CN102869182A - Large-volume microwave plasma generating device based on coupling window radiation - Google Patents
Large-volume microwave plasma generating device based on coupling window radiation Download PDFInfo
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Abstract
本发明涉及一种基于耦合窗辐射的大体积微波等离子体发生装置,属于微波应用技术领域。该发生装置包括包括矩形波导、电感式耦合窗、谐振腔外壳、矩形石英玻璃框、短路活塞、吸收物质和手柄。矩形波导通过电感式耦合窗与谐振腔的一端连通,谐振腔外壳上设有气压测量口、工作气体进气口和工作气体出气口。矩形石英玻璃框置于谐振腔内,其两端部镶嵌在谐振腔的侧壁上,与两侧的谐振腔侧壁形成封闭空间。短路活塞置于谐振腔的另一端,短路活塞与谐振腔外壳成滑动配合。吸收物质固定在短路活塞的前端部,手柄固定在短路活塞的后端部。本装置能够在常温常压下产生大体积的微波等离子体,高效率地制备纳米材料和处理废气尾气。
The invention relates to a large-volume microwave plasma generating device based on coupling window radiation, belonging to the technical field of microwave applications. The generating device includes a rectangular waveguide, an inductive coupling window, a resonant cavity shell, a rectangular quartz glass frame, a short-circuit piston, an absorbing substance and a handle. The rectangular waveguide communicates with one end of the resonant cavity through an inductive coupling window, and the shell of the resonant cavity is provided with a pressure measurement port, a working gas inlet and a working gas outlet. The rectangular quartz glass frame is placed in the resonant cavity, and its two ends are inlaid on the side walls of the resonant cavity, forming a closed space with the side walls of the resonant cavity on both sides. The short-circuit piston is placed at the other end of the resonant cavity, and the short-circuit piston is in sliding fit with the shell of the resonant cavity. The absorbing substance is fixed on the front end of the short-circuit piston, and the handle is fixed on the rear end of the short-circuit piston. The device can generate large-volume microwave plasma under normal temperature and pressure, and can efficiently prepare nanometer materials and treat waste gas and tail gas.
Description
技术领域 technical field
本发明涉及一种基于耦合窗辐射的大体积微波等离子体发生装置,属于微波应用技术领域。The invention relates to a large-volume microwave plasma generating device based on coupling window radiation, belonging to the technical field of microwave applications.
背景技术 Background technique
材料科学与技术作为21世纪人类三大关键科技之一,在国民经济及国防事业中起到至关重要的作用,而纳米技术的出现则开创了材料科学研究的新时代。与宏观尺寸的材料不同,纳米材料(尺度为0.1~100nm)表面的电子结构和晶体结构发生变化,产生表面效应、小尺寸效应、量子效应、宏观量子隧道效应和界面效应等;并表现出优异的光、电、磁和化学特性,因而在诸多领域有着广阔的应用前景。As one of the three key technologies of mankind in the 21st century, materials science and technology play a vital role in the national economy and national defense. The emergence of nanotechnology has created a new era of materials science research. Different from macroscopic materials, the electronic structure and crystal structure of the surface of nanomaterials (0.1~100nm) change, resulting in surface effects, small size effects, quantum effects, macroscopic quantum tunneling effects and interface effects, etc.; and exhibit excellent Optical, electrical, magnetic and chemical properties, so it has broad application prospects in many fields.
目前制备纳米材料的方法很多,但各种方法都有其自身客观的缺点。如传统湿法,工艺过程复杂、粒子表面化学状态难以控制、无氧条件很难创造、无法实现连续化和自动化批量生产;气相-液相法:化学活性低、反应速度慢、广谱性差、只能制备少数几种纳米粒子;直流等离子体和介质阻挡放电等离子体法:存在电极且其电场具有极性和不均匀性、易使生成的纳米磁性粒子发生链状化而团聚并最终使正负极相连导致电极之间发生击穿现象;化学气相沉积法(CVD)和射频等离子体法:温度过高、需要真空条件、而且能耗大。At present, there are many methods for preparing nanomaterials, but each method has its own objective shortcomings. Such as the traditional wet method, the process is complicated, the chemical state of the particle surface is difficult to control, the anaerobic condition is difficult to create, and continuous and automated mass production cannot be realized; the gas phase-liquid phase method: low chemical activity, slow reaction speed, poor broad spectrum, Only a few kinds of nanoparticles can be prepared; DC plasma and dielectric barrier discharge plasma method: there are electrodes and the electric field has polarity and inhomogeneity, and it is easy to chain and agglomerate the generated nano-magnetic particles and finally make positive The connection of the negative electrodes leads to breakdown between the electrodes; chemical vapor deposition (CVD) and radio frequency plasma methods: the temperature is too high, vacuum conditions are required, and the energy consumption is large.
