WO2010118640A1 - Method and apparatus for preparing thin films using continuous liquid phase epitaxy - Google Patents
Method and apparatus for preparing thin films using continuous liquid phase epitaxy Download PDFInfo
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- WO2010118640A1 WO2010118640A1 PCT/CN2010/000510 CN2010000510W WO2010118640A1 WO 2010118640 A1 WO2010118640 A1 WO 2010118640A1 CN 2010000510 W CN2010000510 W CN 2010000510W WO 2010118640 A1 WO2010118640 A1 WO 2010118640A1
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- rotating unit
- furnace chamber
- liquid phase
- chamber
- phase epitaxy
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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
- C30B19/00—Liquid-phase epitaxial-layer growth
- C30B19/06—Reaction chambers; Boats for supporting the melt; Substrate holders
Definitions
- the present invention relates to a liquid phase epitaxy method and apparatus, and more particularly to a method and apparatus for preparing a thin film by continuous liquid phase epitaxy. . Background technique
- LPE liquid phase epitaxy
- GaAs epitaxial layer can be grown from a saturated solution in which Ga is a solvent and As is a solute.
- the liquid phase epitaxy method was proposed by Nelson in 1963.
- liquid phase epitaxy has played an important role in the development of compound semiconductor materials and devices.
- this technology has been widely used to grow semiconductor materials such as GaAs, GaAlAs, GaP, InP, Ga InAsP, and to manufacture light-emitting diodes, laser diodes, solar cells, microwave devices, and the like.
- liquid phase epitaxy furnace in which the substrate holder is located.
- the solvent in the furnace is also cooled and reheated first, a large amount of energy is wasted during the cooling process, and the time required for cooling is long, the operation time is long, and the furnace chamber utilization efficiency is not high.
- the object of the present invention is to provide a method and an epitaxial device for continuous liquid phase epitaxy in the preparation of an epitaxial film by liquid phase epitaxy, in which the substrate sheet and the solvent are cooled for a long time.
- a method for preparing a thin film by continuous liquid phase epitaxy using a device having at least two rotating units comprising:
- A adding a melt in the crucible of the furnace chamber, and loading the substrate sheet in the substrate holder in the first rotating unit;
- the first rotating unit is turned to the upper part of the furnace chamber, and the sealing cover above the furnace chamber and the rotating unit is opened, and the substrate holder is lowered. Go to the furnace chamber for liquid phase epitaxy;
- the second rotating unit is turned over the furnace chamber, and the operation of the first rotating unit is repeated to perform epitaxial growth.
- the method further includes: while the second rotating unit performs epitaxial growth, removing the epitaxially grown substrate piece in the first rotating unit, and loading a new substrate piece to be epitaxially grown, such as a substrate piece in the second rotating unit After the epitaxial growth is completed, the second rotating unit leaves the furnace chamber, the first rotating unit is turned over the furnace chamber, and the epitaxial growth operation is repeated, so that the continuous substrate sheet epitaxial growth is repeated repeatedly.
- the invention relates to a device for preparing a film by liquid phase epitaxy of continuous epitaxy, comprising a furnace chamber and at least two rotating units, wherein: the rotating unit and the furnace chamber are separable, and the rotating unit can be rotated and positioned Above the furnace chamber or above the furnace chamber.
- the rotating unit includes a valve chamber, a lifting rotating shaft and a sub-chamber for accommodating the substrate holder.
- the bottom of the lifting and rotating shaft is connected to the substrate holder.
- the rotating unit is movable up and down along the positioning rotation axis.
- the bottom of the valve chamber of each rotary unit has a removable sealing cover. When moving to the furnace chamber, the sealing cover can be removed, and the valve chamber communicates with the furnace chamber. When leaving the furnace chamber, the sealing cover can be re-opened. Sealed at the bottom of the valve chamber.
- the furnace chamber is divided into an upper furnace chamber and a lower furnace chamber, and the top of the upper furnace chamber has a sealing cover.
- the sealing cover of the upper furnace chamber can be removed, and the valve chamber is provided.
- Communicating with the furnace chamber the sealing cover of the upper furnace chamber can be resealed to the top of the furnace chamber when leaving the furnace chamber.
- the sealing cap at the bottom of the valve chamber cooperates with the sealing cap at the top of the furnace chamber so that the high temperature substrate sheet can always be isolated in a closed space to be protected by an inert gas.
- the invention uses a device having at least two rotating units for liquid phase epitaxial growth, and the substrate sheet can be subjected to epitaxial operation in a rotating unit, and each time the operation is completed, the furnace chamber can be completely cooled without waiting for the furnace chamber to be completely cooled.
- Substrate The sheet is raised into one of the rotating units, and is cooled above the furnace chamber, and the second batch of the substrate sheet in the other rotating unit is transferred into the furnace chamber, and the second batch of liquid phase epitaxy is performed, and thus repeated.
- the method and the device of the invention can shorten the time of each liquid phase epitaxy, and greatly improve the use efficiency of the liquid phase epitaxy furnace, which eliminates the disadvantage that the prior art furnace chamber must be cooled and then reheated, and the energy is greatly increased.
