CN100395373C - Growth Equipment for Chemical Vapor Deposition - Google Patents

Growth Equipment for Chemical Vapor Deposition Download PDF

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CN100395373C
CN100395373C CNB2006100392361A CN200610039236A CN100395373C CN 100395373 C CN100395373 C CN 100395373C CN B2006100392361 A CNB2006100392361 A CN B2006100392361A CN 200610039236 A CN200610039236 A CN 200610039236A CN 100395373 C CN100395373 C CN 100395373C
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casing
quartz tube
reaction chamber
wall
radio frequency
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CN1834286A (en
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韩平
赵红
谢自力
王荣华
王�琦
夏冬梅
修向前
张�荣
郑有炓
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Nanjing University
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化学气相淀积的生长设备,采用射频感应加热,射频感应加热器中间设有石墨反应腔,石墨反应腔置于真空石英管(1)内,在石英管与被感应加热的石墨反应腔(3)之间设有耐高温的热解BN套管(2)组。BN套管组为2-6只套管,套管壁间距、套管壁与石英管壁间距是1mm-10mm。利用多层BN套管组作为辐射蔽罩、有效地降低热辐射所致的能量损失。BN材料导热率低,可实现100℃/mm以上的温度梯度,具有良好的保温效果。石英管内维持较高真空,BN套管之间、BN套管与石英管之间为真空,有助于减少热量损失。

Figure 200610039236

The chemical vapor deposition growth equipment adopts radio frequency induction heating, and a graphite reaction chamber is arranged in the middle of the radio frequency induction heater, and the graphite reaction chamber is placed in a vacuum quartz tube (1). ) is provided with a high temperature resistant pyrolysis BN casing (2) group. The BN casing group consists of 2-6 casings, and the distance between the casing wall and the casing wall and the quartz tube wall is 1mm-10mm. The multi-layer BN sleeve group is used as a radiation shield to effectively reduce the energy loss caused by heat radiation. BN material has low thermal conductivity and can achieve a temperature gradient above 100°C/mm, which has a good thermal insulation effect. A relatively high vacuum is maintained in the quartz tube, and vacuum is maintained between the BN sleeves and between the BN sleeve and the quartz tube, which helps to reduce heat loss.

Figure 200610039236

Description

化学气相淀积的生长设备 Growth Equipment for Chemical Vapor Deposition

技术领域 technical field

本发明涉及制备CVD材料的生长设备的设计,尤其是热解BN套管组作为保温装置的制备CVD材料的生长设备。The invention relates to the design of growth equipment for preparing CVD materials, in particular to the growth equipment for preparing CVD materials with pyrolysis BN casing group as heat preservation device.

背景技术 Background technique

第三代半导体、宽带隙材料具有优异的光电性能,在通讯、信息领域具有广泛的应用。化学气相淀积(CVD)方法是外延生长宽带隙半导体薄膜材料的常用的方法之一。The third-generation semiconductors and wide-bandgap materials have excellent photoelectric properties and are widely used in the fields of communication and information. The chemical vapor deposition (CVD) method is one of the commonly used methods for epitaxially growing wide bandgap semiconductor thin film materials.

SiC、GaN等薄膜材料的外延生长都是在高温下实现的,SiC的生长温度为1300~1600℃,GaN的生长温度为1000~1200℃,所采用的CVD材料生长设备的加热装置应具有优良的保温性能,这样就既能满足材料制备的要求、也能实现低能耗的节能目标。The epitaxial growth of thin film materials such as SiC and GaN is realized at high temperature. The growth temperature of SiC is 1300~1600°C, and that of GaN is 1000~1200°C. The heating device of the CVD material growth equipment used should have excellent Excellent thermal insulation performance, so that it can not only meet the requirements of material preparation, but also achieve the energy-saving goal of low energy consumption.

目前,用于SiC薄膜材料制备的CVD材料的外延设备的加热方式大多采用射频感应加热。由于生长温度高达1300~1600℃,为避免石英管软化,在石英管与被感应加热的石墨反应腔之间需要有耐高温的高纯度保温材料,为得到高质量的外延材料、还需要保证在高温生长过程中没有杂质自保温材料向反应腔内逸出。At present, most of the heating methods of epitaxial equipment for CVD materials used in the preparation of SiC thin film materials use radio frequency induction heating. Since the growth temperature is as high as 1300~1600°C, in order to avoid softening of the quartz tube, a high-temperature resistant high-purity insulation material is required between the quartz tube and the graphite reaction chamber heated by induction. In order to obtain high-quality epitaxial materials, it is also necessary to ensure that the During the high-temperature growth process, no impurities escape from the insulation material into the reaction chamber.

