JP2010143788A - 酸窒化物圧電材料及びその製造方法 - Google Patents
酸窒化物圧電材料及びその製造方法 Download PDFInfo
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- JP2010143788A JP2010143788A JP2008322831A JP2008322831A JP2010143788A JP 2010143788 A JP2010143788 A JP 2010143788A JP 2008322831 A JP2008322831 A JP 2008322831A JP 2008322831 A JP2008322831 A JP 2008322831A JP 2010143788 A JP2010143788 A JP 2010143788A
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Abstract
Description
R.Caracas et al.,Applied Physics Letters,Vol.91,092902(2007)
本発明に係る酸窒化物圧電材料は、下記一般式(1)で表される正方晶ペロブスカイト型酸窒化物からなり、窒素原子がc軸方向に配向していることを特徴とする。
酸窒化物圧電材料は、組成のずれが生じるため、x、y、zは等しくならず、δは0にはならない。また、より望ましくはx=y=zであるが、x≒y>zが好ましい。zがx、yと比べ小さい理由は、窒素原子が導入されにくく、代わりに酸素が取り込まれるためである。そのような組成比でも、c/a比的には1.0を超えるために強誘電性を発現し、圧電材料となる。
配向軸は、ミラー指数を用いて表現する。配向を有する場合の配向軸は、<100>、<110>、<111>が望ましい。
F(HKL)={(P−P0)/(1−P0)}×100(%) ・・・(1)
但し、P=ΣI(HKL)/ΣI(hkl)、
P0=ΣI0(HKL)/ΣI0(hkl)。
ΣI0(hkl)は、酸窒化物配向セラミクスと同一組成を有する酸窒化物無配向セラミクスについて測定されたすべての結晶面(hkl)のX線回折強度の総和である。
ΣI0(HKL)は、酸窒化物配向セラミクスと同一組成を有する酸窒化物無配向セラミクスについて測定された結晶学的に等価な特定の結晶面(HKL)のX線回折強度の総和である。
前記配向工程において、一軸加圧しながら焼結して前記形状異方性粒子を配向させることが好ましい。
第1の実施形態として、一般式(1)におけるAがBa、BがTi、B’がSiからなる酸窒化物に関する実施形態の説明を行う。本実施形態においては、一例として、Ba1−xBixTi1−xSixO3−xNxについて説明を行う。
第一原理計算とはフィッティングパラメータ等を一切使用しない電子状態計算手法の総称であり、単位格子や分子等を構成する各原子の原子番号と座標を入力するだけで、電子状態計算が可能な手法である。
但し、x=0であるBaTiO3及びx=1であるBiSiO2Nの結晶構造については、「ABINIT」と呼ばれる第一原理計算パッケージプログラムによる計算より、予め別途求めている。「ABINIT」は、Cornell大学のX.Gonze教授が中心となって開発した構造最適化も可能なパッケージプログラムである。
ABX3型ペロブスカイト酸窒化物には2つの構造が存在する。これら2つの構造は、図1に示すように、N原子がc軸方向に存在している構造(Nc構造)と図2に示すようにN原子がab面内に存在している構造(Nab構造)である。図1に示すように酸窒化物ABO2NのAサイトの原子をA原子、Bサイトの原子をB原子とよぶ。安定構造を求めるには、A原子とB原子として、然るべき元素を選択し、Nc構造及びNab構造をそれぞれ初期構造として用意し、電子状態計算を行えばよい。係る電子状態計算から求めた安定構造における全エネルギーを、それぞれE_Nc及びE_Nabと定義する。全エネルギーの小さな方が最安定構造、他方が準安定構造であると結論出来る。
また、前記酸窒化物が正方晶からなり、前記酸窒化物の窒素原子がc軸方向に存在することが好ましい。
xが0.5の時、電子状態計算を行って構造最適化することで、圧電定数を求めた結果、d33が73.53[C/m2]となり圧電性を確認した。
粉体の場合、Ba0.6Bi0.4Ti0.6Si0.4O2.6N0.4は以下のように固相合成した。BaCO3((株)高純度化学製、99.99%)とTiO2((株)高純度化学製、99.99%)とBi2O3((株)高純度化学製、99.999%)とSiO2((株)高純度化学製、99.999%)を3:3:1:2のモル比でエタノール溶液に加え、遊星ボールミルを用いて、1時間混合した。Biは蒸気圧が高く、Biが不足する可能性があるので、前述のモル比よりも過剰に加えることが望ましい。
