WO2020207139A1 - Kdp类晶体长籽晶单锥生长方法 - Google Patents

Kdp类晶体长籽晶单锥生长方法 Download PDF

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WO2020207139A1
WO2020207139A1 PCT/CN2020/076923 CN2020076923W WO2020207139A1 WO 2020207139 A1 WO2020207139 A1 WO 2020207139A1 CN 2020076923 W CN2020076923 W CN 2020076923W WO 2020207139 A1 WO2020207139 A1 WO 2020207139A1
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crystal
growth
long seed
kdp
seed crystal
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PCT/CN2020/076923
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English (en)
French (fr)
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王斌
齐红基
邵建达
陈端阳
王虎
王晓亮
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中国科学院上海光学精密机械研究所
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Priority to RU2021109312A priority Critical patent/RU2759189C1/ru
Priority to JP2021518919A priority patent/JP7208371B2/ja
Publication of WO2020207139A1 publication Critical patent/WO2020207139A1/zh
Priority to US17/159,106 priority patent/US11486053B2/en

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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
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/08—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by cooling of the solution
    • 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
    • C30B29/14—Phosphates
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/35—Non-linear optics
    • G02F1/353—Frequency conversion, i.e. wherein a light beam is generated with frequency components different from those of the incident light beams
    • G02F1/354—Third or higher harmonic generation
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/35—Non-linear optics
    • G02F1/355—Non-linear optics characterised by the materials used
    • G02F1/3551—Crystals
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/35—Non-linear optics
    • G02F1/37—Non-linear optics for second-harmonic generation

Definitions

  • the invention relates to KDP crystals, in particular to a KDP crystal long seed crystal single-cone growth method, and aims to rapidly grow KDP crystals with high cutting efficiency and low growth stress.
  • KDP/DKDP crystal materials are widely used in the manufacture of frequency doubling and electro-optical devices due to their large nonlinear optical coefficient, wide transmission band, and excellent optical uniformity.
  • Laser inertial confinement nuclear fusion (ICF) devices in various countries require a large number of high-quality, large-aperture KDP crystals; among them, KDP crystals are used as optical switches and double frequency components, and DKDP crystals are used as triple frequency components.
  • the KDP crystals grown by the prior art mainly have defects such as poor crystal quality and low aspect ratio, and further cause the KDP crystals to have a low slicing rate, prone to have a cylindrical cone interface, and the crystal cylindrical cone interface part
  • the poor quality is a shortcoming that restricts the overall quality of the crystal.
  • the invention patent with application number CN201210102338.9 and application publication number CN103361712A introduces a crystal carrier and growth method for the growth of large cross-section KDP crystals.
  • the upper and lower horizontal plates are both plate-like structures, which greatly disturb the growth solution during the rotation of the crystal growth and cause the crystal quality to decrease; this invention fixes the seed crystal on the lower surface or under the upper horizontal plate The center of the surface of the horizontal plate, but only rotating during crystal growth without stirring effect will cause uneven crystal growth; and when the crystal grows to contact another horizontal plate, collision and contact between the crystal and the horizontal plate will occur , Causing miscellaneous crystal growth.
  • the invention patent with application number CN201710987729.6 and application publication number CN107805844A introduces a method for restricting the growth of KDP-type crystals by growing seeds. This invention will resist the growth of the seed crystals during the growth process, and the growth stress will be greater. The growth is difficult, and the height of the seed crystal needs to be large, which increases the growth pressure.
  • the present invention provides a KDP crystal long seed crystal single cone growth method.
  • This method is conducive to the rapid growth of KDP-like crystals under low growth stress; during the growth process, except for the upper end of the free cone growth, all growth surfaces are cylindrical and the growth environment of each surface is highly similar, which has higher optics Uniformity; and the KDP crystal element that does not contain the cylindrical cone interface can be cut from the cylindrical surface; the KDP crystal obtained by the method provided by the present invention also has high cutting efficiency when cutting the frequency-doubling element.
