CN104388910B - High power microwave plasma reaction unit for chemistry for gas phase depositing diamond film - Google Patents
High power microwave plasma reaction unit for chemistry for gas phase depositing diamond film Download PDFInfo
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 54
- 239000010432 diamond Substances 0.000 title claims abstract description 54
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 27
- 238000000151 deposition Methods 0.000 title claims description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000010453 quartz Substances 0.000 claims abstract description 42
- 230000007246 mechanism Effects 0.000 claims abstract description 22
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- 239000000498 cooling water Substances 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 6
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 claims 6
- 230000003028 elevating effect Effects 0.000 claims 4
- 230000008878 coupling Effects 0.000 abstract description 28
- 238000010168 coupling process Methods 0.000 abstract description 28
- 238000005859 coupling reaction Methods 0.000 abstract description 28
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 12
- 239000012495 reaction gas Substances 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 4
- 238000009827 uniform distribution Methods 0.000 abstract 1
- 239000000758 substrate Substances 0.000 description 31
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- 238000004050 hot filament vapor deposition Methods 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
- H01J37/32192—Microwave generated discharge
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/274—Diamond only using microwave discharges
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/511—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using microwave discharges
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
- H01J37/32192—Microwave generated discharge
- H01J37/32211—Means for coupling power to the plasma
- H01J37/32247—Resonators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
- H01J37/32192—Microwave generated discharge
- H01J37/32211—Means for coupling power to the plasma
- H01J37/32247—Resonators
- H01J37/32256—Tuning means
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Abstract
本发明为一种用于化学气相沉积金刚石膜的高功率微波等离子体反应装置，包括圆柱形谐振腔体，圆柱形谐振腔体分为上、中、下腔体，其中中腔体的直径最小；上腔体的腔顶为圆锥形且上腔体内安装有圆环状石英微波窗口和圆盘状耦合天线；下腔体底部设有总出气孔，下腔体内安装有相互套装的第一圆柱形反射体、第二圆柱形反射体和圆柱形基台，三者分别通过各自的升降机构实现升降动作。本发明装置调节方便，能容纳高的微波功率，对微波的耦合能力及聚焦能力强，反应气体分布均匀，能够以较高的速率制备高纯度的金刚石膜材料。
The invention is a high-power microwave plasma reaction device for chemical vapor deposition of diamond film, comprising a cylindrical resonant cavity, the cylindrical resonant cavity is divided into upper, middle and lower cavities, wherein the diameter of the middle cavity is the smallest ; The roof of the upper cavity is conical and the upper cavity is equipped with a ring-shaped quartz microwave window and a disc-shaped coupling antenna; the bottom of the lower cavity is provided with a total air outlet, and the lower cavity is installed with the first cylinders that fit each other The three-shaped reflector, the second cylindrical reflector and the cylindrical abutment, respectively realize the lifting action through their respective lifting mechanisms. The device of the invention is convenient to adjust, can accommodate high microwave power, has strong coupling ability and focusing ability to microwave, uniform distribution of reaction gas, and can prepare high-purity diamond film material at a relatively high rate.
Description
技术领域 technical field
本发明属于化学气相沉积金刚石膜技术领域，具体是一种用于化学气相沉积金刚石膜的高功率微波等离子体反应装置。 The invention belongs to the technical field of chemical vapor deposition of diamond films, in particular to a high-power microwave plasma reaction device for chemical vapor deposition of diamond films.
背景技术 Background technique
化学气相沉积（CVD）金刚石膜具有硬度高、导热性好、热膨胀系数小、光学和电学性能优异、声传播速度快、介电性能好等众多优点，使它在诸如红外光学窗口、高功率LED、高功率及高频率电子和光电子器件与系统的散热器、高性能抗辐射探测器和传感器等领域有着广泛的应用前景。目前，人们最常用的制备金刚石膜的方法有热丝化学气相沉积法(HFCVD)、直流电弧等离子体喷射化学气相沉积(DC arc plasma jet CVD)法以及微波等离子体化学气相沉积（MPCVD）法三种。在这三种方法中，MPCVD 法的特点在于金刚石膜沉积过程的控制性好、无放电电极的污染，是国际上用于制备高品质金刚石膜的首选方法。但是，MPCVD 法的主要缺点是制备高品质金刚石膜时沉积速率低，导致金刚石膜成本高、价格昂贵，限制了其在多个领域的推广和应用。 Chemical vapor deposition (CVD) diamond film has many advantages such as high hardness, good thermal conductivity, small thermal expansion coefficient, excellent optical and electrical properties, fast sound propagation speed, and good dielectric properties, making it suitable for applications such as infrared optical windows, high-power LEDs, etc. , radiators for high-power and high-frequency electronic and optoelectronic devices and systems, high-performance radiation-resistant detectors and sensors, and other fields have broad application prospects. At present, the most commonly used methods for preparing diamond films are hot wire chemical vapor deposition (HFCVD), direct current arc plasma jet chemical vapor deposition (DC arc plasma jet CVD) and microwave plasma chemical vapor deposition (MPCVD). kind. Among these three methods, MPCVD The method is characterized by good controllability of the diamond film deposition process and no pollution of the discharge electrode. It is the preferred method for preparing high-quality diamond films in the world. However, MPCVD The main disadvantage of this method is that the deposition rate is low when preparing high-quality diamond films, which leads to high cost and high price of diamond films, which limits its promotion and application in many fields.
在MPCVD金刚石膜的制备过程中，等离子体中氢原子的浓度对金刚石膜的品质和沉积速率起着决定性的作用，通过增加功率密度能够提高等离子体中氢原子的浓度。但是，单纯的依靠提高沉积压强，压缩等离子体体积的方法来提高功率密度，会减小所制备的金刚石膜的面积。因此，要兼顾沉积速率和面积就需要在升高沉积压强的同时，增加输入功率，这就需要研究开发能容纳高微波功率的MPCVD装置。 During the preparation of MPCVD diamond film, the concentration of hydrogen atoms in the plasma plays a decisive role in the quality and deposition rate of the diamond film, and the concentration of hydrogen atoms in the plasma can be increased by increasing the power density. However, simply relying on increasing the deposition pressure and compressing the plasma volume to increase the power density will reduce the area of the prepared diamond film. Therefore, in order to balance the deposition rate and area, it is necessary to increase the input power while increasing the deposition pressure, which requires research and development of MPCVD devices that can accommodate high microwave power.
