WO2019223326A1 - 一种激光辅助加热生长大尺寸晶体的方法及专用设备 - Google Patents

一种激光辅助加热生长大尺寸晶体的方法及专用设备 Download PDF

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WO2019223326A1
WO2019223326A1 PCT/CN2019/000103 CN2019000103W WO2019223326A1 WO 2019223326 A1 WO2019223326 A1 WO 2019223326A1 CN 2019000103 W CN2019000103 W CN 2019000103W WO 2019223326 A1 WO2019223326 A1 WO 2019223326A1
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laser
rod
xenon lamp
heating
support rod
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PCT/CN2019/000103
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English (en)
French (fr)
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线全刚
张重远
金浩
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中国科学院金属研究所
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Priority to US16/644,460 priority Critical patent/US11306411B2/en
Publication of WO2019223326A1 publication Critical patent/WO2019223326A1/zh

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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
    • 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
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/16—Heating of the molten zone
    • C30B13/22—Heating of the molten zone by irradiation or electric discharge
    • 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
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/16—Heating of the molten zone
    • C30B13/22—Heating of the molten zone by irradiation or electric discharge
    • C30B13/24—Heating of the molten zone by irradiation or electric discharge using electromagnetic waves
    • 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
    • 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
    • C30B29/20—Aluminium 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
    • 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
    • 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
    • C30B29/28—Complex oxides with formula A3Me5O12 wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. garnets
    • 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
    • C30B29/52—Alloys