  • a method for growing a single cone of KDP-type crystal long seed crystals includes the following steps:
  • the crystal carrier includes an upper beam, a lower tray, a connecting rod, a supporting side rod and two blade-shaped stirring paddles, and the connecting rod is fixed in the center of the upper beam,
  • the lower ends of the supporting side rods are fixed to the two ends of the same diameter of the lower tray, the upper ends of the supporting side rods are fixed to the two ends of the upper beam, and the blade-shaped stirring paddle is a blade-like structure fixed on the supporting side rods
  • the two blade-shaped stirring paddles, the supporting side rods and the upper beam are on the same vertical plane, the upper surface of the lower tray is in the middle of the fixed position of the long seed crystal, and all the connections are smoothly connected to ensure smooth;
  • the height of the long seed crystal is smaller than the height of the support side bar of the crystal carrier, and the horizontal length and width of the long seed crystal range from 5 to 15mm;
  • the KDP-type crystal is KDP crystal or DKDP crystal.
  • the upper beam is a slat with smooth edges
  • the connecting rod is a hollow round rod
  • the lower tray is a circular plate.
  • the fixing method is welding.
  • the lower end of the long seed crystal is restricted by the lower tray, and the upper end is free to grow into a cone.
  • four cylinders in the two directions of [100] and [010] can grow ,
  • There is no growth stress problem in the crystal growth process and all cut optical components have high optical quality.
  • the growth process is the simultaneous growth of four cylinders with highly similar growth environments, and the blade-shaped stirring paddle is used for stirring during the crystal growth process, the cut optical elements all have high optical uniformity.
  • the crystal grown by the present invention Due to the uniqueness of the cutting angle of the KDP-type crystal triple frequency element, the crystal grown by the present invention has a very high cutting efficiency when cutting the frequency triple element, and the horizontal size of the grown crystal can also be known in advance. The area of the largest triple frequency component that comes out.
  • FIG. 1 is a schematic diagram of the assembly of the growth groove and the crystal carrier used in the single cone growth method of the KDP-type crystal long seed crystal of the present invention
  • FIG. 2 is a schematic diagram of the crystal carrier used in the KDP-type crystal long seed crystal single cone growth method of the present invention
  • FIG. 3 is a schematic diagram of the assembly of the leaf-shaped stirring paddle and the supporting side rod used in the KDP-like crystal long seed crystal single-cone growth method of the present invention, and its front, right, left and top views;
  • FIG. 4 is a schematic diagram of cutting multiple pieces of frequency-doubling element of KDP-type crystals grown by the KDP-type crystal growing seed crystal single cone growth method of the present invention
  • Example 1 Single cone growth of KDP crystal long seed crystal
  • the single cone growth of the KDP crystal long seed crystal includes the following steps:
  • the upper part of the growth tank 1 is equipped with a motor 5, and the lower end of the rotating shaft 4 of the motor 5 is connected to the connecting rod 6 of the crystal carrier 3;
  • the crystal carrier 3 includes an upper beam 7, a lower tray 12, a connecting rod 6, a supporting side rod 8, 9 and two blade-shaped stirring paddles 10, 11.