早期的石英管式MPCVD装置，微波聚焦能力较差，同时因使用的石英管直径较小，石英管的刻蚀问题导致其所容许的功率仅为800W左右。在目前人们常使用的几种类型的MPCVD装置中，圆柱谐振腔式MPCVD装置[P.Bachmann, Chemical & Engineering News 67(1989)24]可以容纳较高的功率，但是其主要缺点在于高功率时平板石英玻璃介质窗口附近会产生次生等离子体，造成石英玻璃的刻蚀及能量的分散；石英钟罩式MPCVD装置[P.Bachmann,D.Leers, H.Lydtin, Diamond Relat.Mater. 1(1991)1]和椭球谐振腔式MPCVD装置[M.Funer,C.Wild, P.Koidl, Appl.Phys.Lett. 72(1998)1149]都使用了石英钟罩作为介质窗口，等离子体被约束在石英钟罩内，在较高的功率条件下也无法避免等离子体对钟罩的刻蚀。此外，石英钟罩的使用使装置的反应气体的进、出孔必须设置在沉积基台上，导致气体分布的均匀性较差。 The early quartz tube-type MPCVD devices had poor microwave focusing ability, and the allowable power was only about 800W due to the small diameter of the quartz tube used and the etching problem of the quartz tube. Among the several types of MPCVD devices commonly used by people at present, the cylindrical resonant cavity MPCVD device [P.Bachmann, Chemical & Engineering News 67 (1989) 24] can accommodate higher power, but its main disadvantage is that when the power is high, secondary plasma will be generated near the dielectric window of the flat quartz glass, resulting in the etching of the quartz glass and the dispersion of energy; the quartz bell type MPCVD device [P.Bachmann, D.Leers, H.Lydtin, Diamond Relat. Mater. 1(1991)1] and the ellipsoid resonant cavity MPCVD device [M.Funer, C.Wild, P.Koidl, Appl.Phys.Lett. 72(1998)1149] both used a quartz bell jar as a dielectric window, and the plasma Confined in a quartz bell jar, it is impossible to avoid plasma etching of the bell jar under higher power conditions. In addition, the use of the quartz bell jar makes the inlet and outlet holes of the reaction gas of the device must be arranged on the deposition platform, resulting in poor uniformity of gas distribution.
非圆柱腔圆周天线式MPCVD装置(SekiTechnotron Corp.，http://www.sikitech.biz/.)使用石英环作为介质窗口，圆周天线同时作为基片台，石英环设置在基片台的下方，可以彻底避免等离子体对该窗口的刻蚀。然而，该装置仍存在以下几个缺点：第一，装置在上盖设置了四个进气孔，为使反应气体能够在基片表面均匀分布，在实际中使用了另外一只石英环套在基片台（圆周天线）外侧，由于石英环高于基片台，等离子体仍会对石英环造成刻蚀污染，这成为限制装置提高微波输入功率的因素之一。第二，腔体的高度和基片台（圆周天线）的位置都是固定的，均无法进行调节，缺乏对谐振腔中微波电场和相应产生的等离子体的实时调控手段，而且在使用不同高度的基片沉积时，金刚石膜的均匀性很难保证。第三，由于腔体的结构较复杂，仅能在基片台（圆周天线）和等离子体上方腔体的局部区域设置水冷结构，在进行金刚石膜沉积时过高的腔体温度也成为限制其容纳高微波功率的另一重要因素。第四，石英环窗口安置在沉积台下方，不利于反应腔室内真空度的保持，即不利于金刚石膜品质的提高。 The non-cylindrical cavity circular antenna MPCVD device (SekiTechnotron Corp., http://www.sikitech.biz/.) uses a quartz ring as the dielectric window, and the circular antenna serves as the substrate stage at the same time, and the quartz ring is arranged below the substrate stage. Etching of the window by plasma can be completely avoided. However, this device still has the following disadvantages: first, the device is provided with four air inlets on the upper cover. In order to make the reaction gas evenly distributed on the surface of the substrate, another quartz ring is used in practice. Outside the substrate stage (circumferential antenna), since the quartz ring is higher than the substrate stage, the plasma will still cause etching pollution to the quartz ring, which becomes one of the factors that limit the device to increase the microwave input power. Second, the height of the cavity and the position of the substrate stage (circumferential antenna) are fixed and cannot be adjusted. There is a lack of real-time control means for the microwave electric field and the corresponding plasma generated in the resonator, and when using different heights The uniformity of the diamond film is difficult to guarantee when the substrate is deposited. Third, due to the complex structure of the cavity, water-cooling structures can only be set up in the local area of the cavity above the substrate stage (circumferential antenna) and the plasma, and the excessively high cavity temperature is also a limitation during the deposition of the diamond film. Another important factor in accommodating high microwave power. Fourth, the quartz ring window is placed under the deposition platform, which is not conducive to maintaining the vacuum in the reaction chamber, that is, not conducive to the improvement of the quality of the diamond film.
专利JP 2000-54142A、US20090120366采用了与非圆柱腔圆周天线式MPCVD装置类似的环形介质窗口和圆周天线结构，为增强聚焦能力，圆周天线面对真空腔体的部分设计成凹槽，基台可以通过调节机构上、下移动实现对等离子体的实时调整。这两种装置的缺点是：仅通过升降基台对等离子体进行调整，限制了所使用的基片高度；装置反应气体的进、出孔均设置在腔体底部，导致基片表面的气体分布不均匀，影响金刚石膜的均匀性；装置也存在非圆柱腔圆周天线式MPCVD装置的第四个缺点，即石英环的安放位置不利于反应腔室内真空度的保持。 Patents JP 2000-54142A and US20090120366 use a ring-shaped dielectric window and a circular antenna structure similar to the non-cylindrical cavity circular antenna MPCVD device. In order to enhance the focusing ability, the part of the circular antenna facing the vacuum cavity is designed as a groove, and the abutment can be The real-time adjustment of the plasma is realized by moving the adjustment mechanism up and down. The disadvantages of these two devices are: the plasma is only adjusted by lifting the platform, which limits the height of the substrate used; the inlet and outlet holes of the reaction gas of the device are set at the bottom of the chamber, resulting in gas distribution on the surface of the substrate. Inhomogeneity affects the uniformity of the diamond film; the device also has the fourth shortcoming of the non-cylindrical cavity circular antenna MPCVD device, that is, the placement of the quartz ring is not conducive to maintaining the vacuum in the reaction chamber.