- FIG. 1 is a schematic perspective view of a device for preparing a thin film by a liquid crystal epitaxy method of continuous epitaxy according to the present invention
- FIG. 2 is a top view of a device for preparing a thin film by a liquid phase epitaxy method of continuous epitaxy according to the present invention
- Figure 3 is a schematic view showing one of the rotating units of the present invention rotated to the top of the furnace chamber to cooperate with each other;
- FIG. 4 is a schematic structural view of Embodiment 2 of a device for preparing a thin film by a liquid crystal epitaxial method according to the present invention
- FIG. 5 is a schematic structural view of a sealing unit of a rotary unit and a furnace chamber of Embodiment 2;
- Fig. 6 is a schematic view showing the structure of the sealing unit of the rotary unit and the furnace chamber of the third embodiment. detailed description
- Embodiment 1 As shown in Figs. 1 to 3, a device for preparing a film by a liquid phase epitaxy method of continuous epitaxy, comprising: a first rotating unit 1 and a second rotating unit 2, and a furnace chamber 3.
- the first rotating unit 1 includes a lifting and lowering rotating shaft 11, a sub-chamber 12 and a valve chamber 13 which are erected at the center of the valve chamber 13 and the sub-chamber 12; one side of the valve chamber 13 has a door 16 for The substrate piece or the entire substrate holder enters and exits; a control device is externally connected to the upper part of the lifting and rotating shaft 11, and the axis is controlled to perform lifting or rotating motion.
- the bottom of the lifting rotary shaft 11 is fixedly connected or detachably coupled to a substrate holder 4 which is movable with the lifting rotary shaft, lowered into the furnace chamber 3 or raised into the valve chamber 13.
- the bottom of the valve chamber has a sealing cover 17.
- the first rotating unit 1 is rotatably coupled to the positioning rotary shaft 14 via a connecting member 18, and the positioning rotary shaft 14 is fixed by the column 25.
- the second rotating unit 2 includes a lifting rotary shaft 21, a sub-chamber 22, and a valve chamber 23, and the lifting rotary shaft 21 is erected at the center of the wide chamber 23 and a sub-chamber 22, the valve One side of the chamber 23 has a door 26 for the substrate sheet or the entire substrate holder 4 to enter and exit; the lifting rotary shaft 21 is externally connected to a device for controlling the shaft for lifting or rotating Turn to exercise.
- the bottom of the lifting rotary shaft 21 is fixedly coupled or detachably coupled to a substrate holder 4 which is movable with the lifting rotary shaft, lowered into the furnace chamber 3 or raised into the valve chamber 23.
- the second rotary unit 2 is rotatably coupled to the positioning rotary shaft 14 via a connecting member 18, and the positioning rotary shaft 14 is fixed by the column 25.
- the furnace chamber 3 is divided into an upper furnace chamber 31 and a lower furnace chamber 32.
- the substrate piece is placed on the substrate holder 4, which is then fixed to the bottom of the lifting rotary shaft 11. or 21 via a valve 16 or a valve 26.
- the solute and solvent are first charged in ⁇ 33.
- the first rotating unit 1 is rotated above the furnace chamber 3, fixed, the sealing cover 36 of the furnace chamber 3 and the sealing cover 17 under the valve chamber 13 are opened, the furnace chamber 3 is sealingly coupled with the valve chamber 13, and the vacuum is evacuated to 1 (T 4 After Pa, an inert gas is introduced into the furnace chamber 3 and the valve chamber 13.
- the temperature ⁇ 33 is raised to a desired temperature to melt the solute and the solvent.
- the lifting rotary shaft 11 is lowered from the inside of the valve chamber 13 into the furnace chamber 3 to dissolve the substrate holder.
- the substrate piece on the jig is grown to a certain thickness, and the rotating lifting shaft 11 is lifted to raise the jig to the valve chamber 13.
- the furnace chamber 3 and the valve chamber 12 are sealed, and the entire rotating unit 180 is rotated about the rotating shaft 14. °, the first rotating unit 1 is moved away from the furnace chamber 3.
- the second rotating unit 2 is rotated, and the valve chamber 24 of the second rotating unit 2 is filled with a substrate piece to be liquid-phase-extended, and the step of epitaxial growth is repeated.
- the substrate piece that has been epitaxially grown in the first rotating unit 1 is removed after being cooled, and a new substrate piece to be epitaxially grown, such as the lining in the second rotating unit 2 is loaded.
- the epitaxial wafer is epitaxially grown, it is separated from the upper portion of the furnace chamber, and the first rotating unit 1 is transferred to the upper portion of the furnace chamber to repeat the epitaxial growth operation, so that the continuous substrate sheet epitaxial growth is repeated.
- the present invention can also be designed as three independent rotating units as needed, and the substrate sheets on the jig are sequentially fed into the furnace for epitaxial growth.
- Embodiment 2 is different from Embodiment 1 in that the doors 16 and 26 are not provided in the valve chambers 13, 23 of the first rotating unit 1 and the second rotating unit 2.
- the bottom sealing cover 17 of the rotating unit 1, 2 and the sealing cover 36 of the furnace chamber 3 are of a circular pull type.
- the sealing cover 17 can be opened, and the lifting and rotating shaft 11 can be rotated downward until the substrate piece and the jig 4 protrudes out of the valve chamber 13, which can be conveniently completed.
