CN106757359B - Adjusting reaction kettle for crystal growth and control method thereof - Google Patents
Adjusting reaction kettle for crystal growth and control method thereof Download PDFInfo
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- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 9
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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
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
- C30B29/406—Gallium nitride
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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
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
- C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
- C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
- C30B9/10—Metal solvents
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Abstract
本发明公开了一种用于晶体生长的调节反应釜及其控制方法，包括釜体和设在釜体内的加热器，所述釜体内至少设置一个晶体生长用坩埚和一个反应物溶液调整坩埚，该晶体生长用坩埚和反应物溶液调整坩埚通过充满反应物溶液的连通管路连接，釜体上设有升降移动控制机构，该升降移动控制机构分别与晶体生长用坩埚和反应物溶液调整坩埚连接，带动该晶体生长用坩埚和反应物溶液调整坩埚上升或下降。本发明实现反应物液体在两个坩埚间循环流动，该流动会进一步促进反应物液面的波动，增强反应物液体与氮气的进一步混合，提高材料生长速率和质量。
The present invention discloses a regulating reactor for crystal growth and a control method thereof, comprising a reactor body and a heater arranged in the reactor body, wherein at least one crystal growth crucible and a reactant solution adjustment crucible are arranged in the reactor body, the crystal growth crucible and the reactant solution adjustment crucible are connected through a connecting pipe filled with reactant solution, and a lifting and moving control mechanism is arranged on the reactor body, the lifting and moving control mechanism is respectively connected with the crystal growth crucible and the reactant solution adjustment crucible, and drives the crystal growth crucible and the reactant solution adjustment crucible to rise or fall. The present invention realizes the circulating flow of reactant liquid between two crucibles, and the flow will further promote the fluctuation of reactant liquid level, enhance the further mixing of reactant liquid and nitrogen, and improve the material growth rate and quality.
Description
技术领域technical field
本发明属于半导体，尤其是第三代Ⅲ族氮化物半导体的制备技术领域，具体地说是一种用于晶体生长的调节反应釜及其控制方法。The invention belongs to the technical field of the preparation of semiconductors, especially the third-generation III-nitride semiconductors, in particular to a regulating reaction kettle for crystal growth and a control method thereof.
背景技术Background technique
氮化镓(GaN)作为第三代Ⅲ族氮化物半导体，属于宽带隙半导体材料(～3.4eV)，在光电子器件等诸多应用领域中，厚膜GaN作为同质外延衬底将对器件性能提高起到巨大的推动作用。目前GaN晶体厚膜的研制方法，主要是金属有机化学气相沉积法(MOCVD)、氢化物气相外延法(HVPE)、分子束外延法(MBE)等。气相生长法得到的氮化镓晶体位错密度较大，而传统的制备硅(Si)、砷化镓(GaAs)单晶衬底的液相提拉法很难用于生长GaN衬底材料。为此，人们提出将钠(Na)等碱金属作为溶剂，可在比较温和的条件下液相生长GaN等氮化物晶体。在液相法生长GaN晶体中，晶体生长质量和速率将受到晶种模版表面Ga-Na溶液中氮浓度重要影响，目前有采用旋转、摇摆及搅拌等方法促进氮气与Ga源的混合，但是这些方法都无法使反应溶液整体做均一的运动，不利于获得质量均一的GaN晶体材料。Gallium nitride (GaN), as the third-generation III-nitride semiconductor, is a wide bandgap semiconductor material (~3.4eV). In many applications such as optoelectronic devices, thick-film GaN as a homoepitaxial substrate will improve device performance. play a huge role in promoting. At present, the development methods of GaN crystal thick films are mainly metal organic chemical vapor deposition (MOCVD), hydride vapor phase epitaxy (HVPE), molecular beam epitaxy (MBE) and so on. The dislocation density of the gallium nitride crystal obtained by the vapor phase growth method is relatively high, and the traditional liquid-phase pulling method for preparing silicon (Si) and gallium arsenide (GaAs) single crystal substrates is difficult to grow GaN substrate materials. For this reason, it has been proposed that an alkali metal such as sodium (Na) can be used as a solvent to grow nitride crystals such as GaN in a liquid phase under relatively mild conditions. In the growth of GaN crystals by the liquid phase method, the quality and rate of crystal growth will be greatly affected by the nitrogen concentration in the Ga-Na solution on the surface of the seed crystal template. At present, methods such as rotation, rocking and stirring are used to promote the mixing of nitrogen and Ga sources, but these None of the methods can make the reaction solution move uniformly as a whole, which is not conducive to obtaining GaN crystal materials with uniform quality.
