JPS5969499A - Manufacture of pbtio3 single crystal - Google Patents

Manufacture of pbtio3 single crystal

Info

Publication number
JPS5969499A
JPS5969499A JP57176271A JP17627182A JPS5969499A JP S5969499 A JPS5969499 A JP S5969499A JP 57176271 A JP57176271 A JP 57176271A JP 17627182 A JP17627182 A JP 17627182A JP S5969499 A JPS5969499 A JP S5969499A
Authority
JP
Japan
Prior art keywords
single crystal
pbtio3
slight amount
manufacture
components
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP57176271A
Other languages
Japanese (ja)
Inventor
「峰」岸 敬一
Keiichi Minegishi
Kiyoshi Hasegawa
清 長谷川
Mikio Higuchi
幹雄 樋口
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Chichibu Cement Co Ltd
Original Assignee
Chichibu Cement Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Chichibu Cement Co Ltd filed Critical Chichibu Cement Co Ltd
Priority to JP57176271A priority Critical patent/JPS5969499A/en
Publication of JPS5969499A publication Critical patent/JPS5969499A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B9/00Single-crystal growth from melt solutions using molten solvents
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides
    • C30B29/22Complex oxides
    • C30B29/32Titanates; Germanates; Molybdates; Tungstates
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions

Abstract

PURPOSE:To form a large-sized PbTiO3 single crystal having a good quality and high electric resistance, by adding a slight amount of trivalent metallic oxides in the manufacture of a single crystal consisting essentially of PbTiO3. CONSTITUTION:PbO and TiO2 are mixed with a slight amount of >=1 components among trivalent metallic oxides in prescribed ratios, and the mixture is filled in a platinum crucible to allow to stand at about 1,100 deg.C, for about 5hr. A PbTiO3 single crystal is grown by cooling said mixture gradually at about 10 deg.C/ hr rate to about 700 deg.C. The obtained crystal is dissolved in hot nitric acid to separate from a flux. A slight amount of components are Sb2O3, Bi2O3, Ge2O3 or the like, and the quantities to be added are about 0.01-10mol%.

Description

【発明の詳細な説明】 不発明は、圧電体や焦電体材料として使用されるPbT
iOs単結晶の製造方法に関するものである。
[Detailed description of the invention] The invention is based on PbT used as a piezoelectric or pyroelectric material.
The present invention relates to a method for manufacturing an iOs single crystal.

PbTi0aはB a T i 03と同様にペロブス
カイト型構造を有する強誘電体で、キューリ一点が49
0℃と高温であるため、比較的広範囲の温度で安定に使
用できる圧電体および焦心体材料として期待されている
PbTi0a is a ferroelectric material with a perovskite structure similar to B a T i 03, and one Curie point is 49
Because it has a high temperature of 0°C, it is expected to be a piezoelectric and focused material that can be used stably over a relatively wide range of temperatures.

シタがって、 Pl)Ti03単結晶の育成に関して多
くの研究がなされているが、現在までのところ。
A lot of research has been done on the growth of Pl)Ti03 single crystals, but so far.

良質でしかも大型の単結晶が得られていないのが笑イ青
である。
Laughing Blue is a type of material for which high-quality, large-sized single crystals have not yet been obtained.

良質なPbTiOs単結晶の育成が困難な理由は、公知
のフラックス法、引上げ法、スパッタ法等で単結晶化す
る場合、 pboが高温域において蒸発して半導体化し
てしまうからである。このため抵抗値が106ΩΦcm
程度のものしか得られないため高温で高電界を印加して
分極することができないという問題点があった。
The reason why it is difficult to grow high-quality PbTiOs single crystals is that when single crystals are formed by known flux methods, pulling methods, sputtering methods, etc., pbo evaporates in a high temperature range and becomes a semiconductor. Therefore, the resistance value is 106ΩΦcm
There was a problem that polarization could not be achieved by applying a high electric field at high temperature because only a certain degree of polarization could be obtained.