- Embodiment 3, as shown in Fig. 6, differs from Embodiment 2 in that the bottom seal cover 17 of the rotary unit 1, 2 and the seal cover 36 of the furnace chamber 3 are of a square pull type.
- the invention discloses a method and a device for preparing a film by continuous liquid phase epitaxy, and is designed with two independent rotating units, and the epitaxial growth of the second batch can be carried out without taking out the epitaxial growth epitaxial wafer after the furnace chamber is sufficiently cooled. Therefore, the time of each liquid phase epitaxy can be shortened, the energy consumption can be saved, and the use efficiency of the liquid phase epitaxy furnace is greatly improved.
Abstract
A method and an apparatus for preparing thin films by using continuous liquid phase epitaxy are provided, which conduct the liquid phase epitaxial growth using a device with at least two rotation units (1, 2). Substrates can conduct an alternating operation of epitaxial growth in the rotation units (1, 2), and after each operation of the epitaxial growth, it is not needed to wait for the complete cooling of the chamber (3).Then the substrates can be raised up into one of the rotation units and cooled down after leaving the top of the chamber (3), at the same time, the second batch of the substrates in the other rotation units are rotated into the chamber (3), and then the second batch of epitaxial growth operation is conducted therein.
Description
一种连续液相外延法制备薄膜的方法和装置 技术领域 Method and device for preparing thin film by continuous liquid phase epitaxy
本发明涉及一种液相外延方法及装置，特别涉及一种连续液相外延法制备薄膜的方法 和装置。 . 背景技术 The present invention relates to a liquid phase epitaxy method and apparatus, and more particularly to a method and apparatus for preparing a thin film by continuous liquid phase epitaxy. . Background technique
外延生长是半导体材料和器件制造的一项重要工艺。在单晶衬底上从饱和溶液中生长 外延层的方法称液相外延 (LPE) 。 例如， GaAs外延层就可从以 Ga为溶剂、 As为溶质的饱 和溶液中生长出来。 液相外延方法是在 1963年由纳尔逊 (Nelson)提出的。 Epitaxial growth is an important process in the fabrication of semiconductor materials and devices. The method of growing an epitaxial layer from a saturated solution on a single crystal substrate is called liquid phase epitaxy (LPE). For example, a GaAs epitaxial layer can be grown from a saturated solution in which Ga is a solvent and As is a solute. The liquid phase epitaxy method was proposed by Nelson in 1963.
液相外延技术的出现，对于化合物半导体材料和器件的发展起了重要的推动作用。 目 前这一技术已广泛用于生长 GaAs、 GaAlAs、 GaP、 InP、 Ga InAsP等半导体材料和制作发 光二极管、 激光二极管、 太阳能电池、 微波器件等。 The emergence of liquid phase epitaxy has played an important role in the development of compound semiconductor materials and devices. Currently, this technology has been widely used to grow semiconductor materials such as GaAs, GaAlAs, GaP, InP, Ga InAsP, and to manufacture light-emitting diodes, laser diodes, solar cells, microwave devices, and the like.
液相外延的方法之一是采用液相外延炉， 衬底夹具位于炉中。然而， 传统的液相外延 炉， 每次操作时， 衬底生长后， 只能等衬底片在炉内完全冷却后才能取出， 再进行下一次 操作。在此期间炉内的溶剂也先冷却一再重新加热， 大量能量在冷却过程中被浪费， 并且 由于冷却所需的时间长， 每次操作的时间也长， 炉室利用效率不高。 发明内容 One of the methods of liquid phase epitaxy is to use a liquid phase epitaxy furnace in which the substrate holder is located. However, in the conventional liquid phase epitaxy furnace, after each substrate operation, after the substrate is grown, it can only be taken out after the substrate sheet is completely cooled in the furnace, and then the next operation is performed. During this time, the solvent in the furnace is also cooled and reheated first, a large amount of energy is wasted during the cooling process, and the time required for cooling is long, the operation time is long, and the furnace chamber utilization efficiency is not high. Summary of the invention
本发明的目的在于针对液相外延法制备外延薄膜时，衬底片和溶剂冷却时间过长而设 计一种可连续液相外延的方法及外延设备。 SUMMARY OF THE INVENTION The object of the present invention is to provide a method and an epitaxial device for continuous liquid phase epitaxy in the preparation of an epitaxial film by liquid phase epitaxy, in which the substrate sheet and the solvent are cooled for a long time.