发明内容SUMMARY OF THE INVENTION
本发明要解决的技术问题是提供一种便于控制和操作的用于晶体生长的调节反应釜及其控制方法。The technical problem to be solved by the present invention is to provide a regulating reactor for crystal growth that is easy to control and operate and a control method thereof.
为了解决上述技术问题，本发明采取以下技术方案：In order to solve the above-mentioned technical problems, the present invention adopts the following technical solutions:
一种用于晶体生长的调节反应釜，包括釜体和设在釜体内的加热器，所述釜体内至少设置一个晶体生长用坩埚和一个反应物溶液调整坩埚，该晶体生长用坩埚和反应物溶液调整坩埚通过充满反应物溶液的连通管路连接，釜体上设有升降移动控制机构，该升降移动控制机构分别与晶体生长用坩埚和反应物溶液调整坩埚连接，带动该晶体生长用坩埚和反应物溶液调整坩埚上升或下降。An adjustment reaction kettle for crystal growth, comprising a kettle body and a heater arranged in the kettle body, wherein at least one crystal growth crucible and a reactant solution adjustment crucible are arranged in the kettle body, the crystal growth crucible and reactants are provided The solution adjustment crucible is connected by a communication pipeline filled with the reactant solution, and the kettle body is provided with a lifting movement control mechanism, which is respectively connected with the crystal growth crucible and the reactant solution adjustment crucible, and drives the crystal growth crucible and the reactant solution. The reactant solution adjusts the crucible up or down.
所述连通管路至少设置一条。At least one communication pipeline is provided.
所述连通管路由石英、陶瓷、高纯铜管或不锈钢管材料制成。The communication pipe is made of quartz, ceramic, high-purity copper pipe or stainless steel pipe material.
所述晶体生长用坩埚和反应物溶液调整坩埚的侧面和底面均设有加热器。The crucible for crystal growth and the reactant solution adjustment crucible are provided with heaters on the side and bottom surfaces.
所述晶体生长用坩埚和反应物溶液调整坩埚的数量相同或者不同。The crystal growth crucibles and the reactant solution adjustment crucibles may have the same or different numbers.
所述加热器为红外加热器、电阻加热器或射频加热器。The heater is an infrared heater, a resistance heater or a radio frequency heater.
一种用于晶体生长的调节反应釜的控制方法，包括以下步骤：A kind of control method for the regulation reactor of crystal growth, comprises the following steps:
初始状态下，在晶体生长用坩埚放置晶种模板和填充反应物溶液，在反应物溶液调整坩埚内填充反应物溶液，晶体生长用坩埚的液面和反应物溶液调整坩埚的液面位于同一高度；In the initial state, place the crystal seed template and fill the reactant solution in the crucible for crystal growth, and fill the reactant solution in the reactant solution adjustment crucible. The liquid level of the crystal growth crucible and the liquid level of the reactant solution adjustment crucible are at the same height. ;
启动加热器进行加热升温，同时往釜体内引入氮气；Start the heater to heat up, and introduce nitrogen into the kettle at the same time;
在加热升温过程中，调整晶体生长用坩埚和反应物溶液调整坩埚的相对高度，使晶体生长用坩埚和反应物溶液调整坩埚内的反应物溶液经连通管路相互流动，直到晶体生长完成；During the heating and heating process, adjust the relative height of the crucible for crystal growth and the reactant solution to adjust the crucible, so that the reactant solution in the crucible for crystal growth and the reactant solution to adjust the crucible flow through the communication pipeline until the crystal growth is completed;
晶体生长完成后，使晶体生长用坩埚和反应物溶液调整坩埚复位，重新保持液面相同的高度。After the crystal growth is completed, the crystal growth crucible and the reactant solution adjustment crucible are reset to maintain the same height of the liquid level again.
