JP5715309B2 - 無鉛圧電磁器組成物、それを用いた圧電素子、装置、及び、無鉛圧電磁器組成物の製造方法 - Google Patents
無鉛圧電磁器組成物、それを用いた圧電素子、装置、及び、無鉛圧電磁器組成物の製造方法 Download PDFInfo
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- JP5715309B2 JP5715309B2 JP2014539939A JP2014539939A JP5715309B2 JP 5715309 B2 JP5715309 B2 JP 5715309B2 JP 2014539939 A JP2014539939 A JP 2014539939A JP 2014539939 A JP2014539939 A JP 2014539939A JP 5715309 B2 JP5715309 B2 JP 5715309B2
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- G01L23/22—Devices or apparatus for measuring or indicating or recording rapid changes, such as oscillations, in the pressure of steam, gas, or liquid; Indicators for determining work or energy of steam, internal-combustion, or other fluid-pressure engines from the condition of the working fluid for detecting or indicating knocks in internal-combustion engines; Units comprising pressure-sensitive members combined with ignitors for firing internal-combustion engines
- G01L23/221—Devices or apparatus for measuring or indicating or recording rapid changes, such as oscillations, in the pressure of steam, gas, or liquid; Indicators for determining work or energy of steam, internal-combustion, or other fluid-pressure engines from the condition of the working fluid for detecting or indicating knocks in internal-combustion engines; Units comprising pressure-sensitive members combined with ignitors for firing internal-combustion engines for detecting or indicating knocks in internal combustion engines
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Description
この無鉛圧電磁器組成物によれば、スピネル化合物で構成される第2結晶相が、第1結晶相の構造を安定化するので、圧電特性及び絶縁性に優れた無鉛圧電磁器組成物を提供することができる。
この構成によれば、第2結晶相として、安定した構造のスピネル化合物を得ることができ、この結果、圧電特性に優れた無鉛圧電磁器組成物を提供することができる。