本发明的技术方案如下： The technical solution of the present invention is as follows:
一种连续液相外延法制备薄膜的方法， 使用一种至少具两个旋转单元的设备， 其特征 在于： 该方法包括： A method for preparing a thin film by continuous liquid phase epitaxy using a device having at least two rotating units, the method comprising:
A、 在炉室的坩埚内加入熔料， 在第一旋转单元中的衬底夹具中装入衬底片； A, adding a melt in the crucible of the furnace chamber, and loading the substrate sheet in the substrate holder in the first rotating unit;
B、 第一旋转单元转至炉室上方， 打开炉室上方及旋转单元的密封盖， 下降衬底夹具 认 本 /
至炉室内， 进行液相外延操作； B. The first rotating unit is turned to the upper part of the furnace chamber, and the sealing cover above the furnace chamber and the rotating unit is opened, and the substrate holder is lowered. Go to the furnace chamber for liquid phase epitaxy;
C、 外延生长完成， 上升衬底夹具至第一旋转单元， 然后炉室上方及旋转单元的密封 盖各自封 | ， 第一旋转单元离开炉室上方； C, epitaxial growth is completed, the substrate holder is raised to the first rotating unit, and then the sealing cover above the furnace chamber and the rotating unit are respectively sealed |, the first rotating unit is separated from the furnace chamber;
D、 在第一旋转单元中的衬底片进行外延生长的同时， 在第二旋转单元中的衬底夹具 中装入衬底片； D. loading the substrate sheet in the substrate holder in the second rotating unit while the substrate sheet in the first rotating unit is epitaxially grown;
E、 第一旋转单元离开炉室上方后， 第二旋转单元转至炉室上方， 重复第一旋转单元 的操作， 进行外延生长。 E. After the first rotating unit leaves the furnace chamber, the second rotating unit is turned over the furnace chamber, and the operation of the first rotating unit is repeated to perform epitaxial growth.
该方法进一步包括： 第二旋转单元进行外延生长的同时， 卸下第一旋转单元内已外延 生长的衬底片， 并装入新的待外延生长的衬底片， 等第二旋转单元内的衬底片完成外延生 长后，第二旋转单元离开炉室上方，第一旋转单元转至炉室上方，重新重复外延生长动作， 如此反复重复进行连续的衬底片外延生长。 The method further includes: while the second rotating unit performs epitaxial growth, removing the epitaxially grown substrate piece in the first rotating unit, and loading a new substrate piece to be epitaxially grown, such as a substrate piece in the second rotating unit After the epitaxial growth is completed, the second rotating unit leaves the furnace chamber, the first rotating unit is turned over the furnace chamber, and the epitaxial growth operation is repeated, so that the continuous substrate sheet epitaxial growth is repeated repeatedly.
一种连续外延的液相外延法制备薄膜的装置， 包括一个炉室和至少两个旋转单元， 其 特征在于： 所述的旋转单元与炉室为可分离式， 旋转单元可通过旋转， 定位于炉室上方或 离开炉室上方。 The invention relates to a device for preparing a film by liquid phase epitaxy of continuous epitaxy, comprising a furnace chamber and at least two rotating units, wherein: the rotating unit and the furnace chamber are separable, and the rotating unit can be rotated and positioned Above the furnace chamber or above the furnace chamber.
所述的旋转单元包括一阀室、 一升降旋转轴及一副室， 阀室用于容纳衬底夹具。 所述的升降旋转轴底部与衬底夹具连接。 The rotating unit includes a valve chamber, a lifting rotating shaft and a sub-chamber for accommodating the substrate holder. The bottom of the lifting and rotating shaft is connected to the substrate holder.
还包括至少两个的定位旋转轴， 所述的旋转单元绕定位旋转轴旋转。 Also included is at least two positioning rotation axes that rotate about the positioning rotation axis.
所述的旋转单元可沿定位旋转轴上下移动。每个旋转单元的阀室底部都具有可移开式 密封盖， 当移至炉室上时， 密封盖可移开， 供阀室与炉室相通， 当离开炉室时， 密封盖可 被重新封于阀室底部。 The rotating unit is movable up and down along the positioning rotation axis. The bottom of the valve chamber of each rotary unit has a removable sealing cover. When moving to the furnace chamber, the sealing cover can be removed, and the valve chamber communicates with the furnace chamber. When leaving the furnace chamber, the sealing cover can be re-opened. Sealed at the bottom of the valve chamber.
所述的炉室分为上炉室与下炉室，所述的上炉室顶部具有密封盖， 当阀室移至炉室上 时， 该上炉室的密封盖可移开， 供阀室与炉室相通， 当离开炉室时， 该上炉室的密封盖可 被重新封于炉室顶部。 阀室底部的密封盖与炉室顶部的密封盖互相配合，使高温的衬底片 可始终被隔绝于一封闭空间内， 以被惰性气体保护。 The furnace chamber is divided into an upper furnace chamber and a lower furnace chamber, and the top of the upper furnace chamber has a sealing cover. When the valve chamber is moved to the furnace chamber, the sealing cover of the upper furnace chamber can be removed, and the valve chamber is provided. Communicating with the furnace chamber, the sealing cover of the upper furnace chamber can be resealed to the top of the furnace chamber when leaving the furnace chamber. The sealing cap at the bottom of the valve chamber cooperates with the sealing cap at the top of the furnace chamber so that the high temperature substrate sheet can always be isolated in a closed space to be protected by an inert gas.
从以上描述可知， 发明使用一种至少具两个旋转单元的设备进行液相外延生长， 衬底 片可在旋转单元中轮流进行外延操作， 每次操作完毕， 不必等炉室完全冷却， 即可将衬底
片上升至其中的一个旋转单元内， 离开炉室上方进行冷却， 同时将另一旋转单元内第二批 次的衬底片转入炉室， 进行第二批次的液相外延操作， 如此重复， 消除了现有技术炉室必 须冷却后再重新升温， 能量大量 费的弊端， 本发明的方法及设备可缩短每次液相外延的 时间， 大大提髙了液相外延炉的使用效率。 附图说明 As can be seen from the above description, the invention uses a device having at least two rotating units for liquid phase epitaxial growth, and the substrate sheet can be subjected to epitaxial operation in a rotating unit, and each time the operation is completed, the furnace chamber can be completely cooled without waiting for the furnace chamber to be completely cooled. Substrate The sheet is raised into one of the rotating units, and is cooled above the furnace chamber, and the second batch of the substrate sheet in the other rotating unit is transferred into the furnace chamber, and the second batch of liquid phase epitaxy is performed, and thus repeated. The method and the device of the invention can shorten the time of each liquid phase epitaxy, and greatly improve the use efficiency of the liquid phase epitaxy furnace, which eliminates the disadvantage that the prior art furnace chamber must be cooled and then reheated, and the energy is greatly increased. DRAWINGS
图 1 为本发明一种连续外延的液相外延法制备薄膜的装置的立体结构示意图； 图 2为本发明一种连续外延的液相外延法制备薄膜的装置的顶视图； 1 is a schematic perspective view of a device for preparing a thin film by a liquid crystal epitaxy method of continuous epitaxy according to the present invention; FIG. 2 is a top view of a device for preparing a thin film by a liquid phase epitaxy method of continuous epitaxy according to the present invention;
图 3为本发明其中一个旋转单元旋转至炉室上方， 互相配合的示意图； Figure 3 is a schematic view showing one of the rotating units of the present invention rotated to the top of the furnace chamber to cooperate with each other;
图 4、 为本发明一种连续外延的液相外延法制备薄膜的装置的实施例 2结构示意图； 图 5、 实施例 2的旋转单元及炉室的密封盖结构示意图； 4 is a schematic structural view of Embodiment 2 of a device for preparing a thin film by a liquid crystal epitaxial method according to the present invention; FIG. 5 is a schematic structural view of a sealing unit of a rotary unit and a furnace chamber of Embodiment 2;
图 6、 实施例 3的旋转单元及炉室的密封盖结构示意图。 具体实施方式 Fig. 6 is a schematic view showing the structure of the sealing unit of the rotary unit and the furnace chamber of the third embodiment. detailed description
实施例 1、 如图 1至图 3所示， 一种连续外延的液相外延法制备薄膜的装置， 包括： 第一旋转单元 1和第二旋转单元 2， 以及炉室 3。 Embodiment 1. As shown in Figs. 1 to 3, a device for preparing a film by a liquid phase epitaxy method of continuous epitaxy, comprising: a first rotating unit 1 and a second rotating unit 2, and a furnace chamber 3.
第一旋转单元 1包括一升降旋转轴 11、 一副室 12及一阀室 13， 升降旋转轴 11竖立 设置在阀室 13及副室 12的中心； 阀室 13的一面有一门 16， 用于衬底片或整个衬底夹具 的进出； 升降旋转轴 11上部外接一控制装置， 控制该轴作升降或旋转运动。 升降旋转 轴 11底部固定连接或可拆卸地连接一衬底夹具 4， 该衬底夹具 4可随升降旋转轴运动， 降入炉室内 3内或上升至阀室 13内。 阀室底部具有密封盖 17。 The first rotating unit 1 includes a lifting and lowering rotating shaft 11, a sub-chamber 12 and a valve chamber 13 which are erected at the center of the valve chamber 13 and the sub-chamber 12; one side of the valve chamber 13 has a door 16 for The substrate piece or the entire substrate holder enters and exits; a control device is externally connected to the upper part of the lifting and rotating shaft 11, and the axis is controlled to perform lifting or rotating motion. The bottom of the lifting rotary shaft 11 is fixedly connected or detachably coupled to a substrate holder 4 which is movable with the lifting rotary shaft, lowered into the furnace chamber 3 or raised into the valve chamber 13. The bottom of the valve chamber has a sealing cover 17.
第一旋转单元 1通过连接件 18与定位旋转轴 14转动连接， 定位旋转轴 14通过立柱 25固定。 The first rotating unit 1 is rotatably coupled to the positioning rotary shaft 14 via a connecting member 18, and the positioning rotary shaft 14 is fixed by the column 25.
与第一旋转单元 1类似， 第二旋转单元 2包括一升降旋转轴 21、 一副室 22及一阀室 23, 升降旋转轴 21竖立设置在其阔室 23及一副室 22的中心， 阀室 23的一面有一门 26， 用于衬底片或整个衬底夹具 4的进出； 升降旋转轴 21外接一装置， 控制该轴作升降或旋
转运动。 升降旋转轴 21底部固定连接或可拆卸地连接一衬底夹具 4， 该衬底夹具 4可随 升降旋转轴运动， 降入炉室内 3内或上升至阀室 23内。 Similar to the first rotating unit 1, the second rotating unit 2 includes a lifting rotary shaft 21, a sub-chamber 22, and a valve chamber 23, and the lifting rotary shaft 21 is erected at the center of the wide chamber 23 and a sub-chamber 22, the valve One side of the chamber 23 has a door 26 for the substrate sheet or the entire substrate holder 4 to enter and exit; the lifting rotary shaft 21 is externally connected to a device for controlling the shaft for lifting or rotating Turn to exercise. The bottom of the lifting rotary shaft 21 is fixedly coupled or detachably coupled to a substrate holder 4 which is movable with the lifting rotary shaft, lowered into the furnace chamber 3 or raised into the valve chamber 23.
第二旋转单元 2通过连接件 18与定位旋转轴 14转动连接， 定位旋转轴 14通过立柱 25固定。 The second rotary unit 2 is rotatably coupled to the positioning rotary shaft 14 via a connecting member 18, and the positioning rotary shaft 14 is fixed by the column 25.
同时参见图 1及图 3， 炉室 3分为上炉室 31及下炉室 32， 上炉室 31上方有一密封盖 (图中未显示)； 下炉室 32内有一坩埚 33用于液相外延生长； 石墨坩埚 33外有一石墨加 热器 35， 用于加热石墨坩埚； 石墨加热器 35连接电极 34。 Referring to FIG. 1 and FIG. 3, the furnace chamber 3 is divided into an upper furnace chamber 31 and a lower furnace chamber 32. Above the upper furnace chamber 31, there is a sealing cover (not shown); and a lower chamber 32 has a crucible 33 for liquid phase. Epitaxial growth; a graphite heater 35 outside the graphite crucible 33 for heating the graphite crucible; and a graphite heater 35 connected to the electrode 34.
使用时， 将衬底片安置于衬底夹具 4， 衬底夹具 4再经阀门 16或阀门 26固定于升降 旋转轴 11.或 21底部。 在坩埚 33中先装入溶质和溶剂。 将第一旋转单元 1旋转至炉室 3 上方， 固定， 炉室 3的密封盖 36和阀室 13下的密封盖 17打开， 炉室 3与阀室 13密封联 接，抽真空至 l(T4Pa后往炉室 3和阀室 13内通入惰性气体。升温坩埚 33至所需温度使溶 质和溶剂熔解。升降旋转轴 11由阀室 13内下降至炉室 3内， 使衬底夹具溶于熔液中。 降 温， 待夹具上的衬底片生长至一定厚度， 提升旋转升降轴 11， 使夹具上升至阀室 13。 密 封炉室 3和阀室 12， 绕旋转轴 14旋转整个旋转单元 180° ， 使第一旋转单元 1离开炉室 3上方。 同时旋转第二旋转单元 2， 该第二旋转单元 2的阀室 24内装有待液相外延的衬底 片， 重复前面外延生长的步骤。 In use, the substrate piece is placed on the substrate holder 4, which is then fixed to the bottom of the lifting rotary shaft 11. or 21 via a valve 16 or a valve 26. The solute and solvent are first charged in 坩埚33. The first rotating unit 1 is rotated above the furnace chamber 3, fixed, the sealing cover 36 of the furnace chamber 3 and the sealing cover 17 under the valve chamber 13 are opened, the furnace chamber 3 is sealingly coupled with the valve chamber 13, and the vacuum is evacuated to 1 (T 4 After Pa, an inert gas is introduced into the furnace chamber 3 and the valve chamber 13. The temperature 坩埚 33 is raised to a desired temperature to melt the solute and the solvent. The lifting rotary shaft 11 is lowered from the inside of the valve chamber 13 into the furnace chamber 3 to dissolve the substrate holder. In the molten metal, the substrate piece on the jig is grown to a certain thickness, and the rotating lifting shaft 11 is lifted to raise the jig to the valve chamber 13. The furnace chamber 3 and the valve chamber 12 are sealed, and the entire rotating unit 180 is rotated about the rotating shaft 14. °, the first rotating unit 1 is moved away from the furnace chamber 3. At the same time, the second rotating unit 2 is rotated, and the valve chamber 24 of the second rotating unit 2 is filled with a substrate piece to be liquid-phase-extended, and the step of epitaxial growth is repeated.
第二旋转单元 2进行外延生长的同时，待冷却后卸下第一旋转单元 1内已外延生长的 衬底片，并装入新的待外延生长的衬底片，等第二旋转单元 2内的衬底片完成外延生长后， 离开炉室上方， 第一旋转单元 1转至炉室上方， 重新重复外延生长动作， 如此反复进行连 续的衬底片外延生长。 While the second rotating unit 2 performs epitaxial growth, the substrate piece that has been epitaxially grown in the first rotating unit 1 is removed after being cooled, and a new substrate piece to be epitaxially grown, such as the lining in the second rotating unit 2 is loaded. After the epitaxial wafer is epitaxially grown, it is separated from the upper portion of the furnace chamber, and the first rotating unit 1 is transferred to the upper portion of the furnace chamber to repeat the epitaxial growth operation, so that the continuous substrate sheet epitaxial growth is repeated.
本发明根据需要也可以设计为三个独立的旋转单元 ， 依次将夹具上的衬底片送入炉 内进行外延生长。 The present invention can also be designed as three independent rotating units as needed, and the substrate sheets on the jig are sequentially fed into the furnace for epitaxial growth.
实施例 2， 如附图 4、 图 5所示， 与实施例 1不同之处在于， 第一旋转单元 1、 第二 旋转单元 2的阀室 13、 23上， 均没有设置门 16、 26。 旋转单元 1、 2的底部密封盖 17及 炉室 3的密封盖 36为圆形抽拉式。 衬底片及夹具 4的取放时可打开密封盖 17， 将升降旋 转轴 11向下旋转， 至衬底片及夹具 4伸出阀室 13, 即可方便的完成。
实施例 3, 如图 6所示， 与实施例 2不同之处在于旋转单元 1、 2的底部密封盖 17及 炉室 3的密封盖 36为方形抽拉式。 Embodiment 2, as shown in FIG. 4 and FIG. 5, is different from Embodiment 1 in that the doors 16 and 26 are not provided in the valve chambers 13, 23 of the first rotating unit 1 and the second rotating unit 2. The bottom sealing cover 17 of the rotating unit 1, 2 and the sealing cover 36 of the furnace chamber 3 are of a circular pull type. When the substrate piece and the jig 4 are picked up and lowered, the sealing cover 17 can be opened, and the lifting and rotating shaft 11 can be rotated downward until the substrate piece and the jig 4 protrudes out of the valve chamber 13, which can be conveniently completed. Embodiment 3, as shown in Fig. 6, differs from Embodiment 2 in that the bottom seal cover 17 of the rotary unit 1, 2 and the seal cover 36 of the furnace chamber 3 are of a square pull type.
工业实用性 Industrial applicability
本发明一种连续液相外延法制备薄膜的方法及装置， 设计有两个独立的旋转单元， 无 需等炉室充分冷却才取出外延生长的外延片， 就可进行第二次批次的外延生长， 所以， 可 缩短每次液相外延的时间， 节省能量消耗， 大大提髙了液相外延炉的使用效率。
The invention discloses a method and a device for preparing a film by continuous liquid phase epitaxy, and is designed with two independent rotating units, and the epitaxial growth of the second batch can be carried out without taking out the epitaxial growth epitaxial wafer after the furnace chamber is sufficiently cooled. Therefore, the time of each liquid phase epitaxy can be shortened, the energy consumption can be saved, and the use efficiency of the liquid phase epitaxy furnace is greatly improved.
Claims
权利要求 Rights request
1、 一种连续液相外延法制备薄膜的方法， 使用一种至少具两个旋转单元的设备， 其特征 在于： 该方法包括： A method of preparing a film by continuous liquid phase epitaxy, using a device having at least two rotating units, the method comprising:
A、 在炉室的坩埚内加入熔料， 在第一旋转单元中的衬底夹具中装入衬底片； A, adding a melt in the crucible of the furnace chamber, and loading the substrate sheet in the substrate holder in the first rotating unit;
B、 第一旋转单元转至炉室上方， 打开炉室上方及旋转单元的密封盖， 下降衬底夹具 至炉室内， 进行液相外延操作； B. The first rotating unit is turned to the upper of the furnace chamber, the sealing cover above the furnace chamber and the rotating unit is opened, and the substrate holder is lowered to the furnace chamber for liquid phase epitaxy operation;
C、 外延生长完成， 上升衬底夹具至第一旋转单元， 然后炉室上方及旋转单元的密封 盖各自封闭， 第一旋转单元离开炉室上方； C, epitaxial growth is completed, the substrate holder is raised to the first rotating unit, and then the sealing cover above the furnace chamber and the rotating unit are respectively closed, and the first rotating unit is separated from the furnace chamber;
D、 在第一旋转单元中的衬底片进行外延生长的同时， 在第二旋转单元中的衬底夹具 中装入衬底片； D. loading the substrate sheet in the substrate holder in the second rotating unit while the substrate sheet in the first rotating unit is epitaxially grown;
E、 第一旋转单元离开炉室上方后， 第二旋转单元转至炉室上方， 重复第一旋转单元 的操作， 进行外延生长。 E. After the first rotating unit leaves the furnace chamber, the second rotating unit is turned over the furnace chamber, and the operation of the first rotating unit is repeated to perform epitaxial growth.
2、 如权利要求 1所述的一种连续液相外延法制备薄膜的方法， 其特征在于： 该方法进一 步包括： 第二旋转单元进行外延生长的同时， 待冷却后卸下第一旋转单元内已完成外延生 长的衬底片， 并装入新的待外延生长的衬底片， 等第二旋转单元内的衬底片完成外延生长 后， 第二旋转单元离开炉室上方， 第一旋转单元转至炉室上方， 重新重复外延生长动作， 如此反复重复进行连续的衬底片外延生长。 2. The method for preparing a thin film by continuous liquid phase epitaxy according to claim 1, wherein the method further comprises: removing the first rotating unit after the second rotating unit performs epitaxial growth while being cooled; The epitaxially grown substrate piece has been completed, and a new substrate piece to be epitaxially grown is loaded. After the substrate piece in the second rotating unit is epitaxially grown, the second rotating unit leaves the furnace chamber, and the first rotating unit is transferred to the furnace. Above the chamber, the epitaxial growth operation is repeated, and the continuous epitaxial growth of the substrate piece is repeated repeatedly.
3、 如权利要求 1所述的一种连续液相外延法制备薄膜的方法， 其特征在于： 该方法 B步 骤包括： 第一旋转单元与炉室密封联接， 抽真空至 10—4Pa后， 向炉室和阀室内通入惰性气 体； 升温坩埚至所需温度使溶质和溶剂熔解； 升降旋转轴 11下降， 使衬底夹具溶于熔液 中。 3, a continuous liquid phase process as claimed in claim 1 Preparation of epitaxial films Method, characterized in that: the method step B comprising: a first rotation unit coupled to the furnace chamber is sealed after evacuated to 10- 4 Pa, An inert gas is introduced into the furnace chamber and the valve chamber; the temperature is raised to a desired temperature to melt the solute and the solvent; and the lifting rotary shaft 11 is lowered to dissolve the substrate holder in the melt.
4、 一种连续液相外延法制备薄膜的装置， 包括一个炉室 （3)和至少两个旋转单元 （1) (2)， 所述的旋转单元（1 ) (2)通过旋转， 定位于炉室（3)上方或离开炉室（3)上方； 旋转单元 （1) (2)均可分别与炉室 （3)密封联接。 4. A device for preparing a film by continuous liquid phase epitaxy, comprising a furnace chamber (3) and at least two rotating units (1) (2), wherein the rotating unit (1) (2) is located by rotation Above or away from the furnace chamber (3); the rotating units (1) (2) can each be sealingly coupled to the furnace chamber (3).
5、 如权利要求 3所述的一种连续液相外延法制备薄膜的装置， 其特征在于： 所述的旋转 单元（1 ) 包括一阀室（13)、 一升降旋转轴 （11 )及一副室 （12), 升降旋转轴 （11 ) 竖
立设置在其阀室 （13)及一副室 （12) 的中心。 5. The apparatus for preparing a film by continuous liquid phase epitaxy according to claim 3, wherein: the rotating unit (1) comprises a valve chamber (13), a lifting rotary shaft (11) and a Sub-chamber (12), lifting shaft (11) vertical The column is disposed at the center of its valve chamber (13) and a pair of chambers (12).
6、 如权利要求 5所述的一种连续液相外延法制备薄膜的装置， 其特征在于： 所述的升降 旋转轴 （11 )底部连接一衬底夹具 （4)。 6. A device for preparing a thin film by continuous liquid phase epitaxy according to claim 5, wherein: the bottom of the lifting and rotating shaft (11) is connected to a substrate holder (4).
7、 如权利要求 4所述的一种连续液相外延法制备薄膜的装置， 其特征在于： 还包括至少 两个的定位旋转轴（14) (24), 所述的旋转单元（1) (2)分别与两个的定位旋转轴（14) 7. The apparatus for preparing a thin film by continuous liquid phase epitaxy according to claim 4, further comprising: at least two positioning rotating shafts (14) (24), said rotating unit (1) ( 2) Positioning rotation axis with two (14)
(24)转动连接， 可绕定位旋转轴 （14) (24) 旋转。 (24) Rotate the connection to rotate around the positioning rotary axis (14) (24).
8、 如权利要求 7所述的一种连续液相外延法制备薄膜的装置， 其特征在于： 所述的旋转 单元 （1 )可沿定位旋转轴（14)上下移动。 8. A device for preparing a thin film by continuous liquid phase epitaxy according to claim 7, wherein: said rotating unit (1) is movable up and down along a positioning rotary axis (14).
9、 如权利要求 4所述的一种连续液相外延法制备薄膜的装置， 其特征在于： 每个旋转单 元 （1) (2) 的阀室 （13) (23)底部都具有可移开式密封盖（17) (27)。 9. A device for preparing a film by continuous liquid phase epitaxy according to claim 4, wherein: the bottom of each of the valve chambers (13) (23) of each of the rotary units (1) (2) is removable Sealing cap (17) (27).
10、如权利要求 4所述的一种连续液相外延法制备薄膜的装置， 其特征在于： 所述的 炉室（3)分为上炉室（31)与下炉室（32)， 所述的上炉室（32)顶部具有密封盖（33)。
10. A device for preparing a film by continuous liquid phase epitaxy according to claim 4, wherein: said furnace chamber (3) is divided into an upper furnace chamber (31) and a lower furnace chamber (32). The top of the upper furnace chamber (32) has a sealing cover (33).
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| CN200910111527.0 | 2009-04-17 | ||
| CN200910111527A CN101760775A (en) | 2009-04-17 | 2009-04-17 | Method and device for preparing thin film by continuous liquid phase epitaxial method |
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| CN114752997A (en) * | 2022-04-25 | 2022-07-15 | 哈尔滨工业大学 | Double-crucible liquid phase epitaxial growth device |
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| CN103526281B (en) * | 2013-09-29 | 2016-05-11 | 青岛赛瑞达电子装备股份有限公司 | Vertical solution phase epitaxy stove |
| CN103526282A (en) * | 2013-10-22 | 2014-01-22 | 北京大学东莞光电研究院 | Device and method for growing nitride single-crystal material |
| CN113897667A (en) * | 2021-09-28 | 2022-01-07 | 北京科技大学 | Equipment and method for growing bismuth-tellurium-based alloy epitaxial film |
| CN115074820B (en) * | 2022-06-17 | 2023-07-18 | 哈尔滨工业大学 | Double-crucible liquid phase epitaxy preparation method of single crystal RIG thick film |
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