KR970007336B1 - Process for the preparation of single crystal for radioelectronics and piezotechnology - Google Patents

Process for the preparation of single crystal for radioelectronics and piezotechnology Download PDF

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KR970007336B1
KR970007336B1 KR1019940002789A KR19940002789A KR970007336B1 KR 970007336 B1 KR970007336 B1 KR 970007336B1 KR 1019940002789 A KR1019940002789 A KR 1019940002789A KR 19940002789 A KR19940002789 A KR 19940002789A KR 970007336 B1 KR970007336 B1 KR 970007336B1
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single crystal
sio
piezoelectric element
laser
solution
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KR1019940002789A
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Korean (ko)
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KR950024974A (en
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장영남
배인국
채수천
김문영
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한국자원연구소
강필종
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20—Controlling or regulating

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

La2O3, Ga2O3 and SiO2 of high purity(above 3N) are mixed at a molar ratio of 3:5:2 and annealing at 1,000-1,400 deg.C for 5-20 hr to give 2La2Ga5SiO14, which is heated, rotated at a speed of 20-40 rpm, growing at a speed of 0.5mm/hr-1.0mm/hr, tailing, and cooling to give a final product. La is substitutable by Nd, Ca and Sr, Ga is substitutable by In, and Si is substitutable by Ge.

Description

제1도는 본 발명의 원료분말 제조 공정도.1 is a raw material powder manufacturing process diagram of the present invention.

제2도는 인상법에 의한 단결정 제조 공정도.2 is a single-crystal manufacturing process drawing by the pulling method.

제3도는 직경 자동제어 시스템 공정도.3 is a flow chart of automatic diameter control system.

[발명의 상세한 설명]Detailed description of the invention

본 발명은 압전소자용 및 레이저 발진자용 소재의 단결정 제조법에 관한 것이다.The present invention relates to a method for producing single crystal of piezoelectric element and laser oscillator material.

본 발명의 요체는 상기한 물질류가 인공수정에 비해 결정물리학적으로 우수한 물질로서 현재 각종 전자기기 즉 SAW 필터, 공진기 오실레이터등으로 쓰이는 인공수정의 결점을 확실히 보완할 수 있으며 현재는 단결정으로 육성하여 인공수정을 부분적으로 대체할 수 있을 것이지만 나아가 PZT 등 보다도 우수한 결정 물리적 특성을 가진 물질로 개선해 나아갈 수 있을 것이다.The gist of the present invention is that the above-mentioned materials are crystal physics superior to artificial insemination, which can reliably compensate for the deficiencies of artificial insemination, which is currently used in various electronic devices such as SAW filters, resonator oscillators, etc. It will be able to partially replace artificial insemination, but it can also be improved to materials with better crystal physical properties than PZT.

본 발명의 제조방법은 제1도에서 보는 바와 같은 공정과정을 거치는 것인데 즉 우선, La2O3, Ga2O3, SiO2등의 3N 이상의 고순도 출발물질을 3 : 5 : 2의 몰비율로 평량하여, 3La2O3, 5Ga2O3, 2SiO2준비한후 화학 및 물리적 방법으로 혼합하여 이를 1000-1400℃에서 5-20시간 동안 어니어링(annealing)반응을 통해 균질한 조성의 물질인 2La3Ga5SiO14(LGS)를 합성한다.The manufacturing method of the present invention is subjected to a process as shown in FIG. 1, that is, a high purity starting material of 3N or more such as La 2 O 3 , Ga 2 O 3 , SiO 2, etc., at a molar ratio of 3: 5: 2. After weighing, prepare 3La 2 O 3 , 5Ga 2 O 3 , 2SiO 2 , mix them by chemical and physical methods, and mix them by annealing reaction at 1000-1400 ° C. for 5-20 hours. 3 Ga 5 SiO 14 (LGS) is synthesized.

상기한 물질들은 모두 결정학적으로 트리고날(trigonal) 시스템(공간군 : P321)에 속하며 치환반응에 의해 형성되는 변종들, 특히 Ge 화합물들은 결정구조가 왜곡되어 단사정계에 속하게 된다.All of the above materials are crystallographically belonging to the trigonal system (space group: P321), and the variants formed by the substitution reaction, especially Ge compounds, are distorted in the crystal structure and thus belong to the monoclinic system.

이 패밀리는 대부분 융점이 1450℃±100이며 밀도는 4.00-5.00 정도에 해당하고 대부분 상전이 형상이 없이 용융점까지 안정하다.Most of these families have melting point of 1450 ℃ ± 100, density of 4.00-5.00, and most of them are stable to melting point without phase transition shape.

이렇게 하여 제조된 순수한 물질들을 Pt-Rh 혹은 Mo 도가니에 넣어 1500±50℃에서 용융시킨다.Pure materials thus prepared are placed in a Pt-Rh or Mo crucible and melted at 1500 ± 50 ° C.

또한 이 패밀리에 속하는 화합물들은 상호간에 고용체를 이루므로 예를들면 (1-X)Ca3Ga2Ge4O14-XNd3Ga4GeO14등과 같은 화합물로도 합성이 가능하다.In addition, compounds belonging to this family form a solid solution with each other, and thus, for example, (1-X) Ca 3 Ga 2 Ge 4 O 14 -XNd 3 Ga 4 GeO 14 can be synthesized.

다음은 초크랄스키법(인상법)에 의해 단결정으로 육성시킨다.Next, it grows to a single crystal by the Czochralski method (impression method).

전기로는 RF식 방식이나 저항 발열체 모두 사용가능하며 1450℃-1550℃ 정도의 온도범위에서 용융된 용액으로부터 회전 및 인상시키면서 성장시킨다(제2도 참조).Both electric furnaces and RF heaters can be used and grow while rotating and pulling from the molten solution in the temperature range of 1450 ° C-1550 ° C (see Figure 2).