专利CN101864560B采用了与非圆柱腔圆周天线式MPCVD装置相同的结构，即采用圆周天线同时作为基片台和环形的介质窗口。该装置在腔体上部增加了可升降的反射体，能够实现对微波电场和相应产生的等离子体的实时调控；其腔体为圆柱形结构，形状简单，与等离子体相接触的部件均实现了水冷。但是，实际使用时发现这种装置存在三个缺点：一是，与其他装置相比较，对微波电场的聚焦能力较差，相同条件下金刚石膜的沉积速率较低；二是，反应气体的出口设置在真空腔体的一侧，存在由于反应气体分布不均匀造成的金刚石膜均匀性较差的问题；三是，在较高功率条件下使用时，部分能量会分散于反射体中间的小圆柱体上，其表面会出现非晶碳材料的沉积，不利于高品质金刚石膜的制备。另外，这种装置也未解决非圆柱腔圆周天线式MPCVD装置的第四个缺点。 Patent CN101864560B adopts the same structure as the non-cylindrical cavity circular antenna MPCVD device, that is, the circular antenna is used as the substrate stage and the annular dielectric window at the same time. The device adds a liftable reflector on the upper part of the cavity, which can realize real-time control of the microwave electric field and the corresponding plasma; water cooled. However, in actual use, it is found that this device has three disadvantages: first, compared with other devices, the focusing ability of the microwave electric field is poor, and the deposition rate of the diamond film is low under the same conditions; the second is that the outlet of the reaction gas Installed on one side of the vacuum chamber, there is a problem of poor uniformity of the diamond film due to uneven distribution of reactive gases; third, when used under higher power conditions, part of the energy will be dispersed in the small cylinder in the middle of the reflector In bulk, the deposition of amorphous carbon material will appear on the surface, which is not conducive to the preparation of high-quality diamond films. In addition, this device does not solve the fourth disadvantage of the non-cylindrical cavity circular antenna MPCVD device.
专利CN103305816 A将圆周天线设计成半椭球形状，提高了装置对微波电场的聚焦能力；专利103695865A在圆柱形腔体中设置了可移动的圆柱形上腔体以提高聚焦能力，通过调节在上腔体中的反射体的位置实现对微波电场和等离子体的实时调节。这两种装置都设置了全水冷结构，但是均存在非圆柱腔圆周天线式MPCVD装置第二个和第四个缺点，也均存在专利CN101864560B的第二个缺点。 In patent CN103305816 A, the circular antenna is designed into a semi-ellipsoid shape, which improves the focusing ability of the device to the microwave electric field; in patent 103695865A, a movable cylindrical upper cavity is set in the cylindrical cavity to improve the focusing ability. By adjusting the upper The position of the reflector in the cavity realizes the real-time adjustment of the microwave electric field and the plasma. These two devices are all equipped with a fully water-cooled structure, but both have the second and fourth disadvantages of the non-cylindrical cavity circular antenna MPCVD device, and also have the second disadvantage of the patent CN101864560B.
专利CN 103668127 A将圆周天线设计成圆顶形以增强微波能量的聚焦，同时通过金属薄板反射体阻挡微波向反射体顶部传播，使微波更多地聚集于基片上方。装置的可调节圆环状边缘沉积台、腔体及可调节中心沉积台的升降，可以实现对微波电场和等离子体的实时调节，石英环设置在圆周天线的下方提高了装置的真空性能。这种结构的缺点是：首先，金属薄板反射体直接接触等离子体，且板较薄无法通入冷却水，致使其在高功率条件下使用时，常出现由于温度过高而造成的非晶碳材料的沉积；其次，石英环虽然设置在了谐振腔壁形成的狭缝间，但是仍旧直接面对等离子体，高功率条件下因石英环被刻蚀而污染金刚石膜的情况仍然存在；最后，装置没有设计专门的出气孔，反应气体从环形天线上的进气孔进入反应腔以后，只能通过可调节圆环状边缘沉积台与腔体及可调节中心沉积台的缝隙排出。由于装置工作过程中，圆环状边缘沉积台和中心沉积台均需要进行调节，实际使用时很难保证这两处缝隙的尺寸相同，所以整个反应腔体中气体的流动以及基体表面气体分布的均匀性无法保证。 In patent CN 103668127 A, the circular antenna is designed in a dome shape to enhance the focusing of microwave energy, and at the same time, the metal sheet reflector prevents the microwave from propagating to the top of the reflector, so that more microwaves are concentrated on the substrate. The device's adjustable ring-shaped edge deposition platform, cavity and adjustable center deposition platform can be lifted up and down to realize real-time adjustment of microwave electric field and plasma. The quartz ring is placed under the circular antenna to improve the vacuum performance of the device. The disadvantages of this structure are: firstly, the reflector of the thin metal plate directly contacts the plasma, and the plate is too thin to pass into the cooling water, so that when it is used under high power conditions, amorphous carbon often occurs due to excessive temperature. material deposition; secondly, although the quartz ring is set between the slits formed by the resonant cavity wall, it still directly faces the plasma, and the situation of contaminating the diamond film due to the etching of the quartz ring still exists under high power conditions; finally, The device does not have a special air outlet. After the reaction gas enters the reaction chamber from the air inlet on the loop antenna, it can only be discharged through the gap between the adjustable ring-shaped edge deposition table and the cavity and the adjustable center deposition table. Since both the annular edge deposition platform and the central deposition platform need to be adjusted during the working process of the device, it is difficult to ensure that the two gaps have the same size in actual use, so the flow of gas in the entire reaction chamber and the distribution of gas on the surface of the substrate need to be adjusted. Uniformity cannot be guaranteed.
