CN1320157C - Chemical vapor deposition method of integrating heating and depositing of silicon slices - Google Patents
Chemical vapor deposition method of integrating heating and depositing of silicon slices Download PDFInfo
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Abstract
涉及一种集硅片加热沉积于一体的化学气相沉积方法。其步骤为：将硅片置于电极上，抽真空，启动硅片微区加热控制器电源，直接以硅片为加热装置，设定硅片温度，通入或加入反应物，反应物在硅片表面反应，生成产物；以硅片作为基底，使反应产物在硅片表面沉积。采用可程控硅片加热控制装置，克服了硅片作为加热器负载的缺点，采用硅片直接发热方式，不仅可操作温度范围宽(常温～1200℃)、温度控制灵活、温度变化迅速(大于200℃/S)，温度控制准确(温度波动小于5℃)，增强了可重复性。而且由于硅片体积小，不仅节约能源与实验空间，还可以在同一体系内放置多硅片并独立控制其各自温度，这就大大拓宽了CVD方法的灵活性。It relates to a chemical vapor deposition method which integrates heating and deposition of silicon wafers. The steps are: place the silicon wafer on the electrode, vacuumize, start the power supply of the silicon wafer micro-zone heating controller, directly use the silicon wafer as the heating device, set the temperature of the silicon wafer, feed or add the reactant, and the reactant is in the silicon The reaction on the surface of the wafer produces products; the silicon wafer is used as the substrate to deposit the reaction product on the surface of the silicon wafer. The programmable silicon chip heating control device overcomes the shortcomings of the silicon chip as a heater load. The direct heating method of the silicon chip not only has a wide operating temperature range (normal temperature to 1200 ° C), flexible temperature control, and rapid temperature changes (greater than 200 °C/S), accurate temperature control (temperature fluctuation less than 5 °C), enhanced repeatability. Moreover, due to the small size of the silicon wafer, not only energy and experimental space are saved, but also multiple silicon wafers can be placed in the same system and their respective temperatures can be controlled independently, which greatly broadens the flexibility of the CVD method.
Description
(1)技术领域(1) Technical field
本发明涉及一种集硅片加热沉积于一体的化学气相沉积(CVD)实验方法。The invention relates to a chemical vapor deposition (CVD) experimental method integrating heating and deposition of silicon wafers.
(2)背景技术(2) Background technology
化学气相沉积(CVD)是利用气态物质在一固体表面进行化学反应，生成固态沉积物的过程，是近10年发展起来的制备无机新材料的新技术。它已广泛地用于物质的提纯、新晶体的研制，各种单晶、多晶、玻璃态无机薄膜或涂层的沉积等诸多领域。在上述方法中，无论是热解反应、化学合成反应，还是化学运输反应，温度控制都是一个重要的条件。而许多反应都集中在1200℃以下，管式炉则是最普遍被采样的一种加热方式。但基于管式炉设计上的特点，存在一些自身难以克服的缺点，如功耗大(多数为2000W)、能量利用率低；热容大、温度变化缓慢；产物效率低；中心温区温度受真空度、气体流速等多种因素的影响，温度控制不准确，且由中心向两端温度逐渐降低。这与现在合成实验的环保化、微量化、精准化、高转化率等趋势都不相适应，尤其是对需要快速温交、温度控制精准的CVD实验体系，更是管式炉的致命弱点。Chemical vapor deposition (CVD) is a process in which gaseous substances undergo chemical reactions on a solid surface to form solid deposits. It is a new technology for the preparation of new inorganic materials developed in the past 10 years. It has been widely used in the purification of substances, the development of new crystals, the deposition of various single crystal, polycrystalline, glassy inorganic thin films or coatings, and many other fields. In the above methods, whether it is pyrolysis reaction, chemical synthesis reaction, or chemical transport reaction, temperature control is an important condition. Many reactions are concentrated below 1200 °C, and the tube furnace is the most commonly sampled heating method. However, based on the characteristics of the design of the tube furnace, there are some shortcomings that are difficult to overcome, such as large power consumption (mostly 2000W), low energy utilization rate; large heat capacity, slow temperature change; low product efficiency; the temperature in the central temperature zone is affected. Influenced by various factors such as vacuum degree and gas flow rate, the temperature control is not accurate, and the temperature gradually decreases from the center to both ends. This is not compatible with the trend of environmental protection, miniaturization, precision, and high conversion rate of synthesis experiments, especially for CVD experimental systems that require fast temperature transfer and precise temperature control, which is the Achilles heel of tube furnaces.