  • the upper beam 7 is a slat with smooth edges and corners
  • the connecting rod 6 is a hollow round rod fixed in the middle of the upper beam 7
  • the lower tray 12 is a circular plate
  • the supporting side rods 8, 9 The lower end is welded to the two ends of the same diameter of the lower tray 12, the upper ends of the supporting side rods 8, 9 are welded to both ends of the upper beam 7, and the blade-shaped stirring paddles 10, 11 are welded to the supporting side rods 8, 9
  • the two blade-shaped stirring paddles 10, 11, the supporting side rods 8, 9 and the upper beam 7 are on the same vertical plane, and the upper surface of the lower tray 12 is in the center of the seed crystal The fixed position, all connections are smoothly connected to ensure smoothness;
  • the height of the KDP long seed crystal 13 is smaller than the height of the supporting side bars 8, 9 of the crystal carrier 3, and the KDP long seed crystal 13
  • the horizontal length and width are 5mm;
  • the rotation mode adopts the cycle of 25s forward rotation-deceleration 2s-stop 1s-reverse acceleration 2s-reverse rotation 25s-deceleration 2s-stop 1s-forward acceleration 2s. s is seconds;
  • the matching angle of the KDP crystal 14 is 60°, and the azimuth angle is 0° or 90°, so after the grown KDP crystal 14 is divided into two, each part can follow the [100 ] Direction and at an angle of 30° to the [001] direction to cut out approximately square frequency triplet elements 15 with high cutting efficiency; moreover, the size of these approximately square frequency tripled elements 15 is exactly equal to the length The size of the horizontal section of the KDP crystal 14 formed.
  • Example 2 Single cone growth of DKDP crystal long seed crystal with 30% deuteration rate
  • the single-cone growth of the long seed crystal of DKDP crystal with 30% deuteration rate includes the following steps:
  • the upper part of the growth tank 1 is equipped with a motor 5, and the lower end of the rotating shaft 4 of the motor 5 is connected to the connecting rod 6 of the crystal carrier 3;
  • the crystal carrier 3 includes an upper beam 7, a lower tray 12, a connecting rod 6, a supporting side rod 8, 9 and two blade-shaped stirring paddles 10, 11.
  • the upper beam 7 is a slat with smooth edges and corners
  • the connecting rod 6 is a hollow round rod fixed in the middle of the upper beam 7
  • the lower tray 12 is a circular plate
  • the supporting side rods 8, 9 The lower end is welded to the two ends of the same diameter of the lower tray 12, the upper ends of the supporting side rods 8, 9 are welded to both ends of the upper beam 7, and the blade-shaped stirring paddles 10, 11 are welded to the supporting side rods 8, 9
  • the two blade-shaped stirring paddles 10, 11, the supporting side rods 8, 9 and the upper beam 7 are on the same vertical plane, and the upper surface of the lower tray 12 is in the center of the seed crystal The fixed position, all connections are smoothly connected to ensure smoothness;
  • the height of the DKDP long seed crystal 13 is smaller than the height of the supporting side bars 8, 9 of the crystal carrier 3, and the DKDP long seed crystal
  • the horizontal length and width of 13 are 10mm;
  • the rotation mode adopts the cycle of 25s forward rotation-deceleration 2s-stop 1s-reverse acceleration 2s-reverse rotation 25s-deceleration 2s-stop 1s-forward acceleration 2s, where s is seconds;
  • the matching angle of the DKDP crystal 14 is 59°5', and the azimuth angle is 0° or 90°, so after the grown DKDP crystal 14 is divided into two, each part can follow The [100] direction and the angle of 30°5' with the [001] direction just cut out the approximately square frequency triple element 15 with high cutting efficiency; moreover, the size of the approximately square frequency triple element 15 cut out It is exactly equal to the size of the horizontal section of the grown DKDP crystal 14.
  • Example 3 Single cone growth of DKDP crystal long seed crystal with 70% deuteration rate
  • the single-cone growth of DKDP crystal long seed crystal with 70% deuteration rate includes the following steps:
  • the upper part of the growth tank 1 is equipped with a motor 5, and the lower end of the rotating shaft 4 of the motor 5 is connected to the connecting rod 6 of the crystal carrier 3;
  • the crystal carrier 3 includes an upper beam 7, a lower tray 12, a connecting rod 6, a supporting side rod 8, 9 and two blade-shaped stirring paddles 10, 11.