Definitions

  • the invention relates to a method for preparing a crystal material, and particularly provides a method and special equipment for growing a large-sized crystal by laser-assisted heating.
  • Optical floating zone furnace is a directional solidification furnace with suspended melting zone using light heating. It has the characteristics of no crucible, high cleanliness, high temperature gradient and fast growth rate. It is widely used for crystal growth of intermetallic materials such as oxides and TiAl. Research, especially those crystalline materials with strong melt reactions and high melting points. Currently widely used optical floating zone furnaces are heated by 2 ⁇ 4 ellipsoidal mirror focused xenon lamps. The melt is mainly maintained by surface tension and grows in the vertical direction.
  • the model produced by Japan CSC company is FZ-T-12000 -X-VP-S optical floating zone furnace, evenly distributed with 4 xenon lamps, melting point can reach 3000 °C, temperature gradient is about 200 °C, growth rate can be precisely adjusted in the range of 0 ⁇ 180mm / h, the protection atmosphere can reach Above 99.9999%, it is one of the most advanced optical floating zone furnaces in the world.
  • the heating method of this type of equipment is light heating, that is, the focal spot of the xenon light source is focused on the surface of the test rod after focusing by the ellipsoidal mirror, and then the surface of the test rod is gradually heated up by heat conduction until it melts.
  • the diameter of the test rod is ⁇ 15mm
  • the center of the test rod can be melted thoroughly and the inside and outside can be stirred uniformly.
  • the suspension melting zone remains stable and the crystal growth can be smoothly realized; when the diameter of the test rod is greater than 15mm, it is easy to cause the test rod.
  • the present invention provides a method and special application for laser-assisted heating to grow large-sized crystals.
  • the equipment through the design of the structure and function of special equipment, introduces a high-precision and controllable laser heating heat source in the central part of the levitation melting zone to form a composite heating method of surface xenon lamp heating and heart laser heating, and combines
  • the control of the technological process solves the growth problem of large-sized test rod crystals, enabling them to grow crystals with a diameter of ⁇ 30mm, which is beneficial to the realization of engineering applications.
  • a laser-assisted heating device for growing large-sized crystals is characterized in that the device includes a laser core heating device 1, a xenon lamp surface heating device 2, a base 3, and a vacuum cavity 4, wherein:
  • the laser core heating device 1 is composed of a laser focusing lens 11, a lens holder 12, an upper support rod 13, and an optical fiber 15.
  • the laser focusing lens 11 is mounted on the lens holder 12 and connected to the laser 18 through the optical fiber 15.
  • the upper support rod 13 is The hollow structure is fixed to the lower end of the lens holder 12 through a flange and a sealing sleeve 16, and a lens is arranged between the upper support rod 13 and the laser focusing lens 11, so that the laser can pass through smoothly and play a sealing role;
  • the feeding rod 33 is a hollow structure and is suspended from the lower end of the upper support rod 13; the seed crystal rod 34 is located below the feeding rod 33 and fixed on the lower support rod 35, the lower support rod 35 is fixed on the base 3, and the feeding rod 33 and the seed crystal A suspension melting zone 36 is formed between the rods 34;
  • the xenon lamp surface heating device 2 is composed of a xenon lamp 21, an ellipsoidal mirror 22 and a xenon lamp fixing device 23.
  • the xenon lamp fixing device 23 is located between the lens holder 12 and the base 3, and is used to fix the xenon lamp 21 and the ellipsoidal mirror 22.
  • the vacuum cavity 4 is composed of an upper vacuum cavity 41, a quartz tube 42 and a lower vacuum cavity 43.
  • the upper vacuum cavity 41 and the lower vacuum cavity 43 fix the quartz tube 42 in the middle (the upper vacuum cavity 41 is located in the lens holder 12 And the xenon lamp fixing device 23, the quartz tube 42 is located between the xenon lamp fixing device 23 and the base 3, and the lower vacuum cavity 43 is located below the base 3); the upper vacuum cavity 41, the quartz tube 42 and the lower vacuum cavity 43
  • the flange and the vacuum rubber ring communicate with each other to form a vacuum cavity; the lower end of the upper support rod 13, the feeding rod 33, the seed rod 34 and the upper end of the lower support rod 35 are all inside the quartz tube 41.
  • the inner diameter of the upper support rod 13 is 12 to 15 mm and the outer diameter is 20 mm; the inner diameter of the feeding rod 33 is 12 to 15 mm and the outer diameter is 32 to 35 mm.
  • the lower part of the lens holder 12 is provided with an adjusting device 17 for adjusting the height of the lens holder 12 and the included angle with the horizontal direction.
  • the upper support rod 13, the feeding rod 33, the seed crystal rod 34 and the lower support rod 35 are all coaxial.
  • the upper vacuum cavity 41 is provided with an exhaust port with an exhaust valve 31, and the lower vacuum cavity 43 is provided with an air inlet with an intake valve 32.
  • the laser focusing lens 11 is provided with an air-cooled joint and / or a water-cooled joint.
  • the upper support rod 13 and the lower support rod 35 are respectively connected with the rotating device for driving the feeding rod 33 and the seed rod 34 to rotate; the upper support rod 13 is connected with the lifting device for controlling the lifting of the upper support rod 13.
  • the number of the xenon lamps 21 and the ellipsoidal reflector 22 is the same, both are 2-6, and they are evenly distributed around the feeding rod 33.
  • the invention also provides a method for growing large-sized crystals by using the device, which is characterized in that: a device for growing large-sized crystals using laser-assisted heating and seeding and growth by means of coordinated heating by xenon lamps and lasers, the specific steps are as follows:
