KR920006204B1 - Linbo3 single crystal growing method - Google Patents
Linbo3 single crystal growing method Download PDFInfo
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- KR920006204B1 KR920006204B1 KR1019880011227A KR880011227A KR920006204B1 KR 920006204 B1 KR920006204 B1 KR 920006204B1 KR 1019880011227 A KR1019880011227 A KR 1019880011227A KR 880011227 A KR880011227 A KR 880011227A KR 920006204 B1 KR920006204 B1 KR 920006204B1
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/36—Single-crystal growth by pulling from a melt, e.g. Czochralski method characterised by the seed, e.g. its crystallographic orientation
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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
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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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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Abstract
Description
제1도는 Y축 방향으로 성장시킨 LiNbO3단결정을 도시한 것으로서, (a)는 단결정의 측면도이고, (b)는 횡단면도이다.FIG. 1 shows LiNbO 3 single crystals grown in the Y-axis direction, where (a) is a side view of the single crystal and (b) is a cross sectional view.
제2도는 LiNbO3단결정의 축방향별 온도에 대한 열팽창률을 도시한 그래프.2 is a graph showing the coefficient of thermal expansion with respect to axial temperature of LiNbO 3 single crystal.
제3도는 종래 단결정 성장시 120℃/h의 냉각 속도로 냉각시킨 Y축 방향 LiNbO3단결정의 모양.3 is the shape of the Y-axis direction LiNbO 3 single crystal cooled at a cooling rate of 120 ℃ / h during the conventional single crystal growth.
제4도는 본 발명에 의해 냉각시킨 Y축방향 LiNbO3단결정의 모양.4 is a shape of a Y-axis direction LiNbO 3 single crystal cooled by the present invention.
본 발명은 Y축으로 성장시킨 LiNbO3단결정의 경우 균열(Crack)이 없는 양질의 단결정을 얻기 위하여, 냉각의 Z축과 X측의 열팽창 계수가 온도에 따라 상이하게 변하는것에 착안하여 냉각조건을 설정함으로서 균열이 없는 결정을 성장시키는 방법인 것이다.In the present invention, in order to obtain a high quality single crystal without crack in the case of LiNbO 3 single crystal grown on the Y axis, the cooling conditions are set in consideration of the fact that the thermal expansion coefficients on the Z axis and the X side of the cooling vary with temperature. It is a method of growing a crystal free of cracks.
단결정 성장방법에는 여러 방법이 있는데 그중 대량 생산이 가능하며 대형, 양질의 단결정을 얻을 수 있는 방법이 쵸크랄스키(Czo-chralski)방법이다. Czochralski방법은 도가니에 원료분말을 넣고, 온도를 가하여 원료분말을 녹인후 용응액에 종자결정을 담가 서서히 종자결정을 회전시킴과 동시에 인상시키면 종자결정에서 부터 결정이 성장하여 대형의 결정을 얻을 수 있는 방법이다.There are several methods for growing single crystals, among which mass production is possible, and the Czo-chralski method is a method for obtaining large size and high quality single crystals. Czochralski method adds raw powder to the crucible, melts the raw powder by applying temperature, soaks the seed crystal in the solution, rotates the seed crystal gradually, and raises it. Way.
이때 로내의 온도기울기, 용응액의 온도, 결정회전속도, 인상속도, 냉각속도, 원료분말의 순도등에 의하여 결정의 크기와 질이 좌우되며, 또 같은 종류의 결정을 성장시킨다 할지라도 성장시키는 축방향에 따라서 성장조전이 바꿔지는 특성이 있다.At this time, the size and quality of the crystal are determined by the temperature gradient in the furnace, the temperature of the solution, the crystal rotation speed, the pulling speed, the cooling speed, and the purity of the raw powder. Depending on the characteristics of growth growth.
LiNbO97결정의 성장은 단결정의 사용용도에 따라서 Y축, Z축, 128°Y축등 여러방향으로 성장시키는데, 그중에서도 Y축으로 성장된 LiNbO3단결정은 큰 전기기계 결합계수를 지니며, 음향파 전달시 손실이 매우 적은 표면탄성파(Surface Accustic Wave) 필터용으로 사용된다.The growth of LiNbO9 7 crystal grows in various directions such as Y-axis, Z-axis, and 128 ° Y-axis depending on the usage of single crystal. Among them, LiNbO 3 single crystal grown in Y-axis has a large electromechanical coupling coefficient and transmits acoustic waves It is used for Surface Accustic Wave filter with very low loss.
이러한 단결정을 얻기 위한 종래의 방법으로서는 Y축방향으로 결정을 성장 시킨후 냉각시킬때 보통 1250℃ 상온까지 100℃∼150℃/h의 냉각속도로 냉각을 시키는데, 이러한 조건으로 결정을 냉각시킬 경우, 결정의 내부에서 발생하는 급격한 온도변화에 기인하는 내부응력(Stress)이 발생되어 결정에 균열(Crack)이 발생하며, 또한 상기조건으로 냉각된 결정은 균열이 없어도 가공시 균열이 쉽게 발생하는 문제점이 실험에 의해서 나타났다.As a conventional method for obtaining such a single crystal, the crystal is grown in the Y-axis direction and then cooled at a cooling rate of 100 ° C. to 150 ° C./h up to 1250 ° C. at room temperature. When the crystal is cooled under such conditions, The internal stress (Stress) caused by the rapid temperature change inside the crystal is generated, causing cracks in the crystal, and the crystal cooled under the above conditions is easy to crack during processing without cracks. It is shown by the experiment.
본 발명의 목적은 Y축 방향으로 LiNbO3결정을 성장시킨후 냉각할때 균열(Crack)이 없는 단결정을 얻기 위하여 800℃∼400℃의 냉각구간에서 50℃∼80℃/h의 냉각속도로 결정을 냉각하는 것이다. 상기의 목적을 달성하는 본 발명은 Czochralski방법을 사용하여 Y축 방형으로 LiNbO3단결정을 성장시키는 경우 냉각조건을 설정하는 것으로 도면 제2도에 의한 바와같이 결정의 Z축과 X축의 열팽창 계수가 온도에 따라 크게 변하며, 그 변화하는 특성이 상이하여 균열(Crack)을 유발시키는 원인이 되므로 800℃∼400℃의 온도구간에서 냉각속도를 50℃∼80℃/h로 충분히 낮추어 결정내부에 발생되는 응력(Stress)을 감소시켜 균열이 없으며, 가공시에도 균열이 없는 양질의단결정을 얻게 하는 것으로, 좀더 상세히 설명하면 다음과 같다.An object of the present invention is to grow the LiNbO 3 crystals in the Y-axis direction and to determine a single crystal free of cracks during cooling, determined at a cooling rate of 50 ℃ to 80 ℃ / h in the cooling section of 800 ℃ ~ 400 ℃ To cool. The present invention which achieves the above object is to set the cooling conditions when growing LiNbO 3 single crystal in the Y-axis square by using the Czochralski method, the thermal expansion coefficient of the Z-axis and X-axis of the crystal as shown in FIG. It varies greatly depending on the stress, and its changing characteristics are different, causing cracks. Therefore, the stress generated inside the crystal by sufficiently lowering the cooling rate to 50 ° C to 80 ° C / h in the temperature range of 800 ° C to 400 ° C. (Stress) to reduce the cracks, no cracks during processing to obtain a good quality single crystal, which will be described in more detail as follows.
제3도에 도시된 바와같이 냉각속도를 120℃/h로 할 경우에 X축과 Z축이 결정의 횡단면내(제1도의(b))에 서로 수직으로 위치되어 있으므로 횡단면내에서 열팽창률의 차이가 있어 냉각속도를 빨리하면, 균열이 쉽게 발생하게 된다.As shown in FIG. 3, when the cooling rate is 120 deg. C / h, the X-axis and the Z-axis are located perpendicular to each other in the cross section of the crystal ((b) of FIG. 1). The difference is that if the cooling rate is faster, the cracks are more likely to occur.
따라서, 본 발명에서는 성장된 단결정을 냉각시킬때 그 냉각속도를 800℃∼400℃온도구간에서 50℃∼80℃/h의 냉각속도로 천천히 냉각시키면 제4도와 같이 균열이 없는 양질의 단결정을 실험에 의해서 얻을 수 있었으며, 이에 대한 실시예를 설명하면, 이에 대한 실시예를 설명하면,Therefore, in the present invention, when the grown single crystal is cooled, the cooling rate is slowly cooled at a cooling rate of 50 ° C. to 80 ° C./h at a temperature range of 800 ° C. to 400 ° C. to test a high quality single crystal without cracking as shown in FIG. 4. It was obtained by, and describes an embodiment thereof, when describing the embodiment thereof,
[실시예]EXAMPLE
직경 44mm, 높이 48mm의 백금 도가니에 원료분말 180g을 넣고, 10Kw출력의 Rf제니레이터(Generator)로 가열하여 원료분말을 녹인후 Y축방향의 종자(Seed)를 담가 4∼5mm/h로 인상시켜 길이 5cm, 직경 2.2cm∼2.5cm의 Y축 LiNbO3단결정을 성장시켰다.Put 180g raw material powder into platinum crucible with 44mm diameter and 48mm height, heat it with 10f output Rf generator, melt raw material powder and soak seed in Y-axis direction to 4 ~ 5mm / h Y-axis LiNbO 3 single crystals having a length of 5 cm and a diameter of 2.2 cm to 2.5 cm were grown.
성장시킨 결정을 120℃/h로 냉각시킨 결과 제3도와 같이 균열이 심하게 발생하였으나, 800℃∼400℃의 온도구간에서 50℃∼80℃/h의 냉각속도로 냉각시키고 나머지 온도구간은 120℃/h로 냉각 하였던바, 제4도와 같이 균열이 없는 양질의 LiNbO3단결정을 얻을수 있었으며, 이를 가공할때에도 균열이 발생하지 않았다.When the grown crystals were cooled to 120 ° C / h, cracks were severely generated as shown in FIG. 3, but the cooling was performed at a cooling rate of 50 ° C to 80 ° C / h at a temperature range of 800 ° C to 400 ° C, and the remaining temperature range was 120 ° C. Cooling at / h, it was possible to obtain a high quality LiNbO 3 single crystal without cracks, as shown in Figure 4, the crack did not occur during processing.
상술한 본 발명에 의해 성장된 LiNbO3단결정을 냉각하면 균열이 없고 내부응력이 적은 양질의 결정을 얻을 수 있고, 가공시에도 균열이 발생하지 않는 장점이 있다.By cooling the LiNbO 3 single crystal grown by the present invention described above, it is possible to obtain high quality crystals without cracking and low internal stress, and there is an advantage that cracking does not occur during processing.
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| KR1019880011227A KR920006204B1 (en) | 1988-08-31 | 1988-08-31 | Linbo3 single crystal growing method |
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| KR1019880011227A KR920006204B1 (en) | 1988-08-31 | 1988-08-31 | Linbo3 single crystal growing method |
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