質は、セラミックスであるが、その種類に制限はない。もっとも、耐熱性、化学的安定性及び絶縁性の観点から、安定された酸化ジルコニウム、酸化アルミニウム、酸化マグネシウム、ムライト、窒化アルミニウム、窒化ケイ素及びガラスからなる群より選択される少なくとも1種類を含むセラミックスであることが望ましい。中でも、機械的強度及び靭性の観点から安定化された酸化ジルコニウムがさらに望ましい。「安定化された酸化ジルコニウム」とは、安定化剤の添加によって結晶の相転移を抑制した酸化ジルコニウムをいい、安定化酸化ジルコニウムの他、部分安定化酸化ジルコニムを包含する。
圧電/電歪アクチュエータ1の製造にあたっては、基体11の上に電極膜121が形成される。電極膜121は、イオンビーム、スパッタリング、真空蒸着、PVD(Physical Vapor Deposition)、イオンプレーティング、CVD(Chemical Vapor Deposition)、メッキ、エアロゾルデポジション、スクリーン印刷、スプレー、ディッピング等の方法で形成される。中でも、基体11及び圧電/電歪体膜122との接合性の観点から、スパッタリング法又はスクリーン印刷法が望ましい。形成された電極膜121は、熱処理により、基体11及び圧電/電歪体膜122と固着される。熱処理の温度は、電極膜121の材質や形成方法に応じて異なるが、概ね500〜1400℃である。
第3実施形態は、第1実施形態の圧電/電歪磁器組成物を用いた多層型の圧電/電歪アクチュエータ2に関する。
第4実施形態は、第1実施形態の圧電/電歪磁器組成物を用いた多層型の圧電/電歪アクチュエータ3に関する。
第5実施形態は、第1実施形態の圧電/電歪磁器組成物を用いた圧電/電歪アクチュエータ4に関する。
評価用の圧電/電歪素子の製造にあたっては、炭酸リチウム(Li2CO3)、酒石酸水素ナトリウム一水和物(C4H5O6Na・H2O)、酒石酸水素カリウム(C4H5O6K)、酸化ニオブ(Nb2O5)、酸化タンタル(Ta2O5)及び酸化アンチモン(Sb2O3)の素原料の粉末を、焼成後の酸化物において表1〜表5に示す組成となるように秤量した。表1〜表5の「x」「y」「z」「w」及び「a」の欄には、第1の成分のペロブスカイト型酸化物の組成を一般式{Liy(Na1-xKx)1-y}a(Nb1-z-wTazSbw)O3で表したときのx,y,z,w及びaの値が示されている。
(1)1000℃/時間の昇温速度で1000〜1050℃まで昇温して1分間保持する第1の段階、
(2)400〜2000℃/時間の降温速度で940〜980℃まで降温して3〜6時間保持する第2の段階、
(3)200℃/時間の降温速度で室温まで冷却する第3の段階、
を順次実行する焼成プロファイルを用いて焼成を行った。試料番号E1の焼成雰囲気は、酸素雰囲気である。
(1)200℃/時間の昇温速度で860〜900℃まで昇温して0.5〜3時間保持する第1の段階、
(2)1000℃/時間の昇温速度で1000〜1050℃まで昇温して1分間保持する第2の段階、
(3)400〜2000℃/時間の降温速度で940〜980℃まで降温して3〜6時間保持する第3の段階、
(4)200℃/時間の降温速度で室温まで冷却する第4の段階、
を順次実行する焼成プロファイルを用いて焼成を行った。試料番号E2の焼成雰囲気は、酸素雰囲気である。
評価用の圧電/電歪素子を用いて、圧電定数d31(pm/V)及び歪率S4000(ppm)を測定した。その測定結果を表1〜表5に示す。表1,2,4,5には、エージング処理の後の圧電定数d31及び歪率S4000が示されている。表3には、分極処理の後であってエージング処理の前及びエージング処理の後の圧電定数d31及び歪率S4000が示されている。
122,222,224,402 圧電/電歪体膜
121,123,221,223,225 電極膜
404 内部電極膜
Claims (4)
- Aサイト元素としてLi,Na及びKを含み、Bサイト元素としてNb及びSbを含み、Bサイト元素の総原子数に対するAサイト元素の総原子数の比が1より大きく、Bサイト元素の総原子数に占めるSbの原子数が1mol%以上10mol%以下であるペロブスカイト型酸化物に、Ba,Sr,Ca,La,Ce,Nd,Sm,Dy,Ho及びYbからなる群より選択される一種類以上の選択元素の化合物と、Mnの化合物と、を含有させ、前記ペロブスカイト型酸化物100モル部に対する前記選択元素の化合物の含有量が選択元素原子換算で0.01モル部以上0.2モル部以下である圧電/電歪磁器組成物。
- 前記ペロブスカイト型酸化物がBサイト元素としてさらにTaを含む請求項1の圧電/電歪磁器組成物。
- 一般式{Liy(Na1−xKx)1−y}a(Nb1−z−wTazSbw)O3で表され、a,x,y,z及びwが、それぞれ、1<a≦1.05,0.30≦x≦0.70,0.02≦y≦0.10,0≦z≦0.5及び0.01≦w≦0.1を満たす組成を有するペロブスカイト型酸化物に、Ba,Sr,Ca,La,Ce,Nd,Sm,Dy,Ho及びYbからなる群より選択される一種類以上の選択元素の化合物と、Mnの化合物と、を含有させ、前記ペロブスカイト型酸化物100モル部に対する前記選択元素の化合物の含有量が選択元素原子換算で0.01モル部以上0.2モル部以下である圧電/電歪磁器組成物。
- 前記ペロブスカイト型酸化物100モル部に対する前記Mnの化合物の含有量がMn原子換算で3モル部以下である請求項1ないし請求項3のいずれかの圧電/電歪磁器組成物。
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