  • step 4 the rotation speed of the feeding rod 33 and the seed crystal rod 34 is 0-30 r / min, the rotation directions of the feeding rod 33 and the seed crystal rod 34 are the same or opposite, and the rotation speeds are the same or different.
  • step 5 first turn on the xenon lamp 21 to heat the outside of the feeding rod 33 for 2-10 minutes, and then turn on the laser 18 to heat it to grow a better quality crystal;
  • the xenon lamp power is 1.0-5.0kw
  • the laser 18 heating power is from 0W to The speed of 5-10W / min is evenly adjusted to 0.1kw-1.0kw.
  • Step 6 The size of the final prepared crystal is 15 mm in diameter, and a more preferred size is 30 mm in diameter.
  • a focused laser light source is passed through the heart of the upper support rod and the feeding rod, and irradiated from the top to the center region of the suspension melting zone.
  • the combined heating effect of heating around the xenon lamp and central heating of the laser tip is achieved; at the same time, the surface and core of the suspension melting zone are heated more uniformly and uniformly through the control of the process, and the melting zone achieves stable growth, and the temperature gradient is further improved.
  • the liquid interface is improved, thereby increasing the seeding success rate and crystal quality of large-sized crystals.
  • the invention firstly grows a high-performance crystal with a diameter of 35mm, and solves the growth problem of large-sized test rods (diameter ⁇ 30mm).
  • FIG. 1 is a schematic structural diagram of a device for growing a crystal by laser-assisted heating.
  • FIG. 2 is a schematic structural diagram of a laser core heating device.
  • a laser-assisted heating device for growing crystals includes a laser core heating device 1, a xenon lamp surface heating device 2, a base 3, and a vacuum cavity 4, wherein:
  • the laser core heating device 1 is composed of a laser focusing lens 11, a lens holder 12, an upper support rod 13, and an optical fiber 15.
  • the laser focusing lens 11 is mounted on the lens holder 12 and connected to the laser 18 through the optical fiber 15.
  • the laser focusing lens 11 is The position and angle in the horizontal and vertical directions are adjustable;
  • the upper support rod 13 is a hollow structure (12mm inner diameter and 20mm outer diameter), and is fixed to the lower end of the lens holder 12 through a flange and a sealing sleeve 16, and the upper support rod 13 and A lens is provided between the laser focusing lenses 11, and the lens is sealed with a sealing sleeve 16.
  • the function of the lens is to keep the vacuum of the vacuum chamber 4 while allowing the laser light to smoothly pass through the upper support rod 13 to the center of the suspension melting zone 36;
  • the feeding rod 33 is a hollow structure (inner diameter is 15mm and outer diameter is 32mm) and is suspended from the lower end of the upper support rod 13. During assembly, the height of the upper support rod 13 and the central through hole of the feeding rod 33 should be kept coaxial to ensure a smooth light path;
  • the seed crystal rod 34 is located below the feeding rod 33 and is fixed on the lower support rod 35.
  • the lower support rod 35 is fixed on the base 3, and a suspended melting zone 36 is formed between the feeding rod 33 and the seed crystal rod 34;
  • the xenon lamp surface heating device 2 is composed of a xenon lamp 21, an ellipsoidal mirror 22 and a xenon lamp fixing device 23.
  • the xenon lamp fixing device 23 is located between the lens holder 12 and the base 3, and is used to fix the xenon lamp 21 and the ellipsoidal mirror 22.
  • the feeding rod 33 is located at a focal point of the ellipsoidal reflector 22; four xenon lamps 21 and the ellipsoidal reflector 22 are arranged and evenly distributed around the feeding rod 33;
  • the vacuum cavity 4 is composed of an upper vacuum cavity 41, a quartz tube 42 and a lower vacuum cavity 43.
  • the upper vacuum cavity 41 is located between the lens holder 12 and the xenon lamp fixing device 23, and the quartz tube 42 is located between the xenon lamp fixing device 23 and the base 3.
  • the lower vacuum cavity 43 is located below the base 3; the upper vacuum cavity 41, the quartz tube 42 and the lower vacuum cavity 43 communicate with each other through a flange and a vacuum rubber ring to form a vacuum cavity; the upper support rod 13
  • the lower end, the feeding rod 33, the seed rod 34 and the upper end of the lower support rod 35 are all coaxial and located inside the quartz tube 41.
  • the upper vacuum chamber 41 is provided with an exhaust port with an exhaust valve 31, and the lower vacuum chamber 43 An air inlet with an air inlet valve 32 is provided thereon.
  • the upper support rod 13 and the lower support rod 35 are respectively connected with the rotating device for driving the feeding rod 33 and the seed rod 34 to rotate; the upper support rod 13 is connected with the lifting device for controlling the lifting of the upper support rod 13.
  • the crystal preparation process is as follows:
  • Embodiment 1 The difference from Embodiment 1 is that, as shown in FIG. 2, an adjusting device 17 is provided at the lower portion of the lens holder 12. By adjusting and adjusting the height of the lens holder 12 and the angle between the lens holder 12 and the horizontal direction, the laser beam can smoothly reach the suspension melting zone. 36 center.
  • the implementation effect is the same as in Example 1, and finally a large-sized TiNb crystal with a diameter of 30 mm is prepared.
  • Embodiment 1 The difference from Embodiment 1 is that an air-cooled joint is provided at the laser focusing lens 11 for cooling.
  • the implementation effect is the same as in Example 1, and finally a large-sized TiNb crystal with a diameter of 30 mm is prepared.
  • the difference from the embodiment 1 is that two xenon lamps 21 and two ellipsoidal reflectors 22 are provided, and are symmetrically arranged with respect to the feeding rod 33.
  • the implementation effect is the same as in Example 1, and finally a large-sized TiNb crystal with a diameter of 30 mm is prepared.

