JP7102243B2 - 配向性圧電体膜、およびその製造方法、並びに、液体吐出ヘッド - Google Patents
配向性圧電体膜、およびその製造方法、並びに、液体吐出ヘッド Download PDFInfo
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- JP7102243B2 JP7102243B2 JP2018116838A JP2018116838A JP7102243B2 JP 7102243 B2 JP7102243 B2 JP 7102243B2 JP 2018116838 A JP2018116838 A JP 2018116838A JP 2018116838 A JP2018116838 A JP 2018116838A JP 7102243 B2 JP7102243 B2 JP 7102243B2
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- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- QNZLAXONNWOLJY-UHFFFAOYSA-N hexyl 3-oxobutanoate Chemical compound CCCCCCOC(=O)CC(C)=O QNZLAXONNWOLJY-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- ZEIWWVGGEOHESL-UHFFFAOYSA-N methanol;titanium Chemical compound [Ti].OC.OC.OC.OC ZEIWWVGGEOHESL-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- XPGAWFIWCWKDDL-UHFFFAOYSA-N propan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCC[O-].CCC[O-].CCC[O-].CCC[O-] XPGAWFIWCWKDDL-UHFFFAOYSA-N 0.000 description 1
- ZGSOBQAJAUGRBK-UHFFFAOYSA-N propan-2-olate;zirconium(4+) Chemical compound [Zr+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] ZGSOBQAJAUGRBK-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- JKUYRAMKJLMYLO-UHFFFAOYSA-N tert-butyl 3-oxobutanoate Chemical compound CC(=O)CC(=O)OC(C)(C)C JKUYRAMKJLMYLO-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- PMTRSEDNJGMXLN-UHFFFAOYSA-N titanium zirconium Chemical compound [Ti].[Zr] PMTRSEDNJGMXLN-UHFFFAOYSA-N 0.000 description 1
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 1
- LGQXXHMEBUOXRP-UHFFFAOYSA-N tributyl borate Chemical compound CCCCOB(OCCCC)OCCCC LGQXXHMEBUOXRP-UHFFFAOYSA-N 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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Description
Ba1-xCaxTi1-yZryO3 (0≦x≦0.2、0≦y≦0.2)(1)
で表されるペロブスカイト型結晶によって構成される圧電体膜であって、前記圧電体膜が、(111)配向を有する金属電極上に形成され、擬立方晶表記で(111)配向していることを特徴とする配向性圧電体膜が提供される。
(1)基板上に(111)配向した金属電極を設ける工程と、
(2)前記基板を500℃以上で熱処理する工程と、
(3)前記基板上に、一般式(1)
Ba1-xCaxTi1-yZryO3 (0≦x≦0.2、0≦y≦0.2) (1)
で表わされる金属酸化物の原料化合物を含むチタン酸バリウム系塗工液組成物を塗布する工程と、
(4)100~700℃で仮焼成して塗膜を形成する工程と、
(5)前記仮焼成して形成した塗膜を、700℃を超える温度で焼成する工程と、
を含むことを特徴とする、配向性圧電体膜の製造方法が提供される。
Ba1-xCaxTi1-yZryO3 (0≦x≦0.2、0≦y≦0.2)(1)
で表されるペロブスカイト型結晶によって構成される圧電体膜であって、前記圧電体膜が、(111)配向を有する金属電極上に形成され、擬立方晶表記で(111)配向していることを特徴とする。
本発明に係るチタン酸バリウム系塗工液組成物は、前記一般式(1)で表わされる金属酸化物の原料化合物を含むものである。ここで、原料化合物は、(i)バリウムアルコキシド、バリウムアルコキシドの加水分解物および前記バリウムアルコキシドの加水分解物の縮合物からなる群から選択される少なくとも1種のバリウム成分を必須成分として含むゾル-ゲル原料を含有する。また、原料化合物は、(ii)チタンアルコキシド、チタンアルコキシドの加水分解物および前記チタンアルコキシドの加水分解物の縮合物からなる群から選択される少なくとも1種のチタン成分を必須成分として含むゾル-ゲル原料を含有する。原料化合物は、(iii)カルシウムアルコキシド、カルシウムアルコキシドの加水分解物および前記カルシウムアルコキシドの加水分解物の縮合物からなる群から選択される少なくとも1種のカルシウム成分を任意成分として含むゾル-ゲル原料を含有する。原料化合物は(iv)ジルコニウムアルコキシド、ジルコニウムアルコキシドの加水分解物および前記ジルコニウムアルコキシドの加水分解物の縮合物からなる群から選択される少なくとも1種のジルコニウム成分を任意成分として含むゾル-ゲル原料を含有する。
で表わされる金属酸化物を製造するためのチタン酸バリウム系塗工液組成物を得ることができる。
チタン酸バリウム系塗工液組成物を用いて塗膜を形成する際には、塗布を行う雰囲気を乾燥雰囲気(乾燥空気もしくは乾燥窒素等の乾燥不活性気体雰囲気)とすることが好ましい。乾燥雰囲気の相対湿度は30%以下にすることが好ましい。
本発明の液体吐出ヘッドは、液体吐出口と、前記液体吐出口に連通する圧力室と、前記圧力室に前記液体吐出口から液体を吐出するための容積変化を生じさせるアクチュエーターと、を有する。そして、前記アクチュエーターは、前記圧力室側から順に設けられた振動板と、下部電極と、基板上に形成されているチタン酸バリウム系膜からなる圧電体膜と、上部電極と、を有することを特徴とする。
下地基板1の材料は少なくとも最表層にSiO2を有し、その他としては、塗工後の乾燥工程において熱負荷を与えても、変形や溶融しない材料が好ましい。また、下地基板1は表面が平滑であり、熱処理時の元素の拡散も防止でき、かつ機械的強度も十分であることが好ましい。また、本実施形態により得られるチタン酸バリウム系膜からなる圧電体膜を用いて液体吐出ヘッドを製造する際には、下地基板1が圧力室を形成するための圧力室の振動板を兼ねていてもよい。例えば、このような目的では、熱酸化によって表層がSiO2の膜であるシリコン(Si)からなる半導体基板を好ましく用いることができるが、ジルコニアやアルミナ、シリカなどのセラミックを用いても構わない。また、最表層をSiO2とするならば、これらの材料を複数種類、組み合わせてもよいし、積層して多層構成として用いてもよい。
まず、熱酸化Si基板上に密着層としてTiをDCスパッタ法により成膜した後、PtをDCスパッタ法により成膜した。成膜したPt層は、XRD、後方散乱電子回折(EBSD)評価によると、(111)面に配向しており、その結晶粒径は20~50nmであった。このPt電極付きSi基板を、アニール処理してPt層の配向度(結晶性と結晶粒サイズ)を向上させた。アニール条件としては、アニール温度1000℃で10分間アニール処理することで、Ptの粒径は100~400nmまで増大し、その平均結晶粒径は約150nmとなり、結晶性も向上した。以上によりPt電極のシード効果を高めた基板が得られた。
本実施例は、(111)配向度の高い膜が得られる安定化剤の種類に関する。
安定化剤を、アセト酢酸ブチル、3-オキソヘキサン酸エチル、2-フルオロアセト酢酸エチル、2-メチルアセト酢酸エチル、2-エチルアセト酢酸エチルとして実施例1と同様の実験を行った。安定化剤の量は3モルで固定し、2-メトキシエタノール:3-メトキシメチルブタノール:安定化剤:バリウム-ジ-i-プロポキシド:チタン-n-ブトキシド:ジルコニウム-n-ブトキシド=18:12:3:1:0.97:0.03とした。安定化剤を添加しないものも作製した。以上により調製した塗工液を用いて、実施例1と同様の方法で成膜し、EBSDによる配向評価を行った。それぞれの安定化剤を用いた塗工液から作製した膜の配向度、及び実施例1のアセト酢酸エチルの配向度を表2に示す。また、膜の表面SEM像を図2(a)~(f)に示す。それぞれ(a)アセト酢酸ブチル、(b)3-オキソヘキサン酸エチル、(c)2-フルオロアセト酢酸エチル、(d)2-メチルアセト酢酸エチル、(e)2-エチルアセト酢酸エチル、(f)安定化剤無添加である。アセト酢酸ブチル、3-オキソヘキサン酸エチルを用いた場合は、アセト酢酸エチルと同様に高い配向度を示した。一方、2-フルオロアセト酢酸エチル、2-メチルアセト酢酸エチル、2-エチルアセト酢酸エチルを用いた場合は、安定化剤を添加しない場合と変わらずランダム配向となっており、配向度は低かった。
本実施例は、111配向度の高い膜が得られるPt電極付きSi基板のアニール条件に関する。
実施例1及び実施例2に示したように、アセト酢酸エチル、アセト酢酸ブチル、3-オキソヘキサン酸エチルを用いた場合に111配向度の高い膜が得られるが、ここでは、膜の配向度とPt電極付きSi基板のアニール温度との関係について評価した。まず、実施例1と同様の手法によりPt電極付きSi基板を用意し、アニール温度を400℃、600℃、800℃、1000℃とし、10分間熱処理した基板を用意した。この基板に、上記3種類の安定化剤を用いた塗工液組成物を用いて、実施例1と同様の方法で膜を製造し、EBSDによる配向評価を行った。基板のアニール温度と圧電体膜の配向度との関係を表3に示す。安定化剤としてアセト酢酸ブチルを用いた場合に最も配向度が高くなり、基板のアニール温度が600℃であれば、およそ0.8の配向度が得られた。このことより、アニール温度を500℃以上とすることにより、配向度の高い圧電体膜が得られることがわかった。安定化剤として3-オキソヘキサン酸エチルを用いた場合は、基板のアニール温度は1000℃で良好な配向を示した。また基板のアニール処理をしなかった場合は、いずれの場合においても配向度に優れた圧電体膜が得られなかった。以上より、Pt電極付きSi基板のアニール条件が同じである場合は、アセト酢酸ブチル、アセト酢酸エチル、3-オキソヘキサン酸エチルの順に圧電体膜の配向度が高くなった。
実施例1~3の条件により得られた(111)配向圧電体膜の層の上に、同様の工程を繰り返すことで厚膜化を行った。安定化剤としてアセト酢酸エチル3モルを添加した塗工液組成物を用い、実施例2と同様の手法による膜形成工程を繰り返すことで厚膜化を行った。乾燥工程として、150℃設定したホットプレート上で5分間熱処理した後、仮焼成工程として、赤外線加熱炉中で450℃の条件で10分間熱処理した後、1000℃で10分間焼成する工程を施した。この工程を16回繰り返すことで厚膜を作製し、SEMによる形態観察とEBSDによる配向評価を行った。表面SEM像を図3(a)に、断面SEM像を図3(b)に示す。SEM結果から、数百nmの粒径を有する膜厚900nmの膜が得られていることがわかった。得られた膜の111配向度は0.90と高い配向度を有していた。
ここで、ρ0は無配向サンプルのX線の回折強度(I0)を用いて計算し、(001)配向した正方晶結晶の場合、全回折強度の和に対する、(111)面の回折強度の合計の割合として、式2により求めた。
(h、k、lは整数である。)
ρは配向膜のX線の回折強度(I)を用いて計算し、(111)配向した正方晶結晶の場合、全回折強度の和に対する、(111)面の回折強度の合計の割合として、上式2と同様に式3により求めた。
作製した(111)配向した厚膜のX線回折結果を図4に示す。ほぼ111の回折ピークのみとなっており、ロットゲーリングファクターF=0.98と高い配向度を有していた。
2 中間層
3 下部電極
4 圧電体膜
21 液体吐出ヘッド用基板
21A 開口部
22 液体吐出口
23 圧力室
24 ノズルプレート
25 アクチュエーター
26 振動板
27 圧電層
28 下部電極
29 上部電極
30 圧電体素子
M 液体吐出ヘッド
Claims (10)
- 下記一般式(1)
Ba1-xCaxTi1-yZryO3 (0≦x≦0.2、0≦y≦0.2)(1)
で表されるペロブスカイト型結晶によって構成される配向性圧電体膜であって、前記配向性圧電体膜が、(111)配向を有する金属電極上に形成され、前記配向性圧電体膜が擬立方晶表記で(111)配向し、
後方散乱電子回折(EBSD)法にて測定された(111)配向の存在割合が、膜表面で50%以上であり、かつ膜の法線方向の逆極点図において、(111)配向の角度ばらつきが5度以内であることを特徴とする、配向性圧電体膜。 - 前記金属電極が、白金および金の少なくとも1種を含むことを特徴とする、請求項1に記載の配向性圧電体膜。
- (1)基板上に(111)配向した金属電極を設ける工程と、
(2)前記基板を500℃以上で熱処理する工程と、
(3)前記基板上に、一般式(1)
Ba1-xCaxTi1-yZryO3 (0≦x≦0.2、0≦y≦0.2) (1)
で表わされる金属酸化物の原料化合物を含むチタン酸バリウム系塗工液組成物を塗布する工程と、
(4)200℃を超え、700℃以下の温度で仮焼成して塗膜を形成する工程と、
(5)前記仮焼成して形成した塗膜を、700℃を超える温度で焼成する工程と、
を含むことを特徴とする、請求項1または2に記載の配向性圧電体膜の製造方法。 - 塗膜の膜厚が30~150nmとなるまで、前記工程(3)及び(4)を繰り返すことを特徴とする、請求項3に記載の配向性圧電体膜の製造方法。
- 前記配向性圧電体膜の膜厚が30~150nmとなるまで前記工程(3)~(5)を繰り返すことを特徴とする、請求項3に記載の配向性圧電体膜の製造方法。
- 前記工程(3)は、ディッピング法、スピンコート法、スプレー法、印刷法およびフローコート法からなる群から選択される少なくとも1種の塗布法により塗布することを特徴とする、請求項3~5のいずれか1項に記載の配向性圧電体膜の製造方法。
- 前記チタン酸バリウム系塗工液組成物が、
(a)(i)バリウムアルコキシド、前記バリウムアルコキシドの加水分解物および前記バリウムアルコキシドの加水分解物の縮合物からなる群から選択される少なくとも1種のバリウム成分と、
(ii)チタンアルコキシド、前記チタンアルコキシドの加水分解物および前記チタンアルコキシドの加水分解物の縮合物からなる群から選択される少なくとも1種のチタン成分と、を含む、
ゾル-ゲル原料、および
(b)β-ケトエステル化合物、
を含むことを特徴とする、請求項3~6のいずれか1項に記載の配向性圧電体膜の製造方法。 - 前記(a)ゾル-ゲル原料が、(iii)カルシウムアルコキシド、前記カルシウムアルコキシドの加水分解物および前記カルシウムアルコキシドの加水分解物の縮合物からなる群から選択される少なくとも1種のカルシウム成分をさらに含むことを特徴とする、請求項7に記載の配向性圧電体膜の製造方法。
- 前記(a)ゾル-ゲル原料が、(iv)ジルコニウムアルコキシド、前記ジルコニウムアルコキシドの加水分解物、および前記ジルコニウムアルコキシドの加水分解物の縮合物からなる群から選択される少なくとも1種のジルコニウム成分をさらに含むことを特徴とする、請求項7または8に記載の配向性圧電体膜の製造方法。
- 液体吐出口と、前記液体吐出口に連通する圧力室と、前記圧力室に前記液体吐出口から液体を吐出するための容積変化を生じさせるアクチュエーターと、を有し、
前記アクチュエーターは、前記圧力室側から順に設けられた振動板と、下部電極と、請求項1または2に記載のチタン酸バリウム系膜からなる圧電体膜と、上部電極と、を有することを特徴とする、液体吐出ヘッド。
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