综上所述，截止到目前，人们使用和提出的各种类型的用于化学气相沉积金刚石膜的微波等离子体反应装置，均存在不同的不利于高功率条件下制备高品质金刚石膜的因素，因此迫切需要设计出一种结构和性能完善的高功率反应装置，以满足高品质金刚石膜的快速制备。 In summary, up to now, the various types of microwave plasma reaction devices used and proposed for chemical vapor deposition of diamond films have different factors that are not conducive to the preparation of high-quality diamond films under high-power conditions. Therefore, it is urgent to design a high-power reaction device with complete structure and performance to meet the rapid preparation of high-quality diamond films.
发明内容 Contents of the invention
本发明是为了解决上述现有技术中存在的问题，而提供一种用于化学气相沉积金刚石膜的高功率微波等离子体反应装置。该装置能够克服目前已有的各类反应装置在不同程度上存在的缺少调节机构、介质窗口刻蚀、聚焦能力差、关键部件不易水冷、能量分散、基片表面气体分布不均匀的缺点，因此能够应用于高功率条件下高品质金刚石膜的均匀快速沉积。 The present invention aims to solve the above-mentioned problems in the prior art, and provides a high-power microwave plasma reaction device for chemical vapor deposition of diamond films. This device can overcome the shortcomings of lack of adjustment mechanism, dielectric window etching, poor focusing ability, difficult water cooling of key components, energy dispersion, and uneven gas distribution on the surface of the substrate that exist to varying degrees in the existing various reaction devices. It can be applied to the uniform and rapid deposition of high-quality diamond films under high-power conditions.
本发明是通过如下技术方案实现的： The present invention is achieved through the following technical solutions:
一种用于化学气相沉积金刚石膜的高功率微波等离子体反应装置，包括圆柱形谐振腔体，圆柱形谐振腔体分为上腔体、中腔体和下腔体，中腔体的直径小于上腔体和下腔体的直径；上腔体的腔顶为圆锥形，上腔体内的底部紧贴腔壁安装有圆环状石英微波窗口，圆环状石英微波窗口的上端口设有一圈安装槽，安装槽内安装有圆盘状耦合天线，圆盘状耦合天线的底部中心处设有下凸的圆柱凸台，圆盘状耦合天上线沿其轴线开设有进气孔；下腔体的底部设有总出气孔，下腔体内紧贴腔壁安装有第一圆柱形反射体，第一圆柱形反射体的底面为平面状、顶面为向下沉陷的倒圆台状，第一圆柱形反射体上沿其轴线开设有第一圆筒形安装孔，且在紧邻第一圆筒形安装孔的位置开设有若干出气孔，第一圆筒形安装孔内插装有第二圆柱形反射体，第二圆柱形反射体上沿其轴线开设有第二圆筒形安装孔，第二圆筒形安装孔内插装有圆柱形基台；第一圆柱形反射体、第二圆柱形反射体和圆柱形基台通过各自设置的升降机构能分别实现升降动作； A high-power microwave plasma reaction device for chemical vapor deposition of diamond films, comprising a cylindrical resonant cavity, the cylindrical resonant cavity is divided into an upper cavity, a middle cavity and a lower cavity, and the diameter of the middle cavity is less than The diameter of the upper cavity and the lower cavity; the cavity top of the upper cavity is conical, and the bottom of the upper cavity is close to the cavity wall. A circular quartz microwave window is installed, and the upper port of the circular quartz microwave window is provided with a ring The installation groove, the disk-shaped coupling antenna is installed in the installation groove, the bottom center of the disk-shaped coupling antenna is provided with a convex cylindrical boss, and the disk-shaped coupling antenna line is provided with an air inlet along its axis; the lower cavity There is a total air outlet at the bottom of the lower cavity, and a first cylindrical reflector is installed close to the cavity wall in the lower cavity. A first cylindrical mounting hole is opened on the reflector along its axis, and a number of air outlets are opened at the position close to the first cylindrical mounting hole, and a second cylindrical mounting hole is inserted into the first cylindrical mounting hole. Reflector, the second cylindrical reflector is provided with a second cylindrical mounting hole along its axis, and a cylindrical abutment is inserted in the second cylindrical mounting hole; the first cylindrical reflector, the second cylindrical The reflector and the cylindrical abutment can respectively realize the lifting action through the lifting mechanism provided separately;
上腔体、中腔体、下腔体、圆环状石英微波窗口、圆盘状耦合天线、第一圆柱形反射体、第二圆柱形反射体、圆柱形基台为同轴线设置；圆环状石英微波窗口与上腔体之间、圆环状石英微波窗口与圆盘状耦合天线之间、第一圆柱形反射体与下腔体之间、第一圆柱形反射体与第二圆柱形反射体之间、第二圆柱形反射体与圆柱形基台之间都设有密封圈。 The upper cavity, the middle cavity, the lower cavity, the ring-shaped quartz microwave window, the disc-shaped coupling antenna, the first cylindrical reflector, the second cylindrical reflector, and the cylindrical abutment are coaxially set; Between the ring-shaped quartz microwave window and the upper cavity, between the ring-shaped quartz microwave window and the disc-shaped coupling antenna, between the first cylindrical reflector and the lower cavity, between the first cylindrical reflector and the second cylinder Sealing rings are arranged between the circular reflectors and between the second cylindrical reflector and the cylindrical abutment.
上腔体、中腔体和下腔体共同构成了本发明装置的谐振腔体，上腔体的圆锥形腔顶设计，这种结构能够有效增强微波功率的耦合，降低反射功率。中腔体位于圆环状石英微波窗口与圆柱形基台（圆柱形基台上会形成等离子体）之间，并且中腔体的直径小于上腔体和下腔体的直径（中腔体的直径也小于圆环状石英微波窗口的直径），因此中腔体能够将圆环状石英微波窗口与圆柱形基台上形成的等离子体隔离，避免了等离子体对圆环状石英微波窗口的刻蚀。 The upper cavity, the middle cavity and the lower cavity together constitute the resonant cavity of the device of the present invention, and the conical cavity roof design of the upper cavity can effectively enhance the coupling of microwave power and reduce the reflected power. The middle chamber is located between the annular quartz microwave window and the cylindrical base (on which the plasma will be formed), and the diameter of the middle chamber is smaller than the diameter of the upper and lower chambers (the diameter of the middle chamber The diameter is also smaller than the diameter of the ring-shaped quartz microwave window), so the middle cavity can isolate the ring-shaped quartz microwave window from the plasma formed on the cylindrical pedestal, avoiding the engraving of the plasma on the ring-shaped quartz microwave window eclipse.