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
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Abstract

本发明的目的在于提供一种激光辅助加热生长大尺寸晶体的方法及专用设备，所述设备包括激光心部加热装置、氙灯表面加热装置、底座和真空腔体等，在制备晶体时，采用氙灯与激光协同加热的方式引晶生长。本发明通过对专用设备的结构和功能设计，在悬浮熔区的中央部位引入精度高且可控性强的激光加热热源，形成表面氙灯加热和心部激光加热的复合加热方式，并结合过对工艺过程的控制，解决了大尺寸试棒晶体的生长难题，使其可生长直径达35mm的晶体，以利于实现工程化应用。

Description

一种激光辅助加热生长大尺寸晶体的方法及专用设备 技术领域
本发明涉及晶体材料的制备方法，特别提供一种激光辅助加热生长大尺寸晶体的方法及专用设备。
背景技术
光学浮区炉是一种采用光加热的悬浮熔区定向凝固炉，具有无坩埚、高洁净、高温度梯度及生长速度快等特点；广泛应用于氧化物和TiAl等金属间化合物材料的晶体生长研究，特别是那些熔体反应强烈和高熔点的晶体材料。现在广泛应用的光学浮区炉均都采用2～4椭球反射镜聚焦氙灯加热，熔体主要靠表面张力维持形状，沿竖直方向生长，如日本CSC公司生产的型号为FZ-T-12000-X-VP-S的光学浮区炉，均布有4个氙灯，熔点可达3000℃，温度梯度约为200℃，生长速度可在0～180mm/h范围内精确调节，保护气氛可达99.9999％以上，是目前世界上最为先进的光学浮区炉之一。
然而，由于该类设备的加热方式为光加热，即氙灯光源经椭球反射镜聚焦后焦斑照射在试棒表面，然后通过热传导由表及里逐渐升温直至熔化。针对不同的材料，当试棒直径≤15mm时，试棒的中心能够熔化透彻并且内外能够搅拌均匀，悬浮熔区保持稳定，可顺利实现晶体生长；当试棒直径＞15mm时，易导致试棒心部和表面加热不均匀的现象出现，试棒的中心开始出现熔化不透彻，悬浮熔区无法保持稳定和形状，晶体生长无法进行。对于尺寸相对较大的结构件而言，无法实现工程化应用。因此，无法生长大块晶体已成为光学浮区炉的主要缺陷。
发明内容
针对大尺寸试棒(直径＞15mm)晶体生长过程中的加热不均匀、心部熔化不透 彻及悬浮熔区不稳定等问题，本发明提供了一种激光辅助加热生长大尺寸晶体的方法及专用设备，通过对专用设备的结构和功能设计，在悬浮熔区的中央部位引入精度高且可控性强的激光加热热源，形成表面氙灯加热和心部激光加热的复合加热方式，并结合过对工艺过程的控制，解决了大尺寸试棒晶体的生长难题，使其可生长直径≥30mm的晶体，以利于实现工程化应用。
本发明技术方案如下：
一种激光辅助加热生长大尺寸晶体的装置，其特征在于：所述装置包括激光心部加热装置1、氙灯表面加热装置2、底座3和真空腔体4，其中：
激光心部加热装置1由激光聚焦镜头11、镜头支架12、上支撑杆13和光纤15组成；激光聚焦镜头11安装于镜头支架12上，并通过光纤15与激光器18相连；上支撑杆13为空心结构，通过法兰和密封套16固定于镜头支架12下端，上支撑杆13与激光聚焦镜头11之间设有透镜，使激光顺利通过的同时，又起到密封作用；
送料棒33为空心结构，悬挂于上支撑杆13下端；籽晶棒34位于送料棒33的下方，并固定在下支撑杆35上，下支撑杆35固定在底座3上，送料棒33与籽晶棒34之间形成悬浮熔区36；
氙灯表面加热装置2由氙灯21、椭球反光镜22和氙灯固定装置23组成，氙灯固定装置23位于镜头支架12和底座3之间，用于固定氙灯21和椭球反光镜22，氙灯21设置在椭球反光镜22凹面一侧，且正对送料棒33；
真空腔体4由上真空腔体41、石英管42和下真空腔体43组成，上真空腔体41和下真空腔体43将石英管42固定于中间(上真空腔体41位于镜头支架12和氙灯固定装置23之间，石英管42位于氙灯固定装置23和底座3之间，下真空腔体43位于底座3下方)；上真空腔体41、石英管42和下真空腔体43之 间通过法兰和真空胶圈相连通，形成一个真空腔体；上支撑杆13下端、送料棒33、籽晶棒34与下支撑杆35上端均处于石英管41内部。
作为优选的技术方案：
上支撑杆13内径为12～15mm，外径为20mm；送料棒33内径为12～15mm，外径为32～35mm。
镜头支架12下部设有调整装置17，用于调整镜头支架12的高度以及与水平方向的夹角。
上支撑杆13、送料棒33、籽晶棒34与下支撑杆35均同轴。
上真空腔体41上设置带有排气阀31的排气口，下真空腔体43上设置带有进气阀32的进气口。
激光聚焦镜头11处设有风冷接头和/或水冷接头。
上支撑杆13、下支撑杆35分别与转动装置相连，用于带动送料棒33和籽晶棒34转动；上支撑杆13与升降装置相连，用于控制上支撑杆13的升降。
氙灯21和椭球反光镜22的数量相同，均为2-6个，均匀分布在送料棒33的四周。
本发明还提供了一种采用所述装置生长大尺寸晶体的方法，其特征在于：利用激光辅助加热生长大尺寸晶体的装置，采用氙灯与激光协同加热的方式引晶生长，具体步骤如下：
1)、根据成分和尺寸要求制备送料棒33和籽晶棒34，并将它们分别固定在上支撑杆13、下支撑杆35上；
2)、调节激光器18、光纤15和激光聚焦镜头11，使激光束到达激光聚焦镜头11后，聚焦成Ф3～Ф5mm的平行光束，并确保聚焦的平行光束与上支撑杆13中心通孔、送料棒33中心通孔同轴；
3)、对真空腔体4抽真空，使其内部真空度达到10 -3Pa，然后打开进气阀32和排气阀31，向真空腔体4内持续通入氩气(优选2L/min)；
4)、开启升降装置和转动装置，并设定升降和转动速度；
5)、开启氙灯21和激光器18，对送料棒33进行加热；或先开启氙灯21对送料棒33外部进行加热，待悬浮熔区36建立后，再开启激光器18加热；
6)、最终制备出晶体。
作为优选的技术方案：
步骤4)中，送料棒33和籽晶棒34的旋转速度为0-30r/min，送料棒33和籽晶棒34旋转方向相同或相反，旋转速度相同或不同。