  • the upper beam 7 is a slat with smooth edges and corners
  • the connecting rod 6 is a hollow round rod fixed in the middle of the upper beam 7
  • the lower tray 12 is a circular plate
  • the supporting side rods 8, 9 The lower end is welded to the two ends of the same diameter of the lower tray 12, the upper ends of the supporting side rods 8, 9 are welded to both ends of the upper beam 7, and the blade-shaped stirring paddles 10, 11 are welded to the supporting side rods 8, 9
  • the two blade-shaped stirring paddles 10, 11, the supporting side rods 8, 9 and the upper beam 7 are on the same vertical plane, and the upper surface of the lower tray 12 is in the center of the seed crystal The fixed position, all connections are smoothly connected to ensure smoothness;
  • the height of the DKDP long seed crystal 13 is smaller than the height of the supporting side bars 8, 9 of the crystal carrier 3, and the DKDP long seed crystal
  • the horizontal length and width of 13 are 15mm;
  • the rotation mode adopts the cycle of 25s forward rotation-deceleration 2s-stop 1s-reverse acceleration 2s-reverse rotation 25s-deceleration 2s-stop 1s-forward acceleration 2s. s is seconds;
  • the matching angle of the DKDP crystal 14 is 59°4', and the azimuth angle is 0° or 90°, so after the grown DKDP crystal 14 is divided into two, each part can follow The [100] direction and the [001] direction at an angle of 30°6' just cut out the approximately square frequency triple element 15 with high cutting efficiency; moreover, the size of the approximately square frequency triple element 15 cut out It is exactly equal to the size of the horizontal section of the grown DKDP crystal 14.