通过圆盘状耦合天线的圆盘与圆环状石英微波窗口之间设置的密封圈，使得圆盘状耦合天线以下、下腔体内第一圆柱形反射体以上的这部分空间形成真空反应腔室，圆盘状耦合天线的重力和大气压强的共同作用能够使真空反应腔室保持良好的真空度，有利于高品质金刚石膜的沉积。圆盘状耦合天线底部中心下凸的圆柱凸台和和第一圆柱形反射体的顶面倒圆台状结构，能够极大地提高微波电磁场的聚焦能力。第一圆柱形反射体、第二圆柱形反射体和圆柱形基台都设置有升降机构，三者能够各自改变在下腔体内的高度，这样不但能够实现对下腔体中微波电场和相应等离子体的实时调控，而且在使用不同高度的基片进行金刚石膜沉积时，能够优化调节等离子体的状态，使等离子体始终均匀的分布在基片表面，从而保证金刚石膜沉积的均匀性。本发明装置的进气孔设置在圆盘状耦合天线的轴线上，第一圆柱形反射体上也开设有若干出气孔，第一圆柱形反射体与下腔体之间、第一圆柱形反射体与第二圆柱形反射体之间、第二圆柱形反射体与圆柱形基台之间都设有密封圈，反应气体由进气孔进入反应腔室后，只能通过第一圆柱形反射体的若干出气孔、再经下腔体的总出气孔排出到装置外，这种进出气方式能够保证反应气体在基片表面均匀分布，从而保证所制备金刚石膜的均匀性。 Through the sealing ring provided between the disk of the disk-shaped coupling antenna and the ring-shaped quartz microwave window, the space below the disk-shaped coupling antenna and above the first cylindrical reflector in the lower cavity forms a vacuum reaction chamber , the joint effect of the gravity of the disc-shaped coupling antenna and the atmospheric pressure can keep the vacuum reaction chamber at a good vacuum, which is conducive to the deposition of high-quality diamond films. The convex cylindrical boss at the bottom center of the disc-shaped coupling antenna and the inverted frustum-like structure on the top surface of the first cylindrical reflector can greatly improve the focusing ability of the microwave electromagnetic field. The first cylindrical reflector, the second cylindrical reflector and the cylindrical pedestal are all provided with a lifting mechanism, and the three can respectively change the height in the lower cavity, which can not only realize the control of the microwave electric field and the corresponding plasma in the lower cavity Real-time control, and when using substrates of different heights for diamond film deposition, it can optimize and adjust the plasma state, so that the plasma is always uniformly distributed on the substrate surface, thereby ensuring the uniformity of diamond film deposition. The air inlet of the device of the present invention is arranged on the axis of the disc-shaped coupling antenna, and several air outlets are also provided on the first cylindrical reflector. Between the first cylindrical reflector and the lower cavity, the first cylindrical reflector There are sealing rings between the body and the second cylindrical reflector, and between the second cylindrical reflector and the cylindrical base. After the reaction gas enters the reaction chamber through the air inlet, it can only pass through the first cylindrical reflector. Several gas outlet holes of the body, and then discharged out of the device through the total gas outlet holes of the lower chamber, this gas inlet and outlet method can ensure that the reaction gas is evenly distributed on the substrate surface, thereby ensuring the uniformity of the prepared diamond film.
进一步的，上腔体的圆锥形腔顶的斜边与水平线的夹角为5-20°，圆锥形腔顶设计成这样的角度范围，增强微波功率的耦合、降低反射功率的效果最优异。第一圆柱形反射体上的斜边与水平线的夹角为10-25°，设计成这种角度范围的圆台状，对于微波电磁场的聚焦能力提高最大。 Further, the angle between the hypotenuse of the conical cavity top of the upper cavity and the horizontal line is 5-20°, and the conical cavity top is designed in such an angle range to enhance the coupling of microwave power and reduce the reflection power. The included angle between the hypotenuse on the first cylindrical reflector and the horizontal line is 10-25°, and the conical frustum shape in this angle range is designed to maximize the focusing ability of the microwave electromagnetic field.
上腔体、中腔体、下腔体、圆盘状耦合天线、第一圆柱形反射体及其升降机构、第二圆柱形反射体及其升降机构、圆柱形基台及其升降机构均通过循环冷却水直接冷却。具体是上腔体、中腔体、下腔体、圆盘状耦合天线、第一圆柱形反射体、第二圆柱形反射体、圆柱形基台都设有中空夹层，并设有与中空夹层相通的进、出水口，冷却水由进水口进入再从出水口流出，以此达到冷却的目的。上述循环冷却水系统的设计使得本发明装置能够容纳较高的微波功率。 The upper cavity, the middle cavity, the lower cavity, the disc-shaped coupling antenna, the first cylindrical reflector and its lifting mechanism, the second cylindrical reflector and its lifting mechanism, the cylindrical abutment and its lifting mechanism all pass through The circulating cooling water is directly cooled. Specifically, the upper cavity, the middle cavity, the lower cavity, the disc-shaped coupling antenna, the first cylindrical reflector, the second cylindrical reflector, and the cylindrical abutment are all provided with a hollow interlayer, and are provided with a hollow interlayer Connected water inlet and outlet, cooling water enters from the water inlet and then flows out from the water outlet, so as to achieve the purpose of cooling. The design of the above-mentioned circulating cooling water system enables the device of the present invention to accommodate higher microwave power.
图2为本发明装置的微波电场模拟结果图，从图中可以看出装置只在位于基片上方中有一个幅值最大的电场区域，因此具有很强的聚焦电场的能力；最强电场与石英微波窗口被中腔体隔开，并且石英微波窗口附近没有明显的电场存在，因此可以避免所激发的等离子对该窗口的刻蚀；其他区域电场幅值不足以激发等离子体，这样避免了次生等离子体出现。 Fig. 2 is the microwave electric field simulation result figure of the device of the present invention, as can be seen from the figure that the device only has an electric field region with the largest amplitude in the top of the substrate, so it has a very strong ability to focus the electric field; the strongest electric field and The quartz microwave window is separated by the middle cavity, and there is no obvious electric field near the quartz microwave window, so the etching of the window by the excited plasma can be avoided; the electric field amplitude in other areas is not enough to excite the plasma, thus avoiding secondary Plasma appears.
本发明装置与现有技术相比，具有如下有益效果： Compared with the prior art, the device of the present invention has the following beneficial effects:
1）本发明提出的装置的锥形腔顶，能够有效增强微波功率的耦合，降低反射功率。圆盘状耦合天线上的圆柱形凸台和第一圆柱形反射体的顶面倒圆台状结构，能够极大地提高微波电磁场的聚焦能力； 1) The tapered cavity roof of the device proposed by the present invention can effectively enhance the coupling of microwave power and reduce the reflected power. The cylindrical boss on the disc-shaped coupling antenna and the top surface of the first cylindrical reflector can greatly improve the focusing ability of the microwave electromagnetic field;
2）本发明提出的装置的圆环状石英微波窗口上端口的安装槽，能够方便圆盘状耦合天线的安装和准确定位； 2) The installation groove of the upper port of the circular quartz microwave window of the device proposed by the present invention can facilitate the installation and accurate positioning of the disc-shaped coupling antenna;
3）本发明提出的装置的第一圆柱形反射体、第二圆柱形反射体和圆柱形基台分别具备独立的升降机构，因此可调节各自的位置。通过三者位置的配合，优化调节不同基片直径及不同基片厚度条件下等离子体的状态，保证高功率密度条件下基片表面等离子体的均匀性； 3) The first cylindrical reflector, the second cylindrical reflector and the cylindrical base of the device proposed by the present invention have independent lifting mechanisms, so their positions can be adjusted. Through the coordination of the positions of the three, the state of the plasma under different substrate diameters and different substrate thicknesses can be optimally adjusted to ensure the uniformity of the plasma on the substrate surface under the condition of high power density;
4）本发明提出的装置在第一圆柱形反射体上设有若干出气孔，反应气体由设置在圆盘状耦合天线中央的进气孔进入反应腔室后，只能通过出气孔、再经下腔体的总出气孔排出到装置外，保证了基片表面气体分布的均匀性； 4) The device proposed by the present invention is provided with a number of air outlets on the first cylindrical reflector. After the reaction gas enters the reaction chamber through the air inlet arranged in the center of the disc-shaped coupling antenna, it can only pass through the air outlet, and then through the air outlet. The total air outlet of the lower chamber is discharged out of the device, ensuring the uniformity of gas distribution on the surface of the substrate;
5）本发明提出的装置中整体使用循环水冷却，包括上腔体、中腔体、下腔体、圆盘状耦合天线、第一圆柱形反射体及其升降机构、第二圆柱形反射体及其升降机构、圆柱形基台及其升降机构，能够保证装置在高功率密度条件下安全稳定的长时间运行； 5) The device proposed by the present invention is cooled by circulating water as a whole, including the upper cavity, the middle cavity, the lower cavity, the disc-shaped coupling antenna, the first cylindrical reflector and its lifting mechanism, and the second cylindrical reflector Its lifting mechanism, cylindrical abutment and its lifting mechanism can ensure the safe and stable long-term operation of the device under high power density conditions;
6）本发明提出的装置能够实现大面积、高均匀性金刚石膜材料的高速率沉积。 6) The device proposed in the present invention can achieve high-rate deposition of large-area, high-uniformity diamond film materials.
附图说明 Description of drawings
图1为本发明装置的结构示意图。 Fig. 1 is a structural schematic diagram of the device of the present invention.
图2为本发明装置的微波电场模拟结果图。 Fig. 2 is a diagram of the microwave electric field simulation results of the device of the present invention.
图3为使用本发明装置制备出的金刚石膜的表面微观形貌图。 Fig. 3 is a surface microscopic topography diagram of a diamond film prepared by using the device of the present invention.
图4为使用本发明装置制备出的金刚石膜的拉曼谱线。 Fig. 4 is the Raman spectral line of the diamond film prepared by using the device of the present invention.
图中： 1-上腔体、2-中腔体、3-下腔体、4-圆环状石英微波窗口、5-圆盘状耦合天线、6-圆柱凸台、7-进气孔、8-第一圆柱形反射体、9-第二圆柱形反射体、10-圆柱形基台、11-出气孔、12-升降机构、13-总出气孔、14-密封圈、15-基片、16-等离子体。 In the figure: 1-upper cavity, 2-middle cavity, 3-lower cavity, 4-annular quartz microwave window, 5-disc coupling antenna, 6-cylindrical boss, 7-intake hole, 8-first cylindrical reflector, 9-second cylindrical reflector, 10-cylindrical abutment, 11-air outlet, 12-lifting mechanism, 13-total air outlet, 14-sealing ring, 15-substrate , 16-Plasma.