步骤5)中，先开启氙灯21对送料棒33外部进行加热2-10min后，再开启激光器18加热，以生长出质量更好的晶体；氙灯功率1.0-5.0kw，激光器18加热功率从0W以5-10W/min的速度均匀调至0.1kw-1.0kw。
步骤6)最终制备出的晶体尺寸为直径≥15mm，更优选的尺寸为直径≥30mm。
本发明通过增加激光心部加热装置，同时采用空心上支撑杆和空心送料棒，将聚焦好的激光光源穿过上支撑杆和送料棒的心部，从顶端照射到悬浮熔区的中心区域，从而实现氙灯四周加热和激光顶端中心加热的复合加热效果；同时结合过对工艺过程的控制，使悬浮熔区的表面和心部受热更加均匀一致，熔区实现稳定生长，温度梯度进一步提高，固液界面得到改善，从而提高大尺寸晶体的引晶成功率和晶体质量，本发明首次生长出直径达35mm的高性能晶体，解决了大尺寸试棒(直径≥30mm)晶体的生长难题。
附图说明
图1激光辅助加热生长晶体的装置结构示意图。
图2激光心部加热装置结构示意图。
附图标记：1、激光心部加热装置，2、氙灯表面加热装置，3、底座，4、真空腔体，11、激光聚焦镜头，12、镜头支架，13、上支撑杆，15、光纤，16、密封套，17、调整装置，18、激光器，21、氙灯，22、椭球反光镜，23、氙灯固定装置，31、排气阀，32、进气阀，33、送料棒，34、籽晶棒，35、下支撑杆，36、悬浮熔区，41、上真空腔体，42、石英管，43、下真空腔体。
具体实施方式
如图1所示，一种激光辅助加热生长晶体的装置，包括激光心部加热装置1、氙灯表面加热装置2、底座3和真空腔体4，其中：
激光心部加热装置1由激光聚焦镜头11、镜头支架12、上支撑杆13和光纤15组成；激光聚焦镜头11安装于镜头支架12上，并通过光纤15与激光器18相连，激光聚焦镜头11在水平和竖直方向上的位置和角度可调；上支撑杆13为空心结构(内径为12mm，外径为20mm)，通过法兰和密封套16固定于镜头支架12下端，上支撑杆13与激光聚焦镜头11之间设有透镜，所述透镜用密封套16密封，透镜的作用为：保持真空腔体4真空度的同时使激光顺利通过上支撑杆13到达悬浮熔区36的中心；
送料棒33为空心结构(内径为15mm，外径为32mm)，悬挂于上支撑杆13下端，装配时，需保持上支撑杆13与送料棒33中心通孔高度同轴，以确保光路畅通；籽晶棒34位于送料棒33的下方，并固定在下支撑杆35上，下支撑杆35固定在底座3上，送料棒33与籽晶棒34之间形成悬浮熔区36；
氙灯表面加热装置2由氙灯21、椭球反光镜22和氙灯固定装置23组成，氙灯固定装置23位于镜头支架12和底座3之间，用于固定氙灯21和椭球反光镜22，氙灯21设置在椭球反光镜22凹面一侧，送料棒33位于椭球反光镜22 的一焦点处；氙灯21和椭球反光镜22均设置4个，均匀分布在送料棒33的四周；
真空腔体4由上真空腔体41、石英管42和下真空腔体43组成，上真空腔体41位于镜头支架12和氙灯固定装置23之间，石英管42位于氙灯固定装置23和底座3之间，下真空腔体43位于底座3下方；上真空腔体41、石英管42和下真空腔体43之间通过法兰和真空胶圈相连通，形成一个真空腔体；上支撑杆13下端、送料棒33、籽晶棒34与下支撑杆35上端均同轴，且处于石英管41内部，上真空腔体41上设置带有排气阀31的排气口，下真空腔体43上设置带有的进气阀32的进气口。
上支撑杆13、下支撑杆35分别与转动装置相连，用于带动送料棒33和籽晶棒34转动；上支撑杆13与升降装置相连，用于控制上支撑杆13的升降。
晶体制备过程如下：
1)、根据成分和尺寸要求制备送料棒33和籽晶棒34，并将它们分别固定在上支撑杆13、下支撑杆35上；
2)、调节激光器18、光纤15和激光聚焦镜头11，使激光束到达激光聚焦镜头11后，聚焦成Ф3～Ф5mm的平行光束，并确保聚焦的平行光束与上支撑杆13中心通孔、送料棒33中心通孔同轴；
3)、对真空腔体4抽真空，使其内部真空度达到10 -3Pa，然后打开进气阀32和排气阀31，向真空腔体4内持续通入氩气(2L/min)；
4)、开启升降装置和转动装置，并设定升降和转动速度；
5)、开启氙灯21和激光器18，对送料棒33进行加热；或先开启氙灯21对送料棒33外部进行加热，待悬浮熔区36建立后，再开启激光器18加热；
6)、最终制备出晶体。
实施例1
制备直径30mm的定向TiNb晶体：
生长速度：6mm/h，送料棒33的旋转速度：10r/min，氙灯功率1.5kw(外部加热)，激光功率0.2kw(芯部加热)，在氙灯开启加热5分钟后引入激光加热，激光加热功率从0W以5W/min的速度均匀调至0.2kw，实现氙灯与激光协同加热，最终制备出直径为30mm的大尺寸TiNb晶体。
实施例2
制备直径30mm的定向NbSi晶体：
生长速度：7mm/h，送料棒33的旋转速度：3r/min，氙灯功率2.5kw(外部加热)，激光功率0.5kw(芯部加热)，在氙灯开启加热8分钟后引入激光加热，激光加热功率从0W以6W/min的速度均匀调至0.5kw，实现氙灯与激光协同加热，最终制备出直径为30mm的大尺寸NbSi晶体。
实施例3
制备直径30mm的定向Al 2O 3/YAG晶体：
生长速度：10mm/h，送料棒33的旋转速度：15r/min，氙灯功率2.0kw(外部加热)，激光功率0.3kw(芯部加热)，在氙灯开启加热5分钟后引入激光加热，激光加热功率从0W以5W/min的速度均匀调至0.3kw，实现氙灯与激光协同加热，最终制备出直径为30mm的大尺寸Al 2O 3/YAG晶体。
实施例4
制备直径30mm的定向GaO晶体：
生长速度：5mm/h，送料棒33的旋转速度：12r/min，氙灯功率1.0kw(外部加热)，激光功率0.1kw(芯部加热)，在氙灯开启加热3分钟后引入激光加热，激光加热功率从0W以5W/min的速度均匀调至0.1kw，实现氙灯与激光协同加热，最终制备出直径为30mm的大尺寸GaO晶体。
实施例5
制备直径30mm的定向Ni-Fe-Ga晶体：
生长速度：15mm/h，送料棒33的旋转速度：20r/min，氙灯功率3.0kw(外部加热)，激光功率0.6kw(芯部加热)，在氙灯开启加热6分钟后引入激光加热，激光加热功率从0W以6W/min的速度均匀调至0.6kw，实现氙灯与激光协同加热，最终制备出直径为30mm的大尺寸Ni-Fe-Ga晶体。