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Abstract

一种KDP类晶体长籽晶单锥生长方法，本发明提供的生长方法中，长籽晶下端受到下托盘的限制，上端自由成锥生长，同时[100]和[010]两个方向的四个柱面能够生长，晶体生长过程中不存在生长应力问题，所有切割出来的光学元件都具有很高的光学质量。由于生长过程是四个生长环境高度相似的柱面同时生长，且在晶体生长过程中通过叶状搅拌桨进行搅拌，所以切割出来的光学元件都具有很高的光学均匀性。由于KDP类晶体三倍频元件切割角度的独特性，用本发明长成的晶体切割三倍频元件时具有很高的切割效率，而且还可以通过长成的晶体水平尺寸的大小提前知晓能够切割出来的最大的三倍频元件的面积。

Description

KDP类晶体长籽晶单锥生长方法 技术领域
本发明涉及KDP类晶体，具体涉及KDP类晶体长籽晶单锥生长方法，旨在快速生长出切割效率高、生长应力小的KDP类晶体。
背景技术
磷酸二氢钾/磷酸二氘钾(KDP/DKDP)晶体材料以其较大的非线性光学系数、较宽的透过波段、光学均匀性优良等优点被广泛应用于制作倍频及电光器件。各国的激光惯性约束核聚变(ICF)装置都需要大量高质量、大口径的KDP类晶体；其中，KDP类晶体用作光开关和二倍频元件，DKDP晶体用作三倍频元件。但通过现有技术生长的KDP类晶体主要存在晶体质量较差、纵横比低等缺陷，且进一步造成KDP类晶体的切片率低，容易带有柱锥交界面，而且晶体柱锥交界面部分的质量较差，是制约晶体整体质量的短板。申请号CN201210102338.9、申请公布号CN103361712A的发明专利介绍了一种用于大截面KDP类晶体生长的载晶架及生长方法。该发明提供的载晶架中，上、下横板均为板式结构，在晶体生长旋转过程中对生长溶液扰动大，造成晶体质量下降；该发明将籽晶固定在上横板下表面或下横板上表面的中央，但在晶体生长中仅加以旋转，而无搅拌效果，会造成晶体生长不均匀；并且当晶体生长至接触到另一横板时，会发生晶体和横板的碰撞接触，造成杂晶生长。申请号CN201710987729.6、申请公开号CN107805844A的发明专利介绍了一种KDP类晶体长籽晶限制生长方法，该发明在生长过程中由于籽晶生长的上下都顶住，其生长应力会较大，造成生长困难，且需要提供的籽晶高度要大，增大了生长压力。
发明内容
为克服现有KDP类晶体生长存在的上述问题，本发明提供一种KDP类晶体长籽晶单锥生长方法。该方法有利于在低生长应力下，快速生长出KDP类晶体；生长过程中除自由成锥生长的上端外，所有生长面均为柱面且各个面的生长环境高度相似，具有更高的光学均匀性；且从柱面可切割出不包含柱锥交界面的KDP类晶体元件；利用本发明提供的方法得到的KDP类晶体切割三倍频元件时还具有很高的切割效率。
本发明的技术解决方案如下：
一种KDP类晶体长籽晶单锥生长方法，包括以下步骤：
1)制作晶体生长所用的生长槽，所述的生长槽上部安装电机，该电机的转轴下端连接载晶架的连接杆；
2)制作晶体生长所用的载晶架：所述的载晶架包括上横梁、下托盘、连接杆、支撑侧杆以及两个叶状搅拌桨，所述的连接杆固定在上横梁正中央，所述的支撑侧杆下端固定在下托盘同一直径的两端，所述的支撑侧杆上端固定在上横梁的两端，所述的叶状搅拌桨为固定在支撑侧杆上的叶片状结构，所述的两个叶状搅拌桨和支撑侧杆以及上横梁在同一竖直平面上，所述的下托盘的上表面的正中央为长籽晶的固定位置，所有连接处均平滑相连以保证光滑；
3)制作高度方向是[001]向的长籽晶：所述的长籽晶高度小于所述的载晶架的支撑侧杆高度，所述的长籽晶的水平长度和宽度范围为5～15mm；
4)将所述的长籽晶下端面点上AB胶，安装在所述的载晶架下托盘的上表面的正中央；
5)配制饱和点在40～70℃的晶体生长溶液；
6)将安装有长籽晶的载晶架放入烘箱中预热4～12小时，预热温度为所述的生长溶液的饱和点温度；
7)预热完成后，将安装有长籽晶的载晶架放入配制好的所述的生长溶液中，将所述的载晶架的连接杆连接在所述的电机转轴上，启动电机，设定转速的范围为10～50rpm，旋转模式采用正转25s-减速2s-停止1s-反向加速2s-反转25s-减速2s-停止1s-正向加速2s的周期，其中s为秒；
8)将所述的生长溶液加热至饱和点温度之上5～15℃做过热处理，使所述的长籽晶的四个侧面全部溶解但又不至于将所述的长籽晶溶断，然后降温，使所述的生长溶液的过饱和度始终在5～15％之间，则晶体就在所述的长籽晶上开始单锥生长，继而得到KDP类晶体。
进一步地，所述的KDP类晶体为KDP晶体或DKDP晶体。
上述步骤2)中，所述的上横梁为棱角光滑的板条，所述的连接杆为空心圆杆，所述的下托盘为圆板。
上述步骤2)中，所述的固定方式为焊接。
本发明的技术效果如下：
本发明提供的KDP类晶体长籽晶单锥生长方法中，长籽晶下端受到下托盘的限制，上端自由成锥生长，同时[100]和[010]两个方向的四个柱面能够生长，晶体生长 过程中不存在生长应力问题，所有切割出来的光学元件都具有很高的光学质量。由于生长过程是四个生长环境高度相似的柱面同时生长，且在晶体生长过程中通过叶状搅拌桨进行搅拌，所以切割出来的光学元件都具有很高的光学均匀性。由于KDP类晶体三倍频元件切割角度的独特性，用本发明长成的晶体切割三倍频元件时具有很高的切割效率，而且还可以通过长成的晶体水平尺寸的大小提前知晓能够切割出来的最大的三倍频元件的面积。
附图说明
图1是本发明KDP类晶体长籽晶单锥生长方法所用生长槽和载晶架的组装示意图；
图2是本发明KDP类晶体长籽晶单锥生长方法所用载晶架的示意图；
图3是本发明KDP类晶体长籽晶单锥生长方法所用叶状搅拌桨和支撑侧杆的组装示意图及其正视、右视、左视和俯视图；
图4是用本发明KDP类晶体长籽晶单锥生长方法长成的KDP类晶体切割多片三倍频元件的示意图；
图中：1-生长槽；2-生长溶液；3-载晶架；4-转轴；5-电机；6-连接杆；7-上横梁；8-支撑侧杆；9-支撑侧杆；10-叶状搅拌桨；11-叶状搅拌桨；12-下托盘，13-长籽晶；14-KDP类晶体；15-三倍频元件。
具体实施方式
下面通过实施例结合附图对本发明作进一步的详细描述，但不能用来限制本发明的范围。
实施例1：KDP晶体长籽晶单锥生长
KDP晶体长籽晶单锥生长，包括以下步骤：
1)制作晶体生长所用的生长槽1，所述的生长槽1上部安装电机5，该电机5的转轴4下端连接载晶架3的连接杆6；
2)制作晶体生长所用的载晶架3：所述的载晶架3包括上横梁7、下托盘12、连接杆6、支撑侧杆8、9以及两个叶状搅拌桨10、11，所述的上横梁7为棱角光滑的板条，所述的连接杆6为固定在上横梁7正中间的空心圆杆，所述的下托盘12为圆板，所述的支撑侧杆8、9下端焊接在下托盘12同一直径的两端，所述的支撑侧杆8、9上端焊接在上横梁7的两端，所述的叶状搅拌桨10、11为焊接在支撑侧杆8、9上的叶片状结构，所述的两个叶状搅拌桨10、11和支撑侧杆8、9以及上横梁 7在同一竖直平面上，所述的下托盘12的上表面的正中央为籽晶的固定位置，所有连接处均平滑相连保证光滑；
3)制作高度方向是[001]的KDP长籽晶13：所述的KDP长籽晶13高度小于所述的载晶架3的支撑侧杆8、9高度，所述的KDP长籽晶13的水平长度和宽度为5mm；
4)将所述的KDP长籽晶13下端面点上AB胶，安装在所述的载晶架3的下托盘12的上表面的中心；
5)配制饱和点在40℃的KDP晶体生长溶液2；
6)将安装有KDP长籽晶13的载晶架3放入烘箱中预热7小时，预热温度为40℃；
7)预热完成后，将安装有KDP长籽晶13的载晶架3放入配制好的KDP生长溶液2中，将所述的载晶架3的连接杆6连接在所述电机5的转轴4上，启动电机5，设定转速为30rpm，旋转模式采用正转25s-减速2s-停止1s-反向加速2s-反转25s-减速2s-停止1s-正向加速2s的周期，其中s为秒；