(3)发明内容(3) Contents of the invention
本发明的目的在于提供一种直接采用硅片作为加热器和化学气相沉积基底，可通过程序灵活控制硅片温度，可实现快速温度变化(大于200℃/S)、集硅片加热沉积于一体的化学气相沉积方法。此外还可在一个体系内同时引入多个硅片并独立控制各自温度，建立多种材料的复合化学气相沉积方法。The purpose of the present invention is to provide a silicon chip directly used as a heater and a chemical vapor deposition substrate, which can flexibly control the temperature of the silicon chip through a program, can realize rapid temperature change (greater than 200°C/S), and integrates silicon chip heating and deposition chemical vapor deposition method. In addition, multiple silicon wafers can be introduced into one system at the same time and their respective temperatures can be controlled independently to establish a composite chemical vapor deposition method for multiple materials.
集硅片加热沉积于一体的化学气相沉积方法的步骤为：The steps of the chemical vapor deposition method integrating heating and deposition of silicon wafers are:
1)裁取所需尺寸的硅片，并置于反应装置的两电极上；1) Cut a silicon wafer of required size and place it on the two electrodes of the reaction device;
2)抽真空，真空度视反应物及产物在空气中的稳定性而定；2) vacuuming, the degree of vacuum depends on the stability of the reactants and products in the air;
3)启动硅片微区加热控制器电源，直接以硅片为加热装置，设定硅片温度，数值由具体化学沉积反应要求的反应温度确定；3) Start the power supply of the silicon wafer micro-zone heating controller, directly use the silicon wafer as the heating device, and set the temperature of the silicon wafer. The value is determined by the reaction temperature required by the specific chemical deposition reaction;
4)通入或加入反应物；4) Passing or adding reactants;
5)反应物在硅片表面发生化学反应，生成产物；5) The reactant undergoes a chemical reaction on the surface of the silicon wafer to generate a product;
6)以硅片作为反应物沉积的基底，使反应产物在硅片表面沉积；6) using the silicon wafer as the substrate for the deposition of the reactant, so that the reaction product is deposited on the surface of the silicon wafer;
7)关闭硅片微区加热控制器电源，关闭抽真空系统；7) Turn off the power supply of the silicon wafer micro-zone heating controller, and turn off the vacuum system;
8)将硅片取出，对获得的沉积产物进行性能测试。8) Taking out the silicon wafer, and performing a performance test on the obtained deposition product.
由于硅片其结构的特殊性以及高温下的稳定性，常作为化学气相沉积基底。但硅片特殊的温度特性(低温时为半导体，高温下为导体，从室温到1200℃，电阻变化接近四个数量级)，使其很少直接用于加热(加热电源难以适应如此大的负载变化)，而多采用被动加热方式，这就产生上述的种种问题。而本发明采用可程控硅片加热控制装置，克服了硅片作为加热器负载的缺点，抛弃了常规管式炉的间接加热方式(即通过控制管式炉温度从而间接控制化学气相沉积基底——硅片的温度)，而采用硅片自身直接发热方式，不仅可操作温度范围宽(常温～1200℃)、温度控制灵活(可手调或程控)、温度变化迅速(大于200℃/S)，温度控制准确(温度波动小于5℃)，增强了实验的可重复性。而且由于硅片体积小，不仅节约能源(管式炉为2000W，本发明为240W)与实验空间，还可以在同一体系内放置多硅片并独立控制其各自温度，这就大大拓宽了CVD方法的灵活性。再则，在采用管式炉方式下，热由外往内传，必须先经过外层玻璃反应管，如果硅片需要加热到1000℃，外层的玻璃反应管就必须承受高于1000℃的高温，只能选用高价的石英管；而采用本发明的硅片自热试验体系，硅片达到1000℃时，外层玻璃反应管受硅片热辐射达到的温度不高于400℃，完全可以使用普通玻璃管，节约了试验成本，而且给反应管形状加工带来许多方便；又由于本发明中，玻璃管壁温度远低于硅片温度，反应物只能在硅片表面发生反应并沉积，硅片表面获得沉积产物的效率提高；另外，在采用管式炉加热方式的CVD试验中，由于反应管置于管式炉内，反应的实际情况无法观察，而采用本方法，整个反应过程都可以透过玻璃管直接观测，这也给试验带了方便。Due to the particularity of its structure and the stability at high temperature, silicon wafers are often used as chemical vapor deposition substrates. However, the special temperature characteristics of silicon wafers (semiconductor at low temperature and conductor at high temperature, and the resistance change is close to four orders of magnitude from room temperature to 1200°C) make it rarely used for heating directly (heating power supply is difficult to adapt to such a large load change) ), and more passive heating methods are used, which produces the above-mentioned problems. However, the present invention adopts a programmable silicon chip heating control device, overcomes the shortcoming of the silicon chip as a heater load, and abandons the indirect heating method of the conventional tube furnace (that is, indirectly controls the chemical vapor deposition substrate by controlling the temperature of the tube furnace—— The temperature of the silicon wafer), and the direct heating method of the silicon wafer itself, not only has a wide operating temperature range (normal temperature to 1200°C), flexible temperature control (manually or program-controlled), and rapid temperature changes (greater than 200°C/S), Accurate temperature control (temperature fluctuation is less than 5°C), which enhances the repeatability of the experiment. And because silicon chip volume is little, not only save energy (tube furnace is 2000W, the present invention is 240W) and experiment space, can also place multi-silicon chip in the same system and control its respective temperature independently, and this has just broadened CVD method greatly flexibility. Furthermore, in the tube furnace method, heat is transmitted from the outside to the inside, and must first pass through the outer glass reaction tube. If the silicon wafer needs to be heated to 1000°C, the outer glass reaction tube must withstand a temperature higher than 1000°C. High temperature, only high-priced quartz tubes can be used; while using the silicon wafer self-heating test system of the present invention, when the silicon wafer reaches 1000 °C, the temperature reached by the outer glass reaction tube under the heat radiation of the silicon wafer is not higher than 400 °C, which is completely acceptable. The use of ordinary glass tubes saves test costs and brings convenience to the processing of the shape of the reaction tube; and because the temperature of the glass tube wall is much lower than that of the silicon wafer in the present invention, the reactants can only react and deposit on the surface of the silicon wafer , the efficiency of obtaining deposition products on the surface of the silicon wafer is improved; in addition, in the CVD test using the tube furnace heating method, because the reaction tube is placed in the tube furnace, the actual situation of the reaction cannot be observed, but with this method, the entire reaction process All can be directly observed through the glass tube, which also brings convenience to the experiment.
以下给出本发明与常规管式炉加热的CVD方法的性能比较表：
(4)附图说明(4) Description of drawings
图1为本发明与常规管式炉加热方法的一般化学气相沉积反应过程比较图。在图1中，(a)为本发明，(b)为常规管式炉加热方法；1为反应物，2为产物，3为玻璃管壁，4为硅片。Fig. 1 is a comparison diagram of the general chemical vapor deposition reaction process between the present invention and the conventional tube furnace heating method. In Fig. 1, (a) is the present invention, (b) is conventional tube furnace heating method; 1 is a reactant, 2 is a product, 3 is a glass tube wall, and 4 is a silicon chip.
(5)具体实施方式(5) specific implementation
首先必须设计一个内含两电极，能轻松更换两电极上的硅片，并可抽真空、可通入反应气的玻璃反应装置。电极两端用引线引至真空体系外，并连接至可程控硅片微区加热控制器。First of all, it is necessary to design a glass reaction device that contains two electrodes, can easily replace the silicon wafers on the two electrodes, and can be vacuumed and the reaction gas can be introduced. The two ends of the electrode are led out of the vacuum system with lead wires, and connected to the programmable silicon chip micro-zone heating controller.