实施例6
制备直径33mm的定向TiAl晶体：
生长速度：5mm/h，送料棒33的旋转速度：9r/min，氙灯功率2.0kw(外部加热)，激光功率0.2kw(芯部加热)，在氙灯开启加热5分钟后引入激光加热，激光加热功率从0W以5W/min的速度均匀调至0.2kw，实现氙灯与激光协同加热，最终制备出直径为33mm的大尺寸TiAl晶体。
实施例7
制备直径30mm的定向TiAlNb晶体：
生长速度：15mm/h，送料棒33的旋转速度：12r/min，氙灯功率6.0kw(外部加热)，激光功率0.6kw(芯部加热)，在氙灯开启加热6分钟后引入激光加热，激光加热功率从0W以6W/min的速度均匀调至0.6kw，实现氙灯与激光协同加 热，最终制备出直径为30mm的大尺寸TiAlNb晶体。
实施例8
制备直径30mm的定向Al 2O 3晶体：
生长速度：20mm/h，送料棒33的旋转速度：25r/min，氙灯功率3.0kw(外部加热)，激光功率0.5kw(芯部加热)，在氙灯开启加热6分钟后引入激光加热，激光加热功率从0W以6W/min的速度均匀调至0.6kw，实现氙灯与激光协同加热，最终制备出直径为30mm的大尺寸Al 2O 3晶体。
实施例9
与实施例1的不同之处在于：如图2所示，镜头支架12下部设有调整装置17，通过调整调整镜头支架12的高度以及与水平方向的夹角，使激光束顺利到达悬浮熔区36的中心。其实施效果与实施例1相同，最终制备出直径达到30mm的大尺寸TiNb晶体。
实施例10
与实施例1的不同之处在于：激光聚焦镜头11处设有风冷接头用于冷却。其实施效果与实施例1相同，最终制备出直径达到30mm的大尺寸TiNb晶体。
实施例11
与实施例1的不同之处在于：氙灯21和椭球反光镜22均设置2个，关于送料棒33对称设置。其实施效果与实施例1相同，最终制备出直径达到30mm的大尺寸TiNb晶体。
实施例12
制备直径35mm的定向TiNb晶体：
生长速度：6mm/h，送料棒33的旋转速度：10r/min，氙灯功率1.9kw(外部加热)，激光功率0.29kw(芯部加热)，在氙灯开启加热8分钟后引入激光加热，激光加热功率从0W以5W/min的速度均匀调至0.29kw，实现氙灯与激光协同加热，最终制备出直径为35mm的大尺寸TiNb晶体。
实施例13
制备直径35mm的定向TiAl晶体：
生长速度：5mm/h，送料棒33的旋转速度：9r/min，氙灯功率2.5kw(外部加热)，激光功率0.26kw(芯部加热)，在氙灯开启加热5分钟后引入激光加热，激光加热功率从0W以5W/min的速度均匀调至0.26kw，实现氙灯与激光协同加热，最终制备出直径为35mm的大尺寸TiAl晶体。
实施例14
制备直径35mm的定向TiAlNb晶体：
生长速度：15mm/h，送料棒33的旋转速度：12r/min，氙灯功率8kw(外部加热)，激光功率0.65kw(芯部加热)，在氙灯开启加热8分钟后引入激光加热，激光加热功率从0W以5W/min的速度均匀调至0.65kw，实现氙灯与激光协同加热，最终制备出直径为35mm的大尺寸TiAlNb晶体。
实施例15
制备直径35mm的定向Al 2O 3/YAG晶体：
生长速度：10mm/h，送料棒33的旋转速度：15r/min，氙灯功率2.5kw(外部加热)，激光功率0.35kw(芯部加热)，在氙灯开启加热3分钟后引入激光加热，激光加热功率从0W以5W/min的速度均匀调至0.35kw，实现氙灯与激光协同加热，最终制备出直径为35mm的大尺寸Al 2O 3/YAG晶体。
实施例16
制备直径35mm的定向Al 2O 3晶体：
生长速度：20mm/h，送料棒33的旋转速度：25r/min，氙灯功率3.5kw(外部加热)，激光功率0.55kw(芯部加热)，在氙灯开启加热5分钟后引入激光加热，激光加热功率从0W以5W/min的速度均匀调至0.55kw，实现氙灯与激光协同加热，最终制备出直径为35mm的大尺寸Al 2O 3晶体。
实施例17
制备直径35mm的定向Al 2O 3/ZrO 2：
生长速度：10mm/h，送料棒33的旋转速度：15r/min，氙灯功率1.2kw(外部加热)，激光功率0.25kw(芯部加热)，在氙灯开启加热5分钟后引入激光加热，激光加热功率从0W以5W/min的速度均匀调至0.25kw，实现氙灯与激光协同加热，最终制备出直径为35mm的大尺寸AlO 3/ZrO 2晶体。
实施例18
制备直径35mm的定向Al 2O 3/Y 2O 3晶体：
生长速度：20mm/h，送料棒33的旋转速度：15r/min，氙灯功率1.3kw(外 部加热)，激光功率0.23kw(芯部加热)，在氙灯开启加热5分钟后引入激光加热，激光加热功率从0W以5W/min的速度均匀调至0.23kw，实现氙灯与激光协同加热，最终制备出直径为35mm的大尺寸AlO 3/Y 2O 3晶体。
实施例19
制备直径35mm的定向NiFeGaCo晶体：
生长速度：5mm/h，送料棒33的旋转速度：15r/min，氙灯功率1.0kw(外部加热)，激光功率0.15kw(芯部加热)，在氙灯开启加热3分钟后引入激光加热，激光加热功率从0W以5W/min的速度均匀调至0.15kw，实现氙灯与激光协同加热，最终制备出直径为35mm的大尺寸NiFeGaCo晶体。
实施例20
制备直径35mm的定向Al 2O 3/Sn 2O 3晶体：
生长速度：9mm/h，送料棒33的旋转速度：10r/min，氙灯功率1.0kw(外部加热)，激光功率0.15kw(芯部加热)，在氙灯开启加热8分钟后引入激光加热，激光加热功率从0W以5W/min的速度均匀调至0.15kw，实现氙灯与激光协同加热，最终制备出直径为35mm的大尺寸AlO 3/Sn 2O 3晶体。
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。
此外，本文省略了对公知结构和技术的描述，以避免不必要地混淆本发明的概念。

Claims (10)

  1. 一种激光辅助加热生长大尺寸晶体的装置，其特征在于：所述装置包括激光心部加热装置(1)、氙灯表面加热装置(2)、底座(3)和真空腔体(4)，其中：
    激光心部加热装置(1)由激光聚焦镜头(11)、镜头支架(12)、上支撑杆(13)和光纤(15)组成；激光聚焦镜头(11)安装于镜头支架(12)上，并通过光纤(15)与激光器(18)相连；上支撑杆(13)为空心结构，通过法兰和密封套(16)固定于镜头支架(12)下端，上支撑杆(13)与激光聚焦镜头(11)之间设有透镜；
    送料棒(33)为空心结构，悬挂于上支撑杆(13)下端；籽晶棒(34)位于送料棒(33)的下方，并固定在下支撑杆(35)上，下支撑杆(35)固定在底座(3)上，送料棒(33)与籽晶棒(34)之间形成悬浮熔区(36)；
    氙灯表面加热装置(2)由氙灯(21)、椭球反光镜(22)和氙灯固定装置(23)组成，氙灯固定装置(23)位于镜头支架(12)和底座(3)之间，用于固定氙灯(21)和椭球反光镜(22)，氙灯(21)设置在椭球反光镜(22)凹面一侧，且正对送料棒(33)；
    真空腔体(4)由上真空腔体(41)、石英管(42)和下真空腔体(43)组成，上真空腔体(41)和下真空腔体(43)将石英管(42)固定于中间；上真空腔体(41)、石英管(42)和下真空腔体(43)之间通过法兰和真空胶圈相连通，形成一个真空腔体；上支撑杆(13)下端、送料棒(33)、籽晶棒(34)与下支撑杆(35)上端均处于石英管(41)内部。
  2. 按照权利要求1所述激光辅助加热生长大尺寸晶体的装置，其特征在于：上支撑杆(13)内径为12～15mm，外径为20mm；送料棒(33)内径为12～15mm，外径为32～35mm。
  3. 按照权利要求1所述激光辅助加热生长大尺寸晶体的装置，其特征在于：镜头支架(12)下部设有调整装置(17)，用于调整镜头支架(12)的高度以及与水平方向的夹角。
  4. 按照权利要求1所述激光辅助加热生长大尺寸晶体的装置，其特征在于：上支撑杆(13)、下支撑杆(35)分别与转动装置相连，用于带动送料棒(33)和籽晶棒(34)转动；上支撑杆(13)与升降装置相连，用于控制上支撑杆(13)的升降。
  5. 按照权利要求1所述激光辅助加热生长大尺寸晶体的装置，其特征在于：上真空腔体(41)上设置带有排气阀(31)的排气口，下真空腔体(43)上设置带有进气阀(32)的进气口。
  6. 一种采用权利要求1所述装置生长大尺寸晶体的方法，其特征在于：利用激光辅助加热生长大尺寸晶体的装置，采用氙灯与激光协同加热的方式引晶生长。
  7. 按照权利要求6所述生长大尺寸晶体的方法，其特征在于，具体步骤如下：
    1)、根据成分和尺寸要求制备送料棒(33)和籽晶棒(34)，并将它们分别固定在上支撑杆(13)、下支撑杆(35)上；
    2)、调节激光器(18)、光纤(15)和激光聚焦镜头(11)，使激光束到达激光聚焦镜头(11)后，聚焦成Φ3～Φ5mm的平行光束，并确保聚焦的平行光束与上支撑杆(13)中心通孔、送料棒(33)中心通孔同轴；
    3)、对真空腔体(4)抽真空，使其内部真空度达到10 -3Pa，然后打开进气阀(32)和排气阀(31)，向真空腔体(4)内持续通入氩气；
    4)、开启升降装置和转动装置，并设定升降和转动速度；
    5)、开启氙灯(21)和激光器(18)，对送料棒(33)进行加热；或先开启氙灯(21)对送料棒(33)外部进行加热，待悬浮熔区(36)建立后，再开启激光器(18)加热；
    6)、最终制备出晶体。
  8. 按照权利要求7所述生长大尺寸晶体的方法，其特征在于：步骤4)中，送料棒(33)和籽晶棒(34)的旋转速度为0-30r/min，送料棒(33)和籽晶棒(34)旋转方向相同或相反，旋转速度相同或不同。
  9. 按照权利要求7所述生长大尺寸晶体的方法，其特征在于：步骤5)中，先开启氙灯(21)对送料棒(33)外部进行加热2-10min后，再开启激光器(18)加热；氙灯功率1.0-5.0kw，激光器(18)加热功率从0W以5-10W/min的速度均匀调至0.1kw-1.0kw。
  10. 按照权利要求6所述生长大尺寸晶体的方法，其特征在于：步骤6)最终制备出的晶体尺寸为直径≥30mm。
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Families Citing this family (4)