传统的卧式CVD设备是采用石墨毡来实现耐高温保温功能的。此方法的缺陷是:The traditional horizontal CVD equipment uses graphite felt to realize the function of high temperature resistance and heat preservation. The disadvantages of this method are:

1、石墨毡为多孔状。1. Graphite felt is porous.

易吸附杂质,而不易进行清洗,也不易根据需要进行装配的调整及组合。一定使用期后不能保证在高温生长过程中无杂质逸出。It is easy to absorb impurities, but it is not easy to clean, and it is not easy to adjust and combine assembly according to needs. After a certain period of use, it cannot be guaranteed that no impurities will escape during high temperature growth.

2、石墨毡不能自支撑。2. Graphite felt cannot support itself.

不易在立式CVD设备中使用,而无此配置的CVD设备需要具有较大尺寸的石英腔体,并在石英管壁上附加水冷或气冷夹套管,以保证外延生长过程中管壁处于较低的温度。这样的设备成本高、功耗大。It is not easy to use in vertical CVD equipment, and CVD equipment without this configuration needs to have a larger size quartz chamber, and a water-cooled or air-cooled jacketed tube is attached to the quartz tube wall to ensure that the tube wall is at a constant temperature during the epitaxial growth process. lower temperature. Such devices are expensive and consume a lot of power.

发明内容 Contents of the invention

本发明目的是提出一种制备CVD材料的生长设备的设计,尤其是热解BN套管组作为保温装置的制备CVD材料的生长设备。The object of the present invention is to propose a design for the growth equipment for preparing CVD materials, especially the growth equipment for preparing CVD materials with pyrolysis BN casing set as the heat preservation device.

本发明目的是这样实现的:CVD材料的外延设备,采用射频感应加热,射频感应加热器中间设有石墨反应腔,石墨反应腔置于真空石英管内,其特征是在石英管与被感应加热的石墨反应腔之间设有耐高温的热解BN套管组。The object of the present invention is achieved like this: the epitaxy equipment of CVD material adopts radio frequency induction heating, and the middle of radio frequency induction heater is provided with graphite reaction cavity, and graphite reaction cavity is placed in the vacuum quartz tube, it is characterized in that quartz tube and induction heated A high temperature resistant pyrolysis BN sleeve set is arranged between the graphite reaction chambers.

所述热解BN套管组至少包括两只套管,如2-6只套管构成套管组,套管壁间距、套管壁与石英管壁间距≥1mm,小于10mm。套管壁的厚度为0.2-8mm。The pyrolytic BN casing set includes at least two casings, for example, 2-6 casings constitute the casing set, and the distance between the casing walls and the distance between the casing walls and the quartz pipe walls is ≥1mm and less than 10mm. The thickness of the casing wall is 0.2-8 mm.

本发明尤其是用于在卧式CVD材料生长设备中采用热解BN套管组作为保温装置。The invention is especially used for adopting pyrolysis BN casing group as the heat preservation device in the horizontal CVD material growth equipment.

本发明的机理是:热解BN物质具有高熔点、高绝热性、高纯度、高致密度、长寿命、不易吸附杂质、易清洗等显著特点。按材料性能最佳方案是选用壁厚大于5mm的热解BN套管,以使管壁温度降至常规要求的600℃以下,但此方案的成本极高、且目前加工水平尚难以实现。The mechanism of the present invention is that the pyrolyzed BN material has remarkable characteristics such as high melting point, high heat insulation, high purity, high density, long life, difficult to absorb impurities, and easy cleaning. According to the material properties, the best solution is to use pyrolysis BN casing with a wall thickness greater than 5mm to reduce the temperature of the tube wall to below the conventional requirement of 600°C. However, the cost of this solution is extremely high, and the current processing level is still difficult to achieve.

本发明方案的特点是:The feature of the present invention's scheme is:

1、利用多层BN套管组作为辐射蔽罩、有效地降低热辐射所致的能量损失。1. Use the multi-layer BN bushing group as a radiation shield to effectively reduce the energy loss caused by thermal radiation.

2、BN材料导热率低,可实现100℃/mm以上的温度梯度,具有良好的保温效果。2. BN material has low thermal conductivity, can realize temperature gradient above 100°C/mm, and has good heat preservation effect.

3、石英管内维持较高真空,BN套管之间、BN套管与石英管之间为真空,因此沿石英管径向的热导率低,有助于减少热量损失。3. The quartz tube maintains a relatively high vacuum, and there is a vacuum between the BN sleeves and between the BN sleeve and the quartz tube, so the thermal conductivity along the radial direction of the quartz tube is low, which helps to reduce heat loss.