然后裁取所需尺寸的硅片，并置于反应装置的两电极上；抽真空，真空度视反应物及产物在空气中的稳定性而定，多采用机械泵(少数化学气相沉积也可在空气中直接进行)；启动硅片微区加热控制器电源，设定好硅片温度；通入或加入反应物；反应物在硅片表面发生化学反应，生成产物；反应产物在硅片表面沉积；关闭硅片微区加热控制器电源和真空系统电源；将硅片取出，对获得的沉积产物进行性能测试。Then cut out the required size of the silicon wafer, and place it on the two electrodes of the reaction device; vacuumize, the degree of vacuum depends on the stability of the reactants and products in the air, and mechanical pumps are mostly used (a small number of chemical vapor deposition can also be used) directly in the air); start the power supply of the silicon wafer micro-zone heating controller, set the temperature of the silicon wafer; feed or add reactants; the reactants react chemically on the surface of the silicon wafer to generate products; the reaction products are on the surface of the silicon wafer Deposition; turn off the power supply of the silicon wafer micro-zone heating controller and the power supply of the vacuum system; take out the silicon wafer, and perform a performance test on the obtained deposition product.
如图1所示，本发明的反应一般过程如图1(a)流程：As shown in Figure 1, the reaction general process of the present invention is shown in Figure 1 (a) flow process:
A.反应物迁移到发热硅片表面；A. The reactant migrates to the surface of the heating silicon wafer;
B.反应物在硅片表面反应，转换为产物；B. The reactant reacts on the surface of the silicon wafer and converts it into a product;
C.产物在硅片表面沉积(少数在管壁沉积)。C. The product is deposited on the surface of the silicon wafer (a few are deposited on the tube wall).
图1(b)为常规管式炉加热方式下的一般反应过程：Fig. 1 (b) is the general reaction process under the conventional tube furnace heating mode:
D.反应物迁移至硅片及玻璃管壁表面；D. The reactant migrates to the surface of the silicon wafer and the glass tube wall;
E.反应物在玻璃管壁和硅片表面转化为产物；E. Reactants are converted into products on the glass tube wall and silicon wafer surface;
F.产物在玻璃管壁和硅片表面沉积。F. The product is deposited on the glass tube wall and the surface of the silicon wafer.
比较上述两反应过程，在采用管式炉加热方式下，由于玻璃反应管温度高于硅片，故反应物可以在硅片表面反应，也可以在玻璃管壁反应。且硅片面积远小于玻璃反应管内壁面积，故在硅片表面获得沉积产物为少数，反应效率比较低。而在本试验方法中，玻璃管壁温度远低于硅片表面温度，反应物只能在硅片表面进行反应，大部分反应产物将直接在硅片表面沉积，只有极少数迁移至玻璃管壁沉积，故本方法能获得较高的产率。Comparing the above two reaction processes, in the tube furnace heating mode, since the temperature of the glass reaction tube is higher than that of the silicon wafer, the reactants can react on the surface of the silicon wafer or on the wall of the glass tube. Moreover, the area of the silicon wafer is much smaller than the area of the inner wall of the glass reaction tube, so few deposition products are obtained on the surface of the silicon wafer, and the reaction efficiency is relatively low. In this test method, the temperature of the glass tube wall is much lower than the surface temperature of the silicon wafer, and the reactants can only react on the surface of the silicon wafer. Most of the reaction products will be directly deposited on the surface of the silicon wafer, and only a few migrate to the glass tube wall. deposition, so this method can obtain a higher yield.
实施例1：硅片表面纳米SnO2阵列的制取Embodiment 1: the preparation of nano SnO2 array on silicon chip surface
裁取20mm×5mm的硅片，将其固定在电极上，启动机械泵抽真空，待真空稳定后，启动硅片微区加热控制装置，设定温度为800℃，以四氯化碳气体为缓冲，缓缓通入SnH4气体，等反应结束后，关闭硅片微区加热控制装置电源及机械泵电源，取出硅片。即可在硅片表面获得SnO2纳米阵列。该阵列排列整齐，数量很多，在电境下如连绵稻苗状。控制不同的SnH4气体浓度以及硅片温度，还可以得到如菊花状等多种形状的纳米颗粒。Cut out a 20mm×5mm silicon wafer, fix it on the electrode, start the mechanical pump to evacuate, and after the vacuum is stable, start the silicon wafer micro-zone heating control device, set the temperature at 800°C, and use carbon tetrachloride gas as the Buffer, slowly introduce SnH 4 gas, after the reaction is over, turn off the power supply of the silicon wafer micro-zone heating control device and the power supply of the mechanical pump, and take out the silicon wafer. The SnO 2 nanometer array can be obtained on the surface of the silicon wafer. The arrays are neatly arranged and numerous in number, like continuous rice seedlings in an electric environment. By controlling different SnH 4 gas concentrations and silicon wafer temperatures, nanoparticles of various shapes such as chrysanthemum shapes can also be obtained.