在控制晶体生长用坩埚和反应物溶液调整坩埚的相对高度时，保持晶体生长用坩埚静止不动，使反应物溶液调整坩埚上升和下降；或者保持反应物溶液调整坩埚静止不动，使晶体生长用坩埚上升和下降；或者晶体生长用坩埚和反应物溶液调整坩埚分别上升和下降。When controlling the relative height of the crucible for crystal growth and the reactant solution to adjust the crucible, keep the crucible for crystal growth still, and let the reactant solution adjust the crucible to rise and fall; or keep the reactant solution to adjust the crucible still, so that the crystal grows Use the crucible to ascend and descend; or adjust the crucible to ascend and descend with the crucible and reactant solution for crystal growth.
所述晶体生长用坩埚和/或反应物溶液调整坩埚在上升和下降时，以连续运动、周期运动或间歇运动的方式进行运动。The crystal growth crucible and/or the reactant solution adjusts the crucible to move in the manner of continuous motion, periodic motion or intermittent motion when ascending and descending.
在加热升温过程中，晶体生长用坩埚和反应物溶液调整坩埚的温度相同或者不相同。During the heating and heating process, the temperature of the crucible for crystal growth and the temperature of the reactant solution adjustment crucible are the same or different.
本发明通过控制晶体生长用坩埚和/或反应物溶液调整坩埚的上升和下降，使得两者之间的反应物溶液相互流动，会进一步促进反应物液面的波动，增强反应物液体与氮气的进一步混合，提高材料生长速率和质量。The present invention adjusts the rise and fall of the crucible by controlling the crucible for crystal growth and/or the reactant solution, so that the reactant solution between the two flows mutually, which further promotes the fluctuation of the reactant liquid level and enhances the interaction between the reactant liquid and nitrogen. Further mixing increases material growth rate and quality.
附图说明Description of drawings
附图1为本发明晶体生长用坩埚和反应物溶液调整坩埚处于同一水平面的状态示意图；Accompanying
附图2为本发明晶体生长用坩埚和反应物溶液调整坩埚处于不同水平面的状态示意图；Accompanying
附图3为本发明设置多个晶体生长用坩埚和反应物溶液调整坩埚的俯视示意图。FIG. 3 is a schematic top view of the present invention with a plurality of crucibles for crystal growth and a reactant solution adjustment crucible.
附图标记：Reference number:
1-晶体生长用坩埚；2-反应物溶液调整坩埚；30晶体生长用坩埚内的反应物溶液；31-反应物溶液调整坩埚内的反应物溶液；10-釜体；20-加热器；40-连通管路。1- crucible for crystal growth; 2- reactant solution adjustment crucible; 30-reactant solution in the crucible for crystal growth; 31- reactant solution for adjusting the reactant solution in the crucible; 10- kettle body; 20- heater; 40 - Connecting pipes.
具体实施方式Detailed ways
为了便于本领域技术人员的理解，下面结合附图对本发明作一步的描述。In order to facilitate the understanding of those skilled in the art, the present invention will be further described below with reference to the accompanying drawings.
如附图1和2所示，本发明揭示了一种用于晶体生长的调节反应釜，包括釜体10和设在釜体10内的加热器20，所述釜体10内至少设置一个晶体生长用坩埚1和一个反应物溶液调整坩埚2，该晶体生长用坩埚1和反应物溶液调整坩埚2通过充满反应物溶液的连通管路40连接，釜体10上设有升降移动控制机构，该升降移动控制机构分别与晶体生长用坩埚1和反应物溶液调整坩埚2连接，带动该晶体生长用坩埚和反应物溶液调整坩埚上升或下降。该升降移动控制机构可以设置一个气缸或者电机，通过连杆与气缸或者电机连接，并且连杆与晶体生长用坩埚和反应物溶液调整坩埚连接，从而带动升降运动。或者其他形式的升降移动控制机构，只要能够实现升降移动即可，在此不再一一列举。As shown in Figures 1 and 2, the present invention discloses a regulating reaction kettle for crystal growth, comprising a
连通管路40至少设置一条，可设置多条，晶体生长用坩埚和反应物溶液调整坩埚之间通过多条连通管路连接，实现更快速的反应物溶液流动。连通管路由石英、陶瓷、高纯铜管或不锈钢管材料制成。At least one communicating
晶体生长用坩埚1和反应物溶液调整坩埚2的侧面和底面均设有加热器20。该加热器为红外加热器、电阻加热器或射频加热器，或者其他方式的加热器。The