4、保证在高温生长过程中没有杂质自保温材料向反应腔内逸出,得到高质量的外延材料。4. Ensure that no impurities escape from the insulation material into the reaction chamber during the high-temperature growth process, and obtain high-quality epitaxial materials.

附图说明 Description of drawings

图1是本发明的截面结构示意图,图中标志:石英管1(最外圈)、三层BN套管2、石墨反应腔3、外延基片生长台4(中央矩形)。其中箭头方向表示热辐射方向,箭头密度表示热辐射强度Fig. 1 is the cross-sectional structure schematic diagram of the present invention, mark among the figure: quartz tube 1 (outer circle), three-layer BN sleeve pipe 2, graphite reaction chamber 3, epitaxial substrate growth platform 4 (central rectangle). The direction of the arrow indicates the direction of heat radiation, and the density of the arrow indicates the intensity of heat radiation

具体实施方式 Detailed ways

如图所示,加热和保温装置包括如下结构:As shown in the figure, the heating and heat preservation device includes the following structure:

加热装置,采用射频感应加热,射频感应加热器中间设有石墨反应腔,石墨反应腔置于真空石英管内。在石英管与被感应加热的石墨反应腔之间设有耐高温的热解BN套管组。The heating device adopts radio frequency induction heating, and a graphite reaction chamber is arranged in the middle of the radio frequency induction heater, and the graphite reaction chamber is placed in a vacuum quartz tube. A high temperature-resistant pyrolytic BN sleeve set is arranged between the quartz tube and the induction heated graphite reaction chamber.

射频感应加热炉:功率30~40KW,频率40KHZ左右。RF induction heating furnace: power 30~40KW, frequency about 40KHZ.

石墨反应腔(加热件):中空,尺寸按外延基片直径设计。Graphite reaction chamber (heating element): hollow, the size is designed according to the diameter of the epitaxial substrate.

保温装置,BN套管组:套管数大于2,本实施例中选择三层,较厚的管子选择二层也有较好的效果。要求保温效果好的时候,可以选择四层或更多层数的管。Insulation device, BN casing group: the number of casings is greater than 2, three layers are selected in this embodiment, and two layers are also better for thicker pipes. When good insulation effect is required, pipes with four or more layers can be selected.

套管长度为加热件长度的2-3倍,套管间距、套管与石英管间距≥1mm,套管间、套管与石英管用BN环隔离、支撑,内套管中置加热件(石墨反应腔3、外延基片生长台4)在上述反应腔内,外套管置于石英管中。The length of the casing is 2-3 times the length of the heating element, the spacing between the casing and the distance between the casing and the quartz tube is ≥1mm, the space between the casings, the casing and the quartz tube are isolated and supported by BN rings, and the heating element (graphite) is placed in the inner casing Reaction chamber 3, epitaxial substrate growth platform 4) In the above reaction chamber, the outer tube is placed in the quartz tube.

本发明方案采用的BN套管壁厚选用目前加工水平所能够实现的BN厚度,目前的热解BN套管的加工方法是:聚合物先驱体热解法制备或低成本燃烧合成工艺制备的氮化硼基陶瓷(上海硅酸盐所、哈尔滨工业大学复合材料研究所等采用),目前热解BN套管套管壁的厚度为0.2-2mm。通过组合、装配实现保温,可以保证在高温生长过程中无杂质逸出,同时具有令人满意的性能价格比和较低的制造成本。壁厚大的BN套管的效果更好。The BN bushing wall thickness that the present invention scheme adopts selects the BN thickness that can realize at present processing level, and the processing method of present pyrolysis BN bushing is: the nitrogen that polymer precursor pyrolysis method prepares or the low-cost combustion synthesis process prepares Boron-based ceramics (used by Shanghai Institute of Ceramics, Institute of Composite Materials, Harbin Institute of Technology, etc.), currently the thickness of the casing wall of the pyrolytic BN casing is 0.2-2mm. Insulation is achieved through combination and assembly, which can ensure that no impurities escape during the high-temperature growth process, and meanwhile have satisfactory performance-price ratio and low manufacturing cost. The effect of thicker BN casing is better.

本发明方案的优点还包括:The advantage of the scheme of the present invention also includes:

1、由于可以方便地实行装配的组合和调整,因此该套装置既能在高温下进行SiC、GaN等宽带隙半导体薄膜材料的外延生长,也能在较低温度下实现Si基材料(Si1-xGex、Si1-x-yGexCy等)的外延生长。1. Since the combination and adjustment of assembly can be conveniently implemented, this set of equipment can not only carry out epitaxial growth of SiC, GaN and other wide-bandgap semiconductor thin film materials at high temperature, but also realize Si-based materials (Si 1 -x G x , Si 1-xy G x C y, etc.) epitaxial growth.