微波等离子体由于具有众多优点,有望合成纯度更高、粒度可控、粒径分布更窄、无硬团聚的纳米材料。其优点为:电子温度高,工作气压可更低、电离度高(大约高10倍);反应平衡常数高、温度梯度大、均相成核速率高、粉末更细;高频电磁场的波动作用和大的温度梯度引起的对流作用使颗粒粒径更趋均匀;没有内部电极,等离子体纯净;激发态粒子寿命长,化学活性物种多;微波能量对反应物分子均匀迅速地加热,通过微波的“瞬时加热”及“瞬时停止加热”的特性可以人为控制结晶速度;微波等离子体可被控制在特定的空间,应用方便。Due to its many advantages, microwave plasma is expected to synthesize nanomaterials with higher purity, controllable particle size, narrower particle size distribution, and no hard agglomeration. Its advantages are: high electron temperature, lower working pressure, high ionization degree (about 10 times higher); high reaction equilibrium constant, large temperature gradient, high homogeneous nucleation rate, and finer powder; the fluctuation effect of high-frequency electromagnetic field The convection effect caused by the large temperature gradient makes the particle size more uniform; there is no internal electrode, the plasma is pure; the excited state particles have a long life, and there are many chemically active species; the microwave energy heats the reactant molecules uniformly and rapidly, through the microwave The characteristics of "instantaneous heating" and "instantaneous stop of heating" can artificially control the crystallization speed; microwave plasma can be controlled in a specific space, which is convenient for application.
在城市化和工业化进程中,世界经济突飞猛进地发展,同时也带来了众多环境污染问题,如工业废气和汽车尾气的排放给环境及人类身心健康均带来了严重的危害。科学分析表明,汽车尾气中含有上百种不同的化合物,其中的污染物有固体悬浮微粒、一氧化碳、二氧化碳、碳氢化合物、氮氧化合物、铅及硫氧化合物等。一辆轿车一年排出的有害废气比自身重量大3倍。英国空气洁净和环境保护协会曾发表研究报告称,与交通事故遇难者相比,英国每年死于空气污染的人要多出10倍。因此这些废气的处理已经成为亟待解决的问题。微波等离子体由于其电子温度高、电离度高、激发态粒子寿命长、化学活性物种多及微波技术成熟等诸多优点,也成为了废气处理方式的首要选择。In the process of urbanization and industrialization, the world economy has developed by leaps and bounds, but it has also brought many environmental pollution problems, such as industrial waste gas and automobile exhaust emissions, which have brought serious harm to the environment and human physical and mental health. Scientific analysis shows that automobile exhaust contains hundreds of different compounds, among which pollutants include solid suspended particles, carbon monoxide, carbon dioxide, hydrocarbons, nitrogen oxides, lead, and sulfur oxides. The harmful exhaust gas emitted by a car in a year is three times larger than its own weight. The British Association for Clean Air and Environmental Protection once published a research report saying that compared with the victims of traffic accidents, the number of people who die from air pollution in the UK is 10 times more than that of the victims of traffic accidents every year. Therefore, the treatment of these exhaust gases has become an urgent problem to be solved. Due to its high electron temperature, high degree of ionization, long lifetime of excited particles, many chemically active species, and mature microwave technology, microwave plasma has also become the first choice for waste gas treatment.
发明内容 Contents of the invention
本发明目的是提出一种基于耦合窗辐射的大体积微波等离子体发生装置,以用于纳米材料的制备和工业废气及汽车尾气的处理,并使其能够在常压下长时间工作,便于大规模的工业应用。The purpose of the present invention is to propose a large-volume microwave plasma generating device based on coupling window radiation, which is used for the preparation of nanomaterials and the treatment of industrial waste gas and automobile exhaust gas, and enables it to work for a long time under normal pressure, which is convenient for large-scale large-scale industrial applications.
本发明提出的基于耦合窗辐射的大体积微波等离子体发生装置,包括矩形波导、电感式耦合窗、谐振腔外壳、矩形石英玻璃框、短路活塞、吸收物质和手柄;所述的矩形波导通过电感式耦合窗与谐振腔的一端连通,谐振腔外壳上设有气压测量口、工作气体进气口和工作气体出气口;所述的矩形石英玻璃框置于谐振腔内,矩形石英玻璃框的两端部镶嵌在谐振腔的侧壁上,矩形石英玻璃框与两侧的谐振腔侧壁形成封闭空间;所述的短路活塞置于谐振腔的另一端,短路活塞与谐振腔外壳成滑动配合;所述的吸收物质固定在短路活塞的前端部,并位于谐振腔内,所述的手柄固定在短路活塞的后端部,并位于谐振腔外。The large-volume microwave plasma generating device based on coupling window radiation proposed by the present invention includes a rectangular waveguide, an inductive coupling window, a resonant cavity shell, a rectangular quartz glass frame, a short-circuit piston, an absorbing material and a handle; The type coupling window is connected with one end of the resonant cavity, and the shell of the resonant cavity is provided with an air pressure measurement port, a working gas inlet and a working gas outlet; the rectangular quartz glass frame is placed in the resonant cavity, and the two sides of the rectangular quartz glass frame The end is inlaid on the side wall of the resonant cavity, and the rectangular quartz glass frame forms a closed space with the side walls of the resonant cavity on both sides; the short-circuit piston is placed at the other end of the resonant cavity, and the short-circuit piston is in sliding fit with the shell of the resonant cavity; The absorbing substance is fixed on the front end of the short-circuit piston and located inside the resonant cavity, and the handle is fixed on the rear end of the short-circuit piston and located outside the resonant cavity.
本发明提出的基于耦合窗辐射的大体积微波等离子体发生装置,其优点是:能够在常温常压下产生大体积的微波等离子体,高效率地制备纳米材料和处理废气尾气。本发明的等离子体方式装置,相对于已有的其它微波耦合方式,如孔耦合和狭缝耦合,本发明采用的电感式耦合窗的耦合效率极高,基本消除了微波传输和耦合的损耗,能够在密封环境中形成大体积微波等离子体,一方面在纳米材料制备中保证材料纯度较高,另一方面在废气尾气处理过程中能够防止废气尾气扩散到其它区域。本发明的等离子体发生装置中,安装在矩形谐振腔尾部的可调式滑动短路活塞能够自由调节谐振腔长度以使微波达到最佳谐振状态;矩形谐振腔由多块金属板拼接而成,既能保证微波不泄露造成人身危害,同时方便装置的拆卸及安装。The large-volume microwave plasma generating device based on coupling window radiation proposed by the present invention has the advantages of being able to generate large-volume microwave plasma at normal temperature and pressure, and efficiently prepare nanomaterials and treat exhaust gas. Compared with other existing microwave coupling methods, such as hole coupling and slit coupling, the plasma device of the present invention has an extremely high coupling efficiency of the inductive coupling window, which basically eliminates the loss of microwave transmission and coupling. It can form a large volume of microwave plasma in a sealed environment. On the one hand, it can ensure high material purity in the preparation of nanomaterials, and on the other hand, it can prevent the exhaust gas from diffusing to other areas during the exhaust gas treatment process. In the plasma generating device of the present invention, the adjustable sliding short-circuit piston installed at the tail of the rectangular resonant cavity can freely adjust the length of the resonant cavity so that the microwave can reach the best resonance state; the rectangular resonant cavity is spliced by multiple metal plates, which can Ensure that the microwave does not leak and cause personal harm, and at the same time facilitate the disassembly and installation of the device.
附图说明 Description of drawings
图1是本发明提出的基于耦合窗辐射的大体积微波等离子体发生装置的结构示意图。Fig. 1 is a schematic structural diagram of a large-volume microwave plasma generating device based on coupling window radiation proposed by the present invention.
图2是图1的A-A剖面图。Fig. 2 is a cross-sectional view along line A-A of Fig. 1 .
图3是图2的B-B剖面图。Fig. 3 is a B-B sectional view of Fig. 2 .
图4是与图1相对应剖面的电场分布图。FIG. 4 is an electric field distribution diagram of a section corresponding to FIG. 1 .
图5是与图2相对应剖面的电场分布图。FIG. 5 is an electric field distribution diagram of a section corresponding to FIG. 2 .
图1~3中,1是连接法兰,2是矩形波导,3是电感式耦合窗,4是谐振腔外壳,5是矩形石英玻璃框,6是气压测量口,7是工作气体进气口,8是短路活塞,9是吸收物质,10是手柄,11是工作气体出气口。In Figures 1 to 3, 1 is the connecting flange, 2 is the rectangular waveguide, 3 is the inductive coupling window, 4 is the resonant cavity shell, 5 is the rectangular quartz glass frame, 6 is the air pressure measurement port, and 7 is the working gas inlet , 8 is a short-circuit piