WO2015146607A1 - Mn及びNbドープのPZT系圧電体膜形成用組成物 - Google Patents
Mn及びNbドープのPZT系圧電体膜形成用組成物 Download PDFInfo
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Abstract
Description
本願は、2014年3月28日に、日本に出願された特願2014-067835号に基づき優先権を主張し、その内容をここに援用する。
式(1)中、d31は圧電定数、ε33は誘電率を示す。
+(300clogηrel +(c+1.5clogηrel)2)1/2/(0.15c+0.003c2)
上記式中、「ηrel」は、ポリビニルピロリドン水溶液の水に対する相対粘度を示し、「c」は、ポリビニルピロリドン水溶液中のポリビニルピロリドン濃度(質量%)を示す。ポリビニルピロリドンのk値は、30~90であることが好ましい。厚みのある圧電体膜を形成するためには、組成物を基板等へ塗布する際、塗布された塗膜(ゲル膜)がその厚さを維持するために十分な粘度が必要となるが、k値が下限値未満では、それが得られにくい。一方、上限値を超えると粘度が高くなりすぎて、組成物を均一に塗布することが困難になる。
ここで、上記PZT系前駆体1モルとは、組成式Pbx(MnyNbzZrtTis)O(x+3y+5z/2+t/2+s/2)で表される化合物1モル中に含有される前駆物質の量である。
また、モノマー換算でのモル値とは、高分子を構成するモノマーの分子量を基準としたモル値を意味し、PZT前駆体1モルに対するモノマー換算のモル値とは、高分子(この場合はポリビニルピロリドン)を構成するモノマーの分子量を基準としたPZT前駆体1モルに対するモル値を意味する。
なお、濾過処理等によるパーティクルの除去によって組成物内の0.2μm以上のパーティクルは除去されている状態であることが好ましい。なお、組成物中のパーティクルの個数の測定には、光散乱式パーティクルカウンターを用いる。
先ず、反応容器に酢酸鉛三水和物(Pb源)とプロピレングリコール(ジオール)とを入れ、窒素雰囲気中、150℃の温度で1時間還流した後、この反応容器に2-エチルヘキサン酸マンガン(Mn源)、ニオブペンタエトキシド(Nb源)、ジルコニウムテトラブトキシド(Zr源)、チタンテトライソプロポキシド(Ti源)及びアセチルアセトン(安定化剤)を更に加え、窒素雰囲気中、150℃の温度で1時間還流して反応させることにより、合成液を調製した。ここで、上記酢酸鉛三水和物(Pb源)、2-エチルヘキサン酸マンガン(Mn源)、ニオブペンタエトキシド(Nb源)、ジルコニウムテトラブトキシド(Zr源)及びチタンテトライソプロポキシド(Ti源)の各PZT系前駆体は、液中の金属原子比(Pb:Mn:Nb:Zr:Ti)が以下の表1に示す値になるように秤量した。また、プロピレングリコール(ジオール)を、調製後の組成物100質量%に対して16質量%となるように添加し、アセチルアセトン(安定化剤)を、調製後の組成物に含まれるMn、Nb、Zr及びTiの総量1モルに対して2モルとなる割合で添加した。次いで、上記合成液100質量%中に占めるPZT系前駆体の濃度が酸化物濃度で35質量%になるように、減圧蒸留を行って不要な溶媒を除去した。ここで、合成液中に占めるPZT系前駆体の濃度における酸化物濃度とは、合成液に含まれる全ての金属原子が目的の酸化物になったと仮定して算出した、合成液100質量%に占める金属酸化物の濃度(酸化物換算値)をいう。
調製後の組成物100質量%に占めるプロピレングリコール(ジオール)の割合が、以下の表1に示す割合になるよう調整したこと以外は、実施例1と同様にして組成物を調製し、圧電体膜を形成した。なお、実施例2,3で形成された圧電体膜は、以下の表3に示す組成の膜であった。
組成物100質量%に占めるプロピレングリコール(ジオール)の割合が、以下の表1に示す割合になるよう調整したこと、及びMn、Nb、Zr及びTiの総量1モルに対するアセチルアセトンの割合を、以下の表1に示す割合に調整したこと以外は、実施例1と同様にして組成物を調製し、圧電体膜を形成した。なお、実施例4~6で形成された圧電体膜は、以下の表3に示す組成の膜であった。
組成物100質量%に占めるプロピレングリコール(ジオール)の割合が、以下の表1に示す割合になるよう調整したこと、及び組成物100質量%中に占めるPZT系前駆体の濃度が、酸化物濃度で、以下の表1に示す値になるように調整したこと以外は、実施例1と同様にして組成物を調製し、圧電体膜を形成した。なお、形成後の圧電体膜は、以下の表3に示す組成の膜であった。
先ず、反応容器に酢酸鉛三水和物(Pb源)とプロピレングリコール(ジオール)とを入れ、窒素雰囲気中、150℃の温度で1時間還流した後、この反応容器に2-エチルヘキサン酸マンガン(Mn源)、ニオブペンタエトキシド(Nb源)、ジルコニウムテトラブトキシド(Zr源)、チタンテトライソプロポキシド(Ti源)及びアセチルアセトン(安定化剤)を更に加え、窒素雰囲気中、150℃の温度で1時間還流して反応させることにより、合成液を調製した。ここで、上記酢酸鉛三水和物(Pb源)、2-エチルヘキサン酸マンガン(Mn源)、ニオブペンタエトキシド(Nb源)、ジルコニウムテトラブトキシド(Zr源)及びチタンテトライソプロポキシド(Ti源)の各PZT系前駆体は、液中の金属原子比(Pb:Mn:Nb:Zr:Ti)が以下の表1に示す値になるように秤量した。また、プロピレングリコール(ジオール)を、調製後の組成物100質量%に対して30質量%となるように添加し、アセチルアセトン(安定化剤)を、調製後の組成物に含まれるMn、Nb、Zr及びTiの総量1モルに対して2モルとなるように添加した。次いで、上記合成液100質量%中に占めるPZT系前駆体の濃度が酸化物濃度で35質量%になるように、減圧蒸留を行って不要な溶媒を除去した。ここで、合成液中に占めるPZT系前駆体の濃度における酸化物濃度とは、合成液に含まれる全ての金属原子が目的の酸化物になったと仮定して算出した、合成液100質量%に占める金属酸化物の濃度(酸化物換算値)をいう。
組成物100質量%中に占めるPZT系前駆体の濃度が、酸化物濃度で、以下の表1に示す値になるように調整したこと以外は、実施例8と同様にして組成物を調製し、圧電体膜を形成した。なお、形成後の圧電体膜は、以下の表3に示す組成の膜であった。
組成物100質量%に占めるプロピレングリコール(ジオール)の割合が、以下の表1に示す割合になるよう調整したこと以外は、実施例1と同様にして組成物を調製し、圧電体膜を形成した。なお、実施例10,実施例11で形成された圧電体膜は、以下の表3に示す組成の膜であった。
組成物100質量%に占めるプロピレングリコール(ジオール)の割合が、以下の表1に示す割合になるよう調整したこと、及び調製後の組成物に含まれるMn、Nb、Zr及びTiの総量1モルに対するアセチルアセトンの割合を、以下の表1に示す割合に調整したこと以外は、実施例1と同様にして組成物を調製し、圧電体膜を形成した。実施例12,実施例13で形成された圧電体膜は、以下の表3に示す組成の膜であった。
Mn源、Nb源としてのPZT系前駆体を使用せず、酢酸鉛三水和物(Pb源)、ジルコニウムテトラブトキシド(Zr源)及びチタンテトライソプロポキシド(Ti源)の各PZT系前駆体を、液中の金属原子比(Pb:Mn:Nb:Zr:Ti)が以下の表1に示す値になるように秤量したこと、PZT系前駆体1モルに対してモノマー換算で以下の表1に示す割合となるようにポリビニルピロリドン(PVP:k値=30)を添加したこと以外は、実施例8と同様にして組成物を調製し、圧電体膜を形成した。なお、形成後の圧電体膜は、以下の表3に示す組成の膜であった。
ここで、表1及び後述の表2において、「ジオール[質量%]」欄の数値は、組成物100質量%に対するジオールの量(質量%)である。「アセチルアセトン[モル]」欄の数値は、調製後の組成物に含まれるMn、Nb、Zr及びTiの総量1モルに対するアセチルアセトンの量(モル)である。「PVP[モル]」欄の数値は、PZT系前駆体1モルに対する、モノマー換算したポリビニルピロリドンの量(モル)である。「前駆体濃度(酸化物濃度)[質量%]」欄の数値は、組成物100質量%に占める、酸化物換算した金属酸化物の濃度(質量%)である。
酢酸鉛三水和物(Pb源)、2-エチルヘキサン酸マンガン(Mn源)、ニオブペンタエトキシド(Nb源)、ジルコニウムテトラブトキシド(Zr源)及びチタンテトライソプロポキシド(Ti源)の各PZT系前駆体を、液中の金属原子比(Pb:Mn:Nb:Zr:Ti)が以下の表2に示す値になるように秤量したこと、及びPZT系前駆体1モルに対してモノマー換算で以下の表2に示す割合となるようにポリビニルピロリドン(PVP:k値=30)を添加したこと以外は、実施例8と同様にして組成物を調製し、圧電体膜を形成した。実施例14~21、比較例2~9で形成した圧電体膜は、以下の表4に示す組成の膜であった。
実施例1~21及び比較例1~9で形成した圧電体膜について、膜組成、ヒステリシスのずれ、比誘電率、圧電定数e31.f、クラックの有無、結晶の(100)面における配向度をそれぞれ評価した。また、実施例1~21及び比較例1~9で調整した組成物の保存安定性を評価した。これらの結果を以下の表3,表4に示す。
具体的には、1kHzの周波数で25Vの電圧を印加して圧電体膜の分極量のヒステリシスを測定し、図1のようなX軸を電界(kV/cm)、Y軸を分極量(μC/cm2)としたヒステリシス曲線を得た。そして、得られたヒステリシス曲線において、分極量が0の場合の正側、負側の抗電界の絶対値をそれぞれEc+(kV/cm)、Ec-(kV/cm)とし、Ec+-(Ec++Ec-)/2の値を求め、ヒステリシスのずれとした。なお、比較のため、この方法によって測定された実施例16及び比較例1のヒステリシス曲線を図1に示す。
Claims (6)
- Mn及びNbドープの複合金属酸化物からなるPZT系圧電体膜の形成に用いられる組成物であり、
前記複合金属酸化物を構成する各金属原子を含むPZT系前駆体を含み、
前記組成物中の金属原子比(Pb:Mn:Nb:Zr:Ti)が(1.00~1.25):(0.002~0.056):(0.002~0.056):(0.40~0.60):(0.40~0.60)を満たし、かつ前記Mn及びNbの金属原子比の合計を1としたときの前記Mnの割合が0.20~0.80、前記Zr及びTiの金属原子比の合計を1としたときの前記Zrの割合が0.40~0.60、前記Mn、Nb、Zr及びTiの金属原子比の合計を1としたときの前記Zr及びTiの合計割合が0.9300~0.9902となる割合で、前記PZT系前駆体を含む、Mn及びNbドープのPZT系圧電体膜形成用組成物。 - 安定化剤としてアセチルアセトンを、溶媒としてジオールを更に含む請求項1記載のMn及びNbドープのPZT系圧電体膜形成用組成物。
- 前記ジオールがプロピレングリコール又はエチレングリコールである請求項2記載のMn及びNbドープのPZT系圧電体膜形成用組成物。
- 組成物中に含まれる前記Mn、Nb、Zr及びTiの総量を1モルとしたとき、組成物中に含まれる前記アセチルアセトンの含有量が0.5~4モルである請求項2又は3記載のMn及びNbドープのPZT系圧電体膜形成用組成物。
- 組成物100質量%中の前記ジオールの割合が16~56質量%である請求項2ないし4いずれか1項に記載のMn及びNbドープのPZT系圧電体膜形成用組成物。
- ポリビニルピロリドンを、前記PZT系前駆体1モルに対してモノマー換算で0.01~0.25モルの割合で更に含む請求項1ないし5いずれか1項に記載のMn及びNbドープのPZT系圧電体膜形成用組成物。
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