2、BN套管组保温装置的有效保温效果,可使CVD材料生长设备的功耗明显降低;2. The effective heat preservation effect of the heat preservation device of the BN casing group can significantly reduce the power consumption of the CVD material growth equipment;

3、热解BN可以实现自支撑,既可用于卧式CVD材料生长设备,也可用于立式CVD材料生长设备,因而可以有效降低立式CVD材料生长设备的制造成本、技术难度和使用功耗。3. Pyrolytic BN can be self-supporting, and can be used in both horizontal CVD material growth equipment and vertical CVD material growth equipment, thus effectively reducing the manufacturing cost, technical difficulty and power consumption of vertical CVD material growth equipment .

本发明方案在卧式CVD材料生长设备中已实现的技术指标:The technical index that the scheme of the present invention has realized in the horizontal CVD material growth equipment:

高温生长温度范围:800~1400℃,生长时石英管外壁温度<600℃(风冷);低温生长温度范围:550~850℃,生长时石英管外壁温度<200℃(风冷)。High temperature growth temperature range: 800~1400°C, the temperature of the outer wall of the quartz tube during growth is <600°C (air cooling); low temperature growth temperature range: 550~850°C, the temperature of the outer wall of the quartz tube is less than 200°C (air cooling).

Claims (1)

1.化学气相淀积的生长设备,采用射频感应加热,射频感应加热器中间设有石墨反应腔,石墨反应腔置于真空石英管(1)内,其特征是在石英管与被感应加热的石墨反应腔(3)之间设有耐高温的热解BN套管(2)组;所述BN套管组为2-6只套管,套管壁间距、套管壁与石英管壁间距是1mm-10mm;套管壁的厚度为0.2-8mm;套管长度为加热件石墨反应腔(3)长度的2-3倍,套管壁间、套管与石英管用BN环隔离、支撑。1. The growth equipment of chemical vapor deposition adopts radio frequency induction heating, and a graphite reaction chamber is arranged in the middle of the radio frequency induction heater, and the graphite reaction chamber is placed in a vacuum quartz tube (1). A high temperature resistant pyrolytic BN casing (2) group is arranged between the graphite reaction chambers (3); the BN casing group consists of 2-6 casings, the distance between the casing wall and the distance between the casing wall and the quartz pipe wall It is 1mm-10mm; the thickness of the casing wall is 0.2-8mm; the length of the casing is 2-3 times the length of the graphite reaction chamber (3) of the heating element, and the casing wall, casing and quartz tube are isolated and supported by BN rings.
CNB2006100392361A 2006-03-31 2006-03-31 Growth Equipment for Chemical Vapor Deposition Expired - Fee Related CN100395373C (en)

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CN102465333B (en) * 2010-11-18 2015-04-15 南京大学 Vertical hydride vapor phase epitaxy growth system
CN103184514B (en) * 2013-04-11 2016-07-06 中国科学院苏州纳米技术与纳米仿生研究所 crystal growing furnace
CN103924208B (en) * 2014-04-17 2016-08-24 史永贵 A kind of method preparing multi-layer graphene thin film
CN107740183A (en) * 2017-10-12 2018-02-27 北京大学 A kind of high temperature clean chamber system and method suitable for AlN crystal growths

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CN1052874A (en) * 1988-10-06 1991-07-10 罗纳·布朗克化学公司 Boron nitrogen polymers, their preparation and use as boron nitride precursors
CN2429528Y (en) * 2000-06-16 2001-05-09 烽火通信科技股份有限公司 Preheating furnace for producing preformed products for optical fibers
WO2001061070A1 (en) * 2000-02-18 2001-08-23 G.T. Equipment Technologies Inc. Method and apparatus for chemical vapor deposition of polysilicon

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Publication number Priority date Publication date Assignee Title
CN1052874A (en) * 1988-10-06 1991-07-10 罗纳·布朗克化学公司 Boron nitrogen polymers, their preparation and use as boron nitride precursors
WO2001061070A1 (en) * 2000-02-18 2001-08-23 G.T. Equipment Technologies Inc. Method and apparatus for chemical vapor deposition of polysilicon
CN2429528Y (en) * 2000-06-16 2001-05-09 烽火通信科技股份有限公司 Preheating furnace for producing preformed products for optical fibers

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