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Publication number Priority date Publication date Assignee Title
CN110528062A (zh) * 2018-05-23 2019-12-03 中国科学院金属研究所 激光辅助加热生长大尺寸钛合金晶体的方法及专用设备
CN112663142B (zh) * 2020-12-04 2022-06-07 广东省科学院半导体研究所 Ruddlesden-Popper型锰氧化物单晶及其制备方法
CN114086244B (zh) * 2021-10-12 2023-01-03 杭州富加镓业科技有限公司 一种导模法生长氧化镓晶体的方法
CN114525590B (zh) * 2022-01-26 2023-03-24 深圳先进电子材料国际创新研究院 一种多功能晶体生长装置

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3819421A (en) * 1972-03-01 1974-06-25 Siemens Ag Method for the manufacture of dislocation-free, single-crystal gallium arsenide rod
CN1309196A (zh) * 2000-11-06 2001-08-22 西北工业大学 一种用于晶体生长的加热方法及其装置
CN102051669A (zh) * 2010-11-04 2011-05-11 西北工业大学 一种用于激光悬浮区熔定向凝固的装置及定向凝固方法
CN102051668A (zh) * 2010-11-04 2011-05-11 西北工业大学 105K/cm温度梯度定向凝固装置及定向凝固方法
CN102534791A (zh) * 2012-01-19 2012-07-04 山东大学 激光激活离子掺杂浓度梯度的钒酸盐复合晶体及其制备方法
CN102560666A (zh) * 2012-01-19 2012-07-11 山东大学 一种石榴石结构复合激光晶体的制备方法
CN208395312U (zh) * 2018-05-23 2019-01-18 中国科学院金属研究所 一种激光辅助加热生长晶体的装置

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000007484A (ja) * 1998-06-18 2000-01-11 Advantest Corp 集光加熱装置及び集光加熱式帯溶融装置及びそれにより生産される単結晶及び高純度金属
JP4128278B2 (ja) * 1998-07-27 2008-07-30 株式会社アドバンテスト 単結晶製造装置
DE10055446B4 (de) * 1999-11-26 2012-08-23 Fuji Electric Co., Ltd. Halbleiterbauelement und Verfahren zu seiner Herstellung
WO2008096889A1 (ja) * 2007-02-07 2008-08-14 National Institute For Materials Science ヨウ化物系単結晶体、その製造方法、およびヨウ化物系単結晶体からなるシンチレータ
JP2009051679A (ja) * 2007-08-24 2009-03-12 Nippon Light Metal Co Ltd 単結晶育成装置、単結晶育成方法
JP5279727B2 (ja) * 2007-12-25 2013-09-04 株式会社クリスタルシステム 浮遊帯域溶融装置
US20110192461A1 (en) * 2010-01-20 2011-08-11 Integrated Photovoltaic, Inc. Zone Melt Recrystallization of layers of polycrystalline silicon
JP5926432B1 (ja) * 2015-10-01 2016-05-25 伸 阿久津 単結晶製造装置および単結晶製造方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3819421A (en) * 1972-03-01 1974-06-25 Siemens Ag Method for the manufacture of dislocation-free, single-crystal gallium arsenide rod
CN1309196A (zh) * 2000-11-06 2001-08-22 西北工业大学 一种用于晶体生长的加热方法及其装置
CN102051669A (zh) * 2010-11-04 2011-05-11 西北工业大学 一种用于激光悬浮区熔定向凝固的装置及定向凝固方法
CN102051668A (zh) * 2010-11-04 2011-05-11 西北工业大学 105K/cm温度梯度定向凝固装置及定向凝固方法
CN102534791A (zh) * 2012-01-19 2012-07-04 山东大学 激光激活离子掺杂浓度梯度的钒酸盐复合晶体及其制备方法
CN102560666A (zh) * 2012-01-19 2012-07-11 山东大学 一种石榴石结构复合激光晶体的制备方法
CN208395312U (zh) * 2018-05-23 2019-01-18 中国科学院金属研究所 一种激光辅助加热生长晶体的装置

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