この構成によれば、第2結晶相として、安定した構造のスピネル化合物を得ることができ、この結果、圧電特性に優れた無鉛圧電磁器組成物を提供することができる。
この構成によれば、第2結晶相として、安定した構造のスピネル化合物を得ることができ、この結果、圧電特性に優れた無鉛圧電磁器組成物を提供することができる。
この無鉛圧電磁器組成物によれば、副相が、主相の空孔を充填することによって主相(第1結晶相)の構造を安定化するので、圧電特性に優れた無鉛圧電磁器組成物を提供することができる。
この構成によれば、無鉛圧電磁器組成物の圧電特性及び絶縁特性を更に向上することができる。
この構成によれば、無鉛圧電磁器組成物の特性を更に向上できる。
この構成によれば、第3結晶相によって第2結晶相の構造が安定化するので、無鉛圧電磁器組成物を安定化できる。
この構成によれば、第2結晶相による第1結晶相の構造を安定化の効果が顕著となるので、無鉛圧電磁器組成物の特性を更に向上できる。
この構成によれば、圧電特性に優れた無鉛圧電磁器組成物を得ることができる。
この構成によれば、無鉛圧電磁器組成物の特性を向上させることができる。
この構成によれば、無鉛圧電磁器組成物の特性をさらに向上させることができる。
この構成によれば、前記ニオブ/タンタル酸アルカリ系ペロブスカイト酸化物がタンタル酸アルカリ系ペロブスカイト酸化物である場合と比べて、キュリー温度(Tc)が高い無鉛圧電磁器組成物を提供することができる。
この方法によれば、圧電特性を有するニオブ/タンタル酸アルカリ系ペロブスカイト酸化物からなる第1結晶相と、M−Ti−O系スピネル化合物からなる第2結晶相と、を含む、圧電特性に優れた無鉛圧電磁器組成物を作成することができる。
(KaNabLicCd)e(DfEg)Oh …(1)
ここで、元素CはCa(カルシウム),Sr(ストロンチウム),Ba(バリウム)の一種以上、元素DはNb(ニオブ),Ta(タンタル),Ti(チタン),Zr(ジルコニウム),Hf(ハフニウム),Sn(スズ),Sb(アンチモン),Si(ケイ素)のうちの少なくともNb又はTaを含む一種以上、元素EはMg(マグネシウム),Al(アルミニウム),Sc(スカンジウム),Mn(マンガン),Fe(鉄),Co(コバルト),Ni(ニッケル),Zn(亜鉛),Ga(ガリウム),Y(イットリウム)の一種以上であり、a+b+c+d=1、eは任意、f+g=1、hはペロブスカイトを構成する任意の値である。
(KaNabLicC1d1C2d2)e(D1f1D2f2D3f3E1g1E2g2E3g3)Oh …(1a)
ここで、a+b+c+d1+d2=1、eは任意、f1+f2+f3+g1+g2+g3=1、hはペロブスカイトを構成する任意の値である。この組成式(1a)は、上記組成式(1)と等価である。この例から理解できるように、元素Cが2種類の金属元素を含む場合には、元素Cの係数dの値は、2種類の元素C1,C2の係数d1,d2の和で表される。また、元素Dが3種類の金属元素を含む場合には、元素Dの係数fの値は、3種類の元素D1,D2,D3の係数f1,f2,f3の和で表される。元素Dが4種以上の金属元素を含む場合も同様である。
<好ましい第2結晶相の組成式>
MxTiOy …(2)
ここで、元素Mは、1〜4価の金属元素であり、Li(リチウム),Mg(マグネシウム),Al(アルミニウム),Sc(スカンジウム),Cr(クロム),Mn(マンガン),Fe(鉄),Co(コバルト),Ni(ニッケル),Zn(亜鉛),Ga(ガリウム),Y(イットリウム),Zr(ジルコニウム),Sn(スズ),Sb(アンチモン),Si(ケイ素),Hf(ハフニウム)のうちの少なくとも1種である。なお、元素MとしてLiを含む場合には、第2結晶相がスピネル化合物を形成するために、上記金属元素のうちのLi以外の他の1種以上の金属元素がLiとともに含まれることが好ましい。係数x,yは、Tiの含有量を1としたときの相対値である。第2結晶相がスピネル化合物を形成するために、係数xは、0.5≦x≦5.0を満たすことが好ましい。また、係数yは、スピネル化合物を形成する任意の値であるが、典型的には2≦y≦8を満たすことが好ましい。スピネル化合物で構成される第2結晶相は、第1結晶相の構造を安定化するので、圧電特性に優れた圧電磁器組成物を得ることができる。なお、圧電特性の観点からは、2価の金属元素Mを2個含む組成式M2TiO4 、又は、(M1,M2)TiO4 で表される第2結晶相を採用することが好ましい。