そこで本発明者は種々実験の結果、PbTiOsを主成
分とする組成物の単結晶を製造するに際し、3価の金属
酸化物のうち1種以上を微量添加することによシPbO
の欠陥を補償できるという知見を得、このような組成の
ものを公知の手段により単結晶化することによシ、良質
で大型の高抵抗P b T i O3単結晶の生成に成
功したものである。
Therefore, as a result of various experiments, the present inventor found that when producing a single crystal of a composition mainly composed of PbTiOs, by adding a trace amount of one or more of trivalent metal oxides, PbTiOs
By obtaining the knowledge that defects in P b Ti O3 can be compensated for, and by single-crystallizing the composition using known means, we succeeded in producing a high-quality, large-sized, high-resistance P b Ti O3 single crystal. be.

以下不発明の実施例について説明するが、不発明はこ\
に例示した実施例のみに限定されるものではないことは
勿論である。
Examples of non-invention will be explained below, but the non-invention is as follows.
Of course, the present invention is not limited to the embodiments illustrated in .

実施例 PbOとT i (%と微祉成分を第1表に示す割合で
混合後、白金るつぼ内に充てんし、1100℃にて5時
間保持の後10℃/11rの割合で700℃まで徐冷し
PbTiO3単結晶全育成した。次に、得られた結晶は
熱硝酸による溶出処理によシフラックスから分離した。
Example After mixing PbO and T i (%) and minor components in the proportions shown in Table 1, the mixture was filled into a platinum crucible, held at 1100°C for 5 hours, and then slowly heated to 700°C at a rate of 10°C/11r. The entire cooled PbTiO3 single crystal was grown.Next, the obtained crystal was separated from the syflux by elution treatment with hot nitric acid.

第  1  責 得られた結晶は第2表に示すように最大20關程度の立
方体状のものが得られた。また、電気的測定の結果、比
抵抗は108〜109Ω・cmと高かった。
1. As shown in Table 2, the crystals obtained had a cubic shape of about 20 squares at most. Further, as a result of electrical measurement, the specific resistance was as high as 108 to 109 Ω·cm.

なお3価の金属酸化物の添加量は0.01〜10モルチ
程度が好ましい。
Note that the amount of trivalent metal oxide added is preferably about 0.01 to 10 molty.

第  2  表 以上説明したごとく、不発明によるPbTiO3単結晶
は抵抗値が高く、このため高温でかなジの高電界全印加
して分極することが可能であるから、比較的高温域で安
定に使用できる圧電体および焦電体材料として広く適用
できるものでおる。
Table 2 As explained above, the uninvented PbTiO3 single crystal has a high resistance value and can be polarized by applying a large electric field at high temperatures, so it can be used stably at relatively high temperatures. It can be widely applied as a piezoelectric and pyroelectric material.

上記の実施例ではフラックス法によp単結晶を得たが、
他の方法でもよい。
In the above example, a p single crystal was obtained by the flux method, but
Other methods may also be used.

特許出願人 秩父セメント株式会社Patent applicant: Chichibu Cement Co., Ltd.

Claims (1)

【特許請求の範囲】[Claims] P b T i 01を主成分とする組成物の単結晶を
製造するに際し、3価の金属酸化物のうち1棟以上を微
量添加すること全特徴とするPbTi0B単結晶の製造
方法。
A method for producing a PbTi0B single crystal, which is characterized in that a trace amount of one or more of trivalent metal oxides is added when producing a single crystal of a composition containing PbTi01 as a main component.
JP57176271A 1982-10-08 1982-10-08 Manufacture of pbtio3 single crystal Pending JPS5969499A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP57176271A JPS5969499A (en) 1982-10-08 1982-10-08 Manufacture of pbtio3 single crystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP57176271A JPS5969499A (en) 1982-10-08 1982-10-08 Manufacture of pbtio3 single crystal

Publications (1)

Publication Number Publication Date
JPS5969499A true JPS5969499A (en) 1984-04-19

Family

ID=16010647

Family Applications (1)

Application Number Title Priority Date Filing Date
JP57176271A Pending JPS5969499A (en) 1982-10-08 1982-10-08 Manufacture of pbtio3 single crystal

Country Status (1)

Country Link
JP (1) JPS5969499A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009021079A (en) * 2007-07-11 2009-01-29 Mitsubishi Electric Corp Induction heating device

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009021079A (en) * 2007-07-11 2009-01-29 Mitsubishi Electric Corp Induction heating device

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