具体实施方式 detailed description
以下结合附图对本发明作进一步地描述： The present invention will be further described below in conjunction with accompanying drawing:
如图1所示，一种用于化学气相沉积金刚石膜的高功率微波等离子体反应装置，包括圆柱形谐振腔体，所述的圆柱形谐振腔体分为上腔体1、中腔体2和下腔体3，中腔体2的直径小于上腔体1和下腔体3的直径；上腔体1的腔顶为圆锥形，上腔体1内的底部紧贴腔壁安装有圆环状石英微波窗口4，圆环状石英微波窗口4的上端口设有一圈安装槽，安装槽内安装有圆盘状耦合天线5，圆盘状耦合天线5的底部中心处设有下凸的圆柱凸台6，圆盘状耦合天线5上沿其轴线开设有进气孔7，进气孔7的直径可选择3-8mm；下腔体3的底部设有总出气孔13，下腔体3内紧贴腔壁安装有第一圆柱形反射体8，第一圆柱形反射体8的底面为平面状、顶面为向下沉陷的倒圆台状，第一圆柱形反射体8上沿其轴线开设有第一圆筒形安装孔，且在紧邻第一圆筒形安装孔的位置开设有出气孔11，出气孔11的直径可选择4-6mm，数量为8-24个，第一圆筒形安装孔内插装有第二圆柱形反射体9，第二圆柱形反射体9上沿其轴线开设有第二圆筒形安装孔，第二圆筒形安装孔内插装有圆柱形基台10；第一圆柱形反射体8、第二圆柱形反射体9和圆柱形基台10通过各自设置的升降机构12能分别实现升降动作； As shown in Figure 1, a high-power microwave plasma reaction device for chemical vapor deposition of diamond films includes a cylindrical resonant cavity, and the cylindrical resonant cavity is divided into an upper cavity 1 and a middle cavity 2 and the lower cavity 3, the diameter of the middle cavity 2 is less than the diameter of the upper cavity 1 and the lower cavity 3; the cavity top of the upper cavity 1 is conical, and the bottom of the upper cavity 1 is close to the cavity wall. The ring-shaped quartz microwave window 4, the upper port of the ring-shaped quartz microwave window 4 is provided with a circle of installation grooves, the disk-shaped coupling antenna 5 is installed in the installation groove, and the bottom center of the disk-shaped coupling antenna 5 is provided with a downward convex Cylindrical boss 6, disc-shaped coupling antenna 5 is provided with air inlet 7 along its axis, and the diameter of air inlet 7 can be selected 3-8mm; The bottom of lower cavity 3 is provided with total air outlet 13, lower cavity 3. A first cylindrical reflector 8 is installed close to the wall of the cavity. The bottom surface of the first cylindrical reflector 8 is planar, and the top surface is a rounded platform that sinks downward. The upper surface of the first cylindrical reflector 8 is A first cylindrical installation hole is provided on the axis, and an air outlet hole 11 is provided at a position close to the first cylindrical installation hole. The diameter of the air outlet hole 11 can be selected from 4-6mm, and the number is 8-24. A second cylindrical reflector 9 is inserted in the cylindrical mounting hole, and a second cylindrical mounting hole is opened on the second cylindrical reflector 9 along its axis, and a cylindrical reflector 9 is inserted in the second cylindrical mounting hole. The base 10; the first cylindrical reflector 8, the second cylindrical reflector 9 and the cylindrical base 10 can respectively realize the lifting action through the lifting mechanism 12 provided separately;
上腔体1、中腔体2、下腔体3、圆环状石英微波窗口4、圆盘状耦合天线5、第一圆柱形反射体8、第二圆柱形反射体9、圆柱形基台10为同轴线设置；圆环状石英微波窗口4与上腔体1之间、圆环状石英微波窗口4与圆盘状耦合天线5之间、第一圆柱形反射体8与下腔体3之间、第一圆柱形反射体8与第二圆柱形反射体9之间、第二圆柱形反射体9与圆柱形基台10之间都设有密封圈14。 Upper cavity 1, middle cavity 2, lower cavity 3, ring-shaped quartz microwave window 4, disc-shaped coupling antenna 5, first cylindrical reflector 8, second cylindrical reflector 9, cylindrical abutment 10 is coaxial setting; between the annular quartz microwave window 4 and the upper cavity 1, between the annular quartz microwave window 4 and the disc-shaped coupling antenna 5, between the first cylindrical reflector 8 and the lower cavity 3, between the first cylindrical reflector 8 and the second cylindrical reflector 9, and between the second cylindrical reflector 9 and the cylindrical base 10, a sealing ring 14 is provided.
具体实施时，上腔体1的圆锥形腔顶的斜边与水平线的夹角为5-20°；第一圆柱形反射体8上的斜边与水平线的夹角为10-25°。 During specific implementation, the angle between the hypotenuse of the conical top of the upper chamber 1 and the horizontal line is 5-20°; the angle between the hypotenuse on the first cylindrical reflector 8 and the horizontal line is 10-25°.
上腔体1、中腔体2、下腔体3、圆盘状耦合天线5、第一圆柱形反射体8及其升降机构12、第二圆柱形反射体9及其升降机构12、圆柱形基台10及其升降机构12均通过循环冷却水直接冷却。 Upper cavity 1, middle cavity 2, lower cavity 3, disc-shaped coupling antenna 5, first cylindrical reflector 8 and its lifting mechanism 12, second cylindrical reflector 9 and its lifting mechanism 12, cylindrical Both the base platform 10 and its lifting mechanism 12 are directly cooled by circulating cooling water.
以下结合一个具体的使用实施例，再对本发明装置作进一步地描述： The device of the present invention will be further described below in conjunction with a specific usage example:
实施例1 Example 1
1、使用直径为65mm，厚度为3mm的单晶硅片作为基片15材料，先将圆形基片15的沉积表面用粒径为5μm的金刚石粉均匀研磨，然后分别使用去离子水和丙酮将基片15表面超声清洗干净，并用热风吹干，放置在圆柱形基台10的顶面上； 1. Use a single crystal silicon wafer with a diameter of 65 mm and a thickness of 3 mm as the material of the substrate 15. First, the deposition surface of the circular substrate 15 is uniformly ground with diamond powder with a particle size of 5 μm, and then deionized water and acetone are used respectively Clean the surface of the substrate 15 ultrasonically, dry it with hot air, and place it on the top surface of the cylindrical abutment 10;
2、关闭真空反应腔室，并使用真空泵将反应腔室中的压强抽到1Pa以下； 2. Close the vacuum reaction chamber, and use a vacuum pump to pump the pressure in the reaction chamber below 1Pa;
3、开启循环水冷却系统，给装置各部分通入冷却水； 3. Turn on the circulating water cooling system and supply cooling water to each part of the device;
4、向装置反应腔室中通入流量为600sccm的氢气，调节反应腔室中的压强到2kPa； 4. In the reaction chamber of the device, the hydrogen gas with a flow rate of 600 sccm is introduced, and the pressure in the reaction chamber is adjusted to 2kPa;