一方、薄膜の場合、スパッタリング法、ゾルゲル法、レーザーアブレーション法、CVD法などの公知の方法を用いて容易に成膜が可能である。好ましくは、スパッタリング法である。例えばスパッタ装置による成膜の場合、N2ガス、O2ガス及びArガスが流入しているチャンバー内に、例えば、Bi、Ba、Ti、及びSiの金属ホルダーを用意し、それらのホルダー上にイオン源となるArビームを照射した。所望とする元素組成が得られるように成膜条件を設定し、Arビームにより叩き出された各金属をチャンバー内に備えた基板上に飛翔させることにより、目的とするBa0.6Bi0.4Ti0.6Si0.4O2.6N0.4圧電体膜を形成することが出来た。
第2の実施形態として、酸窒化物において、配向軸を有することについての説明をする。
配向軸を有する酸窒化物圧電材料の工程フローについて図7を用いて説明する。
まず、酸窒化物圧電材料の原料について説明する。原料として、形状異方性粒子31と等方性であるマトリクス粒子32を用いる。
形状異方性粒子とマトリクス粒子は、窒化物、もしくは、酸窒化物、もしくは酸化物のいずれかである。窒化物及び酸窒化物は、酸化物を窒化することで得られる。
次に、酸窒化物圧電材料の製造工程について説明する。製造工程は、混合工程、成形工程、焼結工程から構成される。
この場合、形状異方性粒子が図7に示すように面配向するように成形しても良く、あるいは、図7に示すように軸配向するように成形しても良い。成形方法については、形状異方性粒子を配向させることが可能な方法であれば良く、特に限定されるものではない。形状異方性粒子を面配向させる成形方法として、具体的には、ドクターブレード法、プレス成形法、圧延法等が好適な一例として挙げられる。
また、形状異方性粒子が面配向した成形体の厚さを、配向度を上げるために、成形体に対し、さらに積層圧着、プレス、圧延などの処理を行っても良い。この成形体に対して、いずれか1種類の処理を行っても良く、あるいは、2種以上の処理を行っても良い。
最後に、焼結工程について説明する。焼結工程は、成形工程で得られた成形体を加熱し、焼結させる工程である。
加熱方法は、常圧焼結法、あるいは、一軸加圧焼結法、ホットプレス、ホットフォージング、HIP等の加圧焼結法のいずれを用いても良く、組成、用途等に応じて、最適な方法を選択することができる。好ましくは、一軸加圧焼結を行うことで、配高度をさらに高めることができる。
実施例1
Ba0.6Bi0.4Ti0.6Si0.4O2.6N0.4で表される酸窒化物圧電材料の製造方法について述べる。
BaCO3((株)高純度化学製、99.99%)、TiO2((株)高純度化学製、99.99%)、Bi2O3((株)高純度化学製、99.999%)、GeO2((株)高純度化学製、99.999%)を用いて圧粉体を形成した。これをスパッタリング成膜用のターゲットとして用いた。ガスとしてN2/O2/Ar=4/1/20で、ガス圧を0.1Paから0.7Paに振りLa−SrTiO3(100)基板上に基板温度500℃から700℃でrf−スパッタリング成膜を行った。各元素比を振り、A1−xBix+δ1B1−yB’y−+δ2O3−zNzでAがBa,BとしてTi、B’がGeの酸窒化物を400nmから600nmの膜厚で成膜した。成膜条件で、ガス圧を0.2Paから0.5Paで、基板温度550℃から650℃で成膜した組成がx=0.35から0.65、y=0.35から0.65の膜がX線解析より異相のない良質なABX3型ペロブスカイト化合物で強誘電体であることを確認した。また、窒素量としてzは、0.35から0.5で、δ1とδ2は±0.2の範囲内であった。
2 B原子
3 O原子
4 N原子
11 電気炉
12 酸窒化物
13 石英管
14 トラップ
21 粒
22 単位格子
23 セラミックス
24 分極軸
25 窒素原子
31 形状異方性粒子
32 マトリクス粒子
Claims (8)
- 前記AはBa,Sr,Caから選ばれた少なくとも1種であり、BおよびB’はTi,Zr,Hf,Si,Ge,Snから選ばれた少なくとも1種であることを特徴とする請求項1に記載の酸窒化物圧電材料。
- 前記AがBa、BがTi、B’がSiであることを特徴とする請求項1または2に記載の酸窒化物圧電材料。
- 前記酸窒化物が正方晶からなり、単位格子のc軸長の長さcとa軸長の長さaの比c/aが1.15以上1.269以下であることを特徴とする請求項1乃至3のいずれかの項に記載の酸窒化物圧電材料。
- 前記配向工程において、前記形状異方性粒子をバインダーによってスラリーとし、テープキャスティングして前記形状異方性粒子を配向させることを特徴とする請求項5または6に記載の酸窒化物圧電材料の製造方法。
- 前記配向工程において、一軸加圧しながら焼結して前記形状異方性粒子を配向させることを特徴とする請求項5乃至7のいずれかの項に記載の酸窒化物圧電材料の製造方法。
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US20100155647A1 (en) | 2010-06-24 |
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