(1)Liを含むスピネル化合物の例
LiAlTiO4,LiCrTiO4,LiFeTiO4,LiGaTiO4,LiMnTiO4,LiYTiO4,LiScTiO4,LiCo0.5Ti1.5O4,LiMg0.5Ti1.5O4,LiMn0.5Ti1.5O4,LiZn0.5Ti1.5O4,Li1.33(Zr,Ti)1.67O4
(2)Coを含むスピネル化合物の例
Co2TiO4,CoZnTiO4,CoMgTiO4,CoNiTiO4,CoFeTiO4,CoMnTiO4
(3)Znを含むスピネル化合物の例
Zn2TiO4,ZnMgTiO4,ZnNiTiO4,ZnFeTiO4,ZnMnTiO4
(4)Mgを含むスピネル化合物の例
Mg2TiO4,MgNiTiO4,MgFeTiO4,MgMnTiO4
(5)Niを含むスピネル化合物の例
Ni2TiO4,NiFeTiO4,NiMnTiO4,Ni1.5FeTi0.5O4,Ni2(Ti,Zr)O4
(6)Feを含むスピネル化合物の例
Fe2TiO4,FeMnTiO4,Mn1.5FeTi0.5O4
(7)Mnを含むスピネル化合物の例
Mn2TiO4
(8)好ましいスピネル化合物の例
第2結晶相のM−Ti−O系スピネル化合物は、NiFeTiO4,MgFeTiO4,Ni2(Ti,Zr)O4,Ni1.5FeTi0.5O4,CoMgTiO4,CoFeTiO4,(Fe,Zn,Co)TiO4の中から選ばれた一種以上を含むことが特に好ましい。
<グループ1>サンプルS100〜S114:第1結晶相の元素DがNb,Ti,Zrであり、第2結晶相の元素Mが2〜3種類の金属元素であるサンプル群。但し、サンプルS107は、第1結晶相の元素Dとして、Zrの代わりにHfを含んでいる。
<グループ2>サンプルS114〜S117:第1結晶相の元素EがCo,Feであり、第2結晶相の元素MもCo,Feであるサンプル群。なお、サンプルS114は、グループ1とグループ2の両方に含まれている。サンプルS114とサンプルS115は、第1結晶相の組成の係数a〜dの値が互いに異なる。サンプルS116は第1結晶相の元素DがTaを含む点で他のサンプルS114,S115,S117と異なる。サンプルS117は、第1結晶相の元素CがSrを含む点で他のサンプルS114,S115,S116と異なる。
<グループ3>サンプルS118〜S120:第1結晶相の元素DがNb,Ti,Zrに加えてSn,Sb,Siのいずれか一種類を含み、第2結晶相の元素MがZnに加えてSn,Sb,Siのいずれか一種類を含むサンプル群。
<グループ4>サンプルS121〜S126:第1結晶相の元素DがNb,Ti,Zr、元素EがFe,Ni,Mg,Zn,Mn,Coのいずれか1種類であり、第2結晶相の元素MもFe,Ni,Mg,Zn,Mn,Coのいずれか1種類であるサンプル群。
<グループ5>サンプルS127〜S131:第1結晶相の元素DがNb,Ti,Zr、元素EがFe,Zn,Coであり、第2結晶相の元素MもFe,Zn,Coであるサンプル群。なお、サンプルS131の第2結晶相の組成を詳細に分析したところ、正確な組成式はMg1.1Fe1.55TiOyであった。
(1)第2結晶相の元素Mが1種類の金属元素であるサンプルS121〜S126に比べて、元素Mが2種類以上の金属元素であるサンプルS100〜S102,S105〜S120,S127〜S131の方が圧電特性(特に圧電定数d33及び電気機械結合係数kr)の点で好ましい。特に、第2結晶相の元素Mが2種類以上の金属元素であり、且つ、元素MとしてMn(マンガン)を使用したサンプルS103,S104では、元素Mが1種類の金属元素であるサンプルS121〜S126に比べて、同等の圧電特性を得つつ、機械的品質係数Qmを大きくできる点で好ましい。