5、将频率为2.45GHz微波源的功率设定为2kW后开启，在反应腔室中产生等离子体16； 5. After setting the power of the microwave source with a frequency of 2.45 GHz to 2 kW, turn it on, and generate plasma 16 in the reaction chamber;
6、调整第一圆柱形反射体8、第二圆柱形反射体9和圆柱形基台10的位置，使等离子体16位于基片15的上方，并使反射功率最低，等离子体16的强度达到最高； 6. Adjust the positions of the first cylindrical reflector 8, the second cylindrical reflector 9 and the cylindrical pedestal 10, so that the plasma 16 is positioned above the substrate 15, and the reflected power is the lowest, and the intensity of the plasma 16 reaches Highest;
7、逐渐提高装置中的微波输入功率和压强，并最终使功率达到11kW，压强达到25kPa，在这一过程中利用各升降机构12调整第一圆柱形反射体8、第二圆柱形反射体9和圆柱形基台10的位置，始终保持反射功率最低，等离子体16的强度达到最高，并使基片15表面的温度达到900℃，通过微调圆柱形基台10的高度，使基片15表面不同位置的温度偏差控制在±3℃； 7. Gradually increase the microwave input power and pressure in the device, and finally make the power reach 11kW and the pressure reach 25kPa. In this process, use each lifting mechanism 12 to adjust the first cylindrical reflector 8 and the second cylindrical reflector 9 and the position of the cylindrical base 10, the reflected power is always kept at the lowest level, the intensity of the plasma 16 reaches the highest, and the temperature on the surface of the substrate 15 reaches 900°C. By fine-tuning the height of the cylindrical base 10, the surface of the substrate 15 The temperature deviation of different positions is controlled within ±3°C;
8、向反应腔室中通入流量为12sccm的甲烷气体，1h后在基片15表面完成金刚石膜的形核；将甲烷流量调整为6sccm，开始金刚石膜的生长，金刚石膜的厚度取决于沉积的持续时间； 8. Feed into the reaction chamber a methane gas with a flow rate of 12 sccm, and complete the nucleation of the diamond film on the surface of the substrate 15 after 1 hour; adjust the methane flow rate to 6 sccm to start the growth of the diamond film. The thickness of the diamond film depends on the deposition duration of
9、沉积60h后，逐渐降低反应腔室中的压强和微波输入功率，在压强降至5kPa、微波功率降至3kW时，依次关闭微波源、氢气、甲烷及真空泵，结束金刚石膜的沉积； 9. After 60 hours of deposition, gradually reduce the pressure and microwave input power in the reaction chamber. When the pressure drops to 5kPa and the microwave power drops to 3kW, turn off the microwave source, hydrogen, methane and vacuum pump in turn to end the deposition of the diamond film;
10、开启充气阀给装置中充入空气至一个大气压后，开启装置取出样品； 10. Open the inflation valve to fill the device with air to an atmospheric pressure, and then open the device to take out the sample;
11、使用体积比为2:1的硝酸和氢氟酸混合溶液将单晶硅基片15腐蚀去除，得到厚度约为0.42mm的高品质金刚石膜，计算其沉积速率为7μm/h，不均匀度＜5%。图3为使用本发明装置制备出的金刚石膜的表面微观形貌图，从图中可以看出所制备的金刚石膜连续、致密，金刚石晶界间没有明显的间隙，也不存在明显的二次形核颗粒等缺陷。图4为使用本发明装置制备出的金刚石膜的拉曼谱线，从图中可以看出金刚石膜的拉曼光谱中只有1332 cm-1附近的一个金刚石特征峰，而且没有明显的石墨及其它杂质的特征峰出现，金刚石拉曼特征峰的半高宽为2.4 cm-1，这表明所制备的金刚石膜具有优良的品质。 11. Use a mixed solution of nitric acid and hydrofluoric acid with a volume ratio of 2:1 to etch and remove the single crystal silicon substrate 15 to obtain a high-quality diamond film with a thickness of about 0.42 mm. The calculated deposition rate is 7 μm/h, which is uneven degree <5%. Fig. 3 is the surface microscopic topography diagram of the diamond film prepared by using the device of the present invention, as can be seen from the figure, the prepared diamond film is continuous and dense, there is no obvious gap between the diamond grain boundaries, and there is no obvious secondary shape Defects such as nuclear particles. Fig. 4 is the Raman spectral line of the diamond film prepared by using the device of the present invention, as can be seen from the figure, there is only a diamond characteristic peak near 1332 cm in the Raman spectrum of the diamond film, and there is no obvious graphite and other The characteristic peaks of impurities appear, and the full width at half maximum of diamond Raman characteristic peaks is 2.4 cm -1 , which indicates that the prepared diamond film has excellent quality.
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| CN104988578B (en) * | 2015-07-24 | 2017-08-25 | 哈尔滨工业大学 | A kind of method that utilization plasma screen optimizes single-crystal diamond isoepitaxial growth |
| CN105239057B (en) * | 2015-11-06 | 2018-05-01 | 武汉理工大学 | Microwave plasma CVD device |
| CN106987827B (en) * | 2017-04-14 | 2019-03-29 | 太原理工大学 | Plasma activated chemical vapour deposition microwave cavity and device |
| CN106929828B (en) * | 2017-05-12 | 2023-05-23 | 中国工程物理研究院应用电子学研究所 | Substrate table for preparing diamond film by microwave plasma chemical vapor deposition method |
| CN107227450A (en) * | 2017-07-25 | 2017-10-03 | 无锡远稳烯科技有限公司 | A kind of microwave plasma CVD device and its production method |
| CN110230037A (en) * | 2018-03-06 | 2019-09-13 | 丁召民 | Microwave plasma reaction unit and microwave plasma reaction system |
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| CN110565160B (en) * | 2018-06-05 | 2021-11-09 | 广东众元半导体科技有限公司 | Microwave plasma chemical vapor deposition device |
| CN110913556A (en) * | 2018-09-18 | 2020-03-24 | 清华大学 | A microwave plasma reaction device |
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| CN111188023B (en) * | 2020-02-26 | 2022-04-15 | 美若科技有限公司 | Microwave Plasma Reactor |
| CN112103160B (en) * | 2020-08-19 | 2021-09-10 | 上海征世科技股份有限公司 | Substrate table and method for adjusting stability of microwave plasma ball |
| CN114164418A (en) * | 2021-11-29 | 2022-03-11 | 深圳优普莱等离子体技术有限公司 | Microwave plasma reaction cavity and equipment for chemical vapor deposition |
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| JPH11167998A (en) * | 1997-12-04 | 1999-06-22 | Canon Inc | Plasma processing device and processing method using parabolic antenna |
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