회전속도는 로의 온도 분포에 따라 20-40rpm으로 변화가 가능하며 인상속도는 0.5mm/hr-1.0mm/hr로 사용목적에 따라 변화하면 된다.Rotating speed can be changed to 20-40rpm according to the temperature distribution of the furnace and pulling speed is 0.5mm / hr-1.0mm / hr depending on the purpose of use.

종자결정을 상부 사프트에 매달고 용액과 접촉시킨후 완만한 속도로 인상시키면 단결정으로 성장시킬 수 있다.Seed crystals can be grown to single crystals by hanging them on the upper shaft, contacting with solution and pulling them at a gentle rate.

직경이 일정하도록 다이아미터 오토콘트롤 프로그램과 무게 센서를 이용하여 웨이퍼화 하기 쉽도록 원기둥 모양으로 성장시킨다(제3도 참조).Using a diameter autocontrol program and a weight sensor to keep the diameter constant, it grows in a cylindrical shape for easy wafering (see Figure 3).

이와 같이 발명된 단결정 소재는 현재 La 대신에 Nd, Sr 등의 희토류 원소로 치환이 가능하며 Si 대신에 Ge 등을 치환한 단결정 제조가 가능하므로 해당되는 각종 산업분야에서 실용화 시킬 수 있는 것이다.The single crystal material invented as described above can be replaced by rare earth elements such as Nd and Sr instead of La, and can be used in various industrial fields as it is possible to manufacture single crystals substituted with Ge instead of Si.

앞으로는 La 대신에 각종 희토류 원소로, Ga 대신에 In, Ta, Al 등의 3족 원소로의 치환이 가능할 것이다.In the future, it will be possible to substitute various rare earth elements in place of La and group III elements such as In, Ta, and Al instead of Ga.

또한 이 패밀리에 속하는 화합물들이 상호간에 고용체를 이루므로 이러한 고용체를 단결정으로 육성할 수도 있다.In addition, since the compounds belonging to this family form a solid solution with each other, it is possible to grow such a solid solution into a single crystal.

압전소자용 및 레이저 발진자용 소재물질의 단결정 제조법Method of manufacturing single crystal of piezoelectric element and laser oscillator material

Claims (3)

압전소자 및 레이저 소재로 쓰일 수 있는 LGS의 단결정 제조법에 관한 것으로서 제조방법은 La2O3, Ga2O3, SiO2등의 3N 이상의 고순도 출발물질을 3 : 5 : 2의 몰비율인 3La2O3, 5Ga2O3, 2SiO2로 각각 평량한 후 이를 혼합하여 도가니에 넣고 이를 1000-1400℃에서 5-20시간 동안 어니어링(annealing)반응을 통해 2La3Ga5SiO14의 균질하고 순수한 물질을 합성한 후 합성된 물질들을 각기 가열반응에 의해 용융된 용액으로부터 회전 및 인상시키면서 성장시키되 회전속도는 로의 온도분포에 따라 20-40rpm으로 변화가 가능하며 인상속도는 0.5mm/hr-1.0mm/hr로 사용목적에 따라 변화시키고 종자결정을 상부 사프트에 매달고 용액과 접촉시킨후 직경이 일정하도록 다이아미터 오토콘트롤 프로그램과 무게센서를 이용하여 웨이퍼화 하기 쉽도록 모양의 단결정으로 성장시킨 것을 특징으로 하는 압전소자용 및 레이저 발진자용 소재물질의 단결정 제조법.Relates to a single crystal production method of the LGS that can be used as a piezoelectric element and a laser material manufacturing method is La 2 O 3, Ga 2 O 3, SiO 2 and 3 a high purity starting material, 3N or more of: 5: the molar ratio of 2 3La 2 After weighing each with O 3 , 5Ga 2 O 3 , 2SiO 2 , mixed them, put them in a crucible, and then homogenized and pure 2La 3 Ga 5 SiO 14 by annealing at 1000-1400 ° C. for 5-20 hours. After synthesizing the materials, the synthesized materials are grown while rotating and raising the melted solution from the molten solution by heating reaction, but the rotation speed can be changed to 20-40rpm according to the temperature distribution of the furnace and the pulling speed is 0.5mm / hr-1.0mm / hr, depending on the purpose of use, seed crystals are suspended on the upper shaft, contacted with the solution, and grown into a single crystal shaped to be easily wafered using a diameter auto control program and a weight sensor so that the diameter is constant. Single crystal production method of the piezoelectric element material and the material for the laser resonator, characterized in that. 제1항에 있어서, LGS 물질은 La3Ga4SiO14와 화학적 치환이 가능한 것을 특징으로 하는 압전소자용 및 레이저 발진자용 소재물질의 단결정 제조법.The method of claim 1, wherein the LGS material is chemically substituted with La 3 Ga 4 SiO 14 . 제1항에 있어서, La 원소는 Nd 등의 희토류 원소와 Ca, Sr 원소에 의해 치환이 가능하며 Ga 원소는 In에 의해, Si 원소는 Ge에 의해 치환이 가능한 것을 특징으로 하는 압전소자용 및 레이저 발진자용 소재물질의 단결정 제조법.The piezoelectric element and laser of claim 1, wherein the La element is replaceable by a rare earth element such as Nd and Ca and Sr elements, the Ga element is replaced by In, and the Si element is replaced by Ge. Single crystal manufacturing method of oscillator material.
KR1019940002789A 1994-02-17 1994-02-17 Process for the preparation of single crystal for radioelectronics and piezotechnology KR970007336B1 (en)

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