(2)第1結晶相の元素DとしてHfを使用したサンプルS107も、HfでなくZrを使用したサンプルS100〜S106,S108〜S114とほぼ同等の良好な圧電特性を有する。
(3)第1結晶相の元素DとしてTaを使用したサンプルS116も良好な圧電特性を有するが、TaでなくZrを使用したサンプルS114,S115の方が圧電特性の点でより好ましい。
(4)第1結晶相の元素CとしてSrを使用したサンプルS117も、SrでなくBaを使用したサンプルS114,S115とほぼ同等の良好な圧電特性を有する。
(5)第1結晶相の元素DとしてSn,Sb,Siのいずれか一種類を含むサンプルS118〜S120についても、比較的良好な圧電特性を有する。
(6)副相が、A3B5O15系化合物からなる第3結晶相を含むサンプルS100,S106,S107,S109,S112,S121,S122,S124,S125,SS127〜S131も、良好な圧電特性を有する。なお、上述したように、これらの第3結晶相は、図12A,12Bにおける第1結晶相と第2結晶相の組成に応じて図1の工程に従って圧電磁器組成物を作成した結果、析出したものである。但し、副相が第3結晶相を含む圧電磁器組成物を作成する場合に、意図的に第3結晶相の原料を副相の原料に混合するようにしても良い。
(i)圧電素子を恒温槽にいれ、室温での圧電特性を評価する(初期値)。
(ii)次に、2℃/分の温度変化率で−50℃から+150℃の間で温度を変化させる熱サイクルを、1000回繰り返す(−50℃と+150℃での保持時間は1時間)。
(iii)その後、室温にて圧電特性を再度、評価する(熱サイクル後の特性値)。
なお、この発明は上記の実施例や実施形態に限られるものではなく、その要旨を逸脱しない範囲において種々の態様において実施することが可能である。例えば、圧電特性に影響を与えず、かつ、−50℃〜+150℃の間において急激な特性の変動が無いという性状を有する範囲であれば、上記した実施例の圧電磁器組成物に、第2結晶相以外の副相が含まれていてもよい。その副相としては、A−Ti−B−O系複合酸化物(元素Aはアルカリ金属、元素BはNbとTaのうちの少なくとも1種、元素Aと元素BとTiの含有量はいずれもゼロで無い)で構成される結晶相、より具体的には、K1-xTiNb1+xO5 (0≦x≦0.15)で表される結晶相を例示することができる。
2…主体金具
2a…透孔
2b…筒体
2c…座面部分
2d…ネジ山
2e…溝
3…絶縁スリーブ
4…絶縁板
5…絶縁板
6…圧電素子
6a,6b…薄板電極
6c…圧電磁器
7…特性調整用ウェイト
8…ワッシャ
9…ナット
10…ハウジング
20…超音波振動子
22…圧電素子対
23a,23b…圧電素子
24a,24b…電極板
25…前面板
26…裏打板
27…中心ボルト
28,29…円錐部
30…超音波放射面
31…盲端孔
40…切削工具
42…スピンドル
43…圧電素子
44…取り付け治具
45…砥石部
46…基材
47…放射方向
48…回転方向
100…圧電磁器
200…圧電素子
301…電極
400…超音波センサ
410…ケース本体
411…筒部
413…底部
415…鍔部
420…圧電素子
421…撚り線
423…第一端子
425…第二端子
430…ベース
433…ガラス材
435…絶縁ラベル
437…樹脂製カバー
440…音響整合材
500…アクチュエータ
520…圧電素子
531…電極層
540…上下方向
550…左右方向
Claims (17)
- 無鉛圧電磁器組成物であって、
圧電特性を有するニオブ/タンタル酸アルカリ系ペロブスカイト酸化物からなる第1結晶相で形成された主相と、
M−Ti−O系スピネル化合物(元素Mは1〜4価の元素)からなる第2結晶相を含む副相と、
を含むことを特徴とする無鉛圧電磁器組成物。 - 請求項1に記載の無鉛圧電磁器組成物であって、
前記元素Mは、Li,Mg,Al,Sc,Cr,Mn,Fe,Co,Ni,Zn,Ga,Y,Zrのうちの少なくとも1種の金属元素を含むことを特徴とする無鉛圧電磁器組成物。 - 請求項1又は2に記載の無鉛圧電磁器組成物であって、
前記M−Ti−O系スピネル化合物は、組成式MxTiOy(係数x,yはTiの含有量を1としたときの相対値)で表され、
前記係数xが、0.5≦x≦5.0を満たすことを特徴とする無鉛圧電磁器組成物。 - 請求項3に記載の無鉛圧電磁器組成物であって、
前記係数yが2≦y≦8を満たすことを特徴とする無鉛圧電磁器組成物。 - 請求項1〜4のいずれか一項に記載の無鉛圧電磁器組成物であって、
前記副相は、前記主相の間に形成される空孔を充填するものであることを特徴とする無鉛圧電磁器組成物。 - 請求項1〜5のいずれか一項に記載の無鉛圧電磁器組成物であって、
前記無鉛圧電磁器組成物における前記第2結晶相の含有割合は、0.5体積%以上で5.0体積%以下であることを特徴とする無鉛圧電磁器組成物。 - 請求項1〜6のいずれか一項に記載の無鉛圧電磁器組成物であって、
前記M−Ti−O系スピネル化合物は、前記元素Mとして2種類以上の金属元素を含む、ことを特徴とする無鉛圧電磁器組成物。 - 請求項1〜7のいずれか一項に記載の無鉛圧電磁器組成物であって、
前記副相は、前記第2結晶相の他に、A3B5O15系化合物(元素Aは1〜2価の金属、元素Bは2〜5価の金属)からなる第3結晶相を含む、ことを特徴とする無鉛圧電磁器組成物。 - 請求項1〜8のいずれか一項に記載の無鉛圧電磁器組成物であって、
前記副相の全体を100%としたときの前記第2結晶相の体積割合が50%以上である、ことを特徴とする無鉛圧電磁器組成物。 - 請求項1〜9のいずれか一項に記載の無鉛圧電磁器組成物であって、
前記第1結晶相を形成するニオブ/タンタル酸アルカリ系ペロブスカイト酸化物は、アルカリ土類金属を含むことを特徴とする無鉛圧電磁器組成物。 - 請求項10に記載の無鉛圧電磁器組成物であって、
前記第1結晶相を形成するニオブ/タンタル酸アルカリ系ペロブスカイト酸化物は、組成式(KaNabLicCd)e(DfEg)Oh (元素CはCa,Sr,Baの一種以上、元素DはNb,Ta,Ti,Zr,Hf,Sn,Sb,Siのうちの少なくともNb又はTaを含む一種以上、元素EはMg,Al,Sc,Mn,Fe,Co,Ni,Zn,Ga,Yの一種以上、a+b+c+d=1、a+b+cはゼロでなく、eは0.80≦e≦1.10を満たし、f+g=1、hはペロブスカイトを構成する任意の値)で表されることを特徴とする無鉛圧電磁器組成物。 - 請求項11に記載の無鉛圧電磁器組成物であって、
前記係数eが、0.88≦e≦1.07を満たすことを特徴とする無鉛圧電磁器組成物。 - 請求項1〜12のいずれか一項に記載の無鉛圧電磁器組成物であって、
前記ニオブ/タンタル酸アルカリ系ペロブスカイト酸化物は、ニオブ酸アルカリ系ペロブスカイト酸化物であることを特徴とする無鉛圧電磁器組成物。 - 請求項1〜13のいずれか一項に記載の無鉛圧電磁器組成物で形成された圧電磁器と、
前記圧電磁器に取り付けられた電極と、
を備えることを特徴とする圧電素子。 - 請求項14に記載の圧電素子を備えることを特徴とする装置。
- 請求項15に記載の装置であって、
前記装置は、ノックセンサと、超音波振動子と、切削工具と、超音波センサと、アクチュエータと、のうちのいずれかであることを特徴とする装置。 - 請求項1〜13のいずれか一項に記載の無鉛圧電磁器組成物の製造方法であって、
前記第1結晶相の原料を混合し、仮焼して第1の粉末を作成する工程と、
前記第2結晶相の原料を混合し、仮焼して第2の粉末を作成する工程と、
前記第1と第2の粉末を混合し、成形し、焼成することによって、前記無鉛圧電磁器組成物を生成する工程と、
を備え、
前記焼成は、密閉容器内に成形体を封入して焼成を行う密閉焼成であることを特徴とする無鉛圧電磁器組成物の製造方法。
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