实施例2：硅片表面Mo2O3纳米带的制取Embodiment 2: Preparation of Mo 2 O 3 nanobelts on silicon wafer surface
裁取20mm×5mm的硅片，将其固定在电极上，启动机械泵抽真空，待真空稳定后，启动硅片微区加热控制装置，设定温度为1000℃，将金属钼粉末置于硅片表面加热气化并沉积(可在抽真空前，预先置于硅片表面)，等反应结束后，关闭硅片微区加热控制装置电源及机械泵电源，取出硅片。即可获得氧化钼纳米带，在电境下观察，带的长、宽、厚度之比约100∶10∶1。此外还获得许多其他形状的纳米氧化钼颗粒。Cut out a 20mm×5mm silicon wafer, fix it on the electrode, start the mechanical pump to evacuate, and after the vacuum is stable, start the silicon wafer micro-zone heating control device, set the temperature at 1000°C, and place the metal molybdenum powder on the silicon The surface of the wafer is heated, vaporized and deposited (it can be placed on the surface of the silicon wafer before vacuuming). After the reaction is completed, turn off the power supply of the silicon wafer micro-zone heating control device and the power supply of the mechanical pump, and take out the silicon wafer. The molybdenum oxide nanobelt can be obtained, and the ratio of the length, width and thickness of the ribbon is about 100:10:1 when observed under electric conditions. In addition, many other shapes of nanomolybdenum oxide particles were obtained.
实施例3：硅片表面纳米金颗粒的制取(本发明的扩展应用)Embodiment 3: Preparation of nano-gold particles on the surface of silicon wafer (extended application of the present invention)
传统的硅片表面纳米金颗粒制取需要用多孔硅，而要把直接购买来的单晶硅圆片(非多孔硅)制成多孔硅并不简单。本方法利用该新加热技术温度变化迅速的特点，先在5mm×20mm的硅片表面喷金，而后将硅片固定在电极上，启动硅片微区加热控制器电源，设定温度在1100℃，达到温度后切断电源，硅片迅速降温退火，即可在硅片表面获得20～100nm的金颗粒，而且金颗粒分布很均匀，相互间不相连。控制喷金的厚度和退火温度，还可以获得粒径不同的金颗粒。大小颗粒直径比一般不大于5/2。从而给其它的CVD试验做了很好的铺垫。Porous silicon is required for the preparation of traditional gold nanoparticles on the surface of silicon wafers, but it is not easy to make porous silicon from directly purchased single crystal silicon wafers (non-porous silicon). This method utilizes the characteristic of rapid temperature change of the new heating technology, first sprays gold on the surface of a 5mm×20mm silicon wafer, then fixes the silicon wafer on the electrode, starts the silicon wafer micro-zone heating controller power supply, and sets the temperature at 1100°C After reaching the temperature, cut off the power supply, quickly cool down and anneal the silicon wafer, and then obtain 20-100nm gold particles on the surface of the silicon wafer, and the gold particles are evenly distributed and not connected to each other. By controlling the thickness and annealing temperature of gold spraying, gold particles with different particle sizes can also be obtained. The ratio of particle size to diameter is generally not more than 5/2. This paves the way for other CVD experiments.
此外本方法用于ZnO2等纳米颗粒的制取，也获得了很好的效果。该方法还进一步被推广至激光化学气相沉积体系、微波等离子化学气相沉积体系等。In addition, this method is used in the preparation of ZnO 2 and other nanoparticles, and good results have also been obtained. This method has been further extended to laser chemical vapor deposition system, microwave plasma chemical vapor deposition system and so on.
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