在整个生长过程中，晶体生长用坩埚1和反应物溶液调整坩埚2通过交替上升下降的循环运动，实现反应物溶液在彼此间的循环，每一次循环都会促进反应物溶液的流动，并在流动中通过液面的变化，实现新鲜氮气不断进入液体镓，向已经消耗掉氮气的非饱和液体中补充氮气，反应得以顺利进行。当晶体生长用坩埚1高于反应物溶液调整坩埚2时，晶体生长用坩埚1中的反应物溶液30流向反应物溶液调整坩埚2；当反应物溶液调整坩埚2高于晶体生长用坩埚1时，反应物溶液调整坩埚2的反应物溶液31流向晶体生长用坩埚1，实现反应物溶液的彼此流动，从而有利于促进氮化镓晶体高速生长。During the whole growth process, the
此外，晶体生长用坩埚和反应物溶液调整坩埚的数量相同或者不同。而且，如附图3所示，设置两个晶体生长用坩埚1和两个反应物溶液调整坩埚2，该两个晶体生长用坩埚1和两个反应物溶液调整坩埚2通过连通管路40两两相连。In addition, the number of crucibles for crystal growth and the number of reactant solution adjustment crucibles are the same or different. Moreover, as shown in FIG. 3 , two
另外，本发明还揭示了一种用于晶体生长的调节反应釜的控制方法，包括以下步骤：In addition, the present invention also discloses a control method for adjusting the reactor for crystal growth, comprising the following steps:
S1,初始状态下，在晶体生长用坩埚放置晶种模板和填充反应物溶液，在反应物溶液调整坩埚内填充反应物溶液，晶体生长用坩埚的液面和反应物溶液调整坩埚的液面位于同一高度。此时两个坩埚的反应物溶液不会相互流动。S1, in the initial state, place the crystal seed template and fill the reactant solution in the crucible for crystal growth, fill the reactant solution in the reactant solution adjustment crucible, and the liquid level of the crucible for crystal growth and the liquid level of the reactant solution adjustment crucible are located at the same height. The reactant solutions of the two crucibles do not flow to each other at this time.
S2，启动加热器进行加热升温，同时往釜体内引入氮气。晶体生长用坩埚和反应物溶液调整坩埚的温度相同或者不相同。S2, start the heater to heat up, and introduce nitrogen into the kettle at the same time. The temperature of the crystal growth crucible and the reactant solution adjustment crucible are the same or different.
S3，在加热升温过程中，调整晶体生长用坩埚和反应物溶液调整坩埚的相对高度，使晶体生长用坩埚和反应物溶液调整坩埚内的反应物溶液经连通管路相互流动，直到晶体生长完成；S3, during the heating and heating process, adjust the crucible for crystal growth and the reactant solution to adjust the relative height of the crucible, so that the crucible for crystal growth and the reactant solution adjust the reactant solution in the crucible to flow each other through the communication pipeline until the crystal growth is completed. ;
S4，晶体生长完成后，使晶体生长用坩埚和反应物溶液调整坩埚复位，重新保持液面相同的高度。S4, after the crystal growth is completed, the crystal growth crucible and the reactant solution adjustment crucible are reset to maintain the same height of the liquid level again.
在控制晶体生长用坩埚和反应物溶液调整坩埚的相对高度时，保持晶体生长用坩埚静止不动，使反应物溶液调整坩埚上升和下降；或者保持反应物溶液调整坩埚静止不动，使晶体生长用坩埚上升和下降；或者晶体生长用坩埚和反应物溶液调整坩埚分别上升和下降。When controlling the relative height of the crucible for crystal growth and the reactant solution to adjust the crucible, keep the crucible for crystal growth still, and let the reactant solution adjust the crucible to rise and fall; or keep the reactant solution to adjust the crucible still, so that the crystal grows Use the crucible to ascend and descend; or adjust the crucible to ascend and descend with the crucible and reactant solution for crystal growth.
通过以上实施例中的技术方案对本发明进行清楚、完整的描述，显然所描述的实施例为本发明一部分实施例，而不是全部。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The present invention is clearly and completely described through the technical solutions in the above embodiments, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of them. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
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