8)将所述的KDP生长溶液2加热至50℃做过热处理，使所述的KDP长籽晶13的四个侧面全部溶解但又不至于将该KDP长籽晶13溶断，然后降温，使所述的KDP生长溶液2的过饱和度始终在15％，则KDP晶体就在所述的KDP长籽晶13上开始单锥生长，继而得到KDP晶体14。
特别是在切割三倍频元件15时，KDP晶体14的匹配角为60°，方位角为0°或90°，所以长成的KDP晶体14一分为二后每一部分都可以沿着[100]方向且与[001]方向成30°的角度正好切割出近似正方形的三倍频元件15，切割效率很高；而且，这些切出来的近似正方形的三倍频元件15的大小正好近似等于长成的KDP晶体14水平截面的大小。
实施例2：30％氘化率的DKDP晶体长籽晶单锥生长
30％氘化率的DKDP晶体长籽晶单锥生长，包括以下步骤：
1)制作晶体生长所用的生长槽1，所述的生长槽1上部安装电机5，该电机5的转轴4下端连接载晶架3的连接杆6；
2)制作晶体生长所用的载晶架3：所述的载晶架3包括上横梁7、下托盘12、连接杆6、支撑侧杆8、9以及两个叶状搅拌桨10、11，所述的上横梁7为棱角光滑的板条，所述的连接杆6为固定在上横梁7正中间的空心圆杆，所述的下托盘12为 圆板，所述的支撑侧杆8、9下端焊接在下托盘12同一直径的两端，所述的支撑侧杆8、9上端焊接在上横梁7的两端，所述的叶状搅拌桨10、11为焊接在支撑侧杆8、9上的叶片状结构，所述的两个叶状搅拌桨10、11和支撑侧杆8、9以及上横梁7在同一竖直平面上，所述的下托盘12的上表面的正中央为籽晶的固定位置，所有连接处均平滑相连保证光滑；
3)制作高度方向是[001]向的DKDP长籽晶13：所述的DKDP长籽晶13高度小于所述的载晶架3的支撑侧杆8、9高度，所述的DKDP长籽晶13的水平长度和宽度为10mm；
4)将所述的DKDP长籽晶13下端面点上AB胶，安装在所述的载晶架3的下托盘12的上表面的中心；
5)配制饱和点在55℃的DKDP晶体生长溶液2；
6)将安装有DKDP长籽晶13的载晶架3放入烘箱中预热4小时，预热温度为55℃；
7)预热完成后，将安装有DKDP长籽晶13的载晶架3放入配制好的DKDP生长溶液2中，将所述的载晶架3的连接杆6连接在所述电机5的转轴4上，启动电机5，设定转速为10rpm，旋转模式采用正转25s-减速2s-停止1s-反向加速2s-反转25s-减速2s-停止1s-正向加速2s的周期，其中s为秒；
8)将所述的DKDP生长溶液2加热至60℃做过热处理，使所述的DKDP长籽晶13的四个侧面全部溶解但又不至于将该DKDP长籽晶13溶断，然后降温，使所述的DKDP生长溶液2的过饱和度始终在5％，则DKDP晶体就在所述的DKDP长籽晶13上开始单锥生长，继而得到DKDP晶体14。
特别是在切割三倍频元件15时，DKDP晶体14的匹配角为59°5′，方位角为0°或90°，所以长成的DKDP晶体14一分为二后每一部分都可以沿着[100]方向且与[001]方向成30°5′的角度正好切割出近似正方形的三倍频元件15，切割效率很高；而且，这些切出来的近似正方形的三倍频元件15的大小正好近似等于长成的DKDP晶体14水平截面的大小。
实施例3：70％氘化率的DKDP晶体长籽晶单锥生长
70％氘化率的DKDP晶体长籽晶单锥生长，包括以下步骤：
1)制作晶体生长所用的生长槽1，所述的生长槽1上部安装电机5，该电机5的转轴4下端连接载晶架3的连接杆6；
2)制作晶体生长所用的载晶架3：所述的载晶架3包括上横梁7、下托盘12、连接杆6、支撑侧杆8、9以及两个叶状搅拌桨10、11，所述的上横梁7为棱角光滑的板条，所述的连接杆6为固定在上横梁7正中间的空心圆杆，所述的下托盘12为圆板，所述的支撑侧杆8、9下端焊接在下托盘12同一直径的两端，所述的支撑侧杆8、9上端焊接在上横梁7的两端，所述的叶状搅拌桨10、11为焊接在支撑侧杆8、9上的叶片状结构，所述的两个叶状搅拌桨10、11和支撑侧杆8、9以及上横梁7在同一竖直平面上，所述的下托盘12的上表面的正中央为籽晶的固定位置，所有连接处均平滑相连保证光滑；
3)制作高度方向是[001]向的DKDP长籽晶13：所述的DKDP长籽晶13高度小于所述的载晶架3的支撑侧杆8、9高度，所述的DKDP长籽晶13的水平长度和宽度为15mm；
4)将所述的DKDP长籽晶13下端面点上AB胶，安装在所述的载晶架3的下托盘12的上表面的中心；
5)配制饱和点在70℃的DKDP晶体生长溶液2；
6)将安装有DKDP长籽晶13的载晶架3放入烘箱中预热12小时，预热温度为70℃；
7)预热完成后，将安装有DKDP长籽晶13的载晶架3放入配制好的DKDP生长溶液2中，将所述的载晶架3的连接杆6连接在所述电机5的转轴4上，启动电机5，设定转速为50rpm，旋转模式采用正转25s-减速2s-停止1s-反向加速2s-反转25s-减速2s-停止1s-正向加速2s的周期，其中s为秒；
8)将所述的DKDP生长溶液2加热至85℃做过热处理，使所述的DKDP长籽晶13的四个侧面全部溶解但又不至于将该DKDP长籽晶13溶断，然后降温，使所述的DKDP生长溶液2的过饱和度始终在10％，则DKDP晶体就在所述的DKDP长籽晶13上开始单锥生长，继而得到DKDP晶体14。
特别是在切割三倍频元件15时，DKDP晶体14的匹配角为59°4′，方位角为0°或90°，所以长成的DKDP晶体14一分为二后每一部分都可以沿着[100]方向且与[001]方向成30°6′的角度正好切割出近似正方形的三倍频元件15，切割效率很高；而且，这些切出来的近似正方形的三倍频元件15的大小正好近似等于长成的DKDP晶体14水平截面的大小。

Claims (4)

  1. 一种KDP类晶体长籽晶单锥生长方法，其特征在于，包括以下步骤：
    1)制作晶体生长所用的生长槽，所述的生长槽上部安装电机，该电机的转轴下端连接载晶架的连接杆；
    2)制作晶体生长所用的载晶架：所述的载晶架包括上横梁、下托盘、连接杆、支撑侧杆以及两个叶状搅拌桨，所述的连接杆固定在上横梁正中央，，所述的支撑侧杆下端固定在下托盘同一直径的两端，所述的支撑侧杆上端固定在上横梁的两端，所述的叶状搅拌桨为固定在支撑侧杆上的叶片状结构，所述的两个叶状搅拌桨和支撑侧杆以及上横梁在同一竖直平面上，所述的下托盘的上表面的正中央为长籽晶的固定位置，所有连接处均平滑相连以保证光滑；
    3)制作高度方向是[001]向的长籽晶：所述的长籽晶高度小于所述的载晶架的支撑侧杆高度，所述的长籽晶的水平长度和宽度范围为5～15mm；
    4)将所述的长籽晶下端面点上AB胶，安装在所述的载晶架下托盘的上表面的正中央；
    5)配制饱和点在40～70℃的晶体生长溶液；
    6)将安装有长籽晶的载晶架放入烘箱中预热4～12小时，预热温度为所述的生长溶液的饱和点温度；
    7)预热完成后，将安装有长籽晶的载晶架放入配制好的所述的生长溶液中，将所述的载晶架的连接杆连接在所述的电机转轴上，启动电机，设定转速的范围为10～50rpm，旋转模式采用正转25s-减速2s-停止1s-反向加速2s-反转25s-减速2s-停止1s-正向加速2s的周期，其中s为秒；
    8)将所述的生长溶液加热至饱和点温度之上5～15℃做过热处理，使所述的长籽晶的四个侧面全部溶解但又不至于将所述的长籽晶溶断，然后降温，使所述的生长溶液的过饱和度始终在5～15％之间，则晶体就在所述的长籽晶上开始单锥生长，继而得到KDP类晶体。
  2. 如权利要求1所述的生长方法，其特征在于，步骤2)中，所述的上横梁为棱角光滑的板条，所述的连接杆为空心圆杆，所述的下托盘为圆板。
  3. 如权利要求1所述的生长方法，其特征在于，步骤2)中，所述的固定方式为焊接。
  4. 如权利要求1所述的生长方法，其特征在于，所述的KDP类晶体为KDP晶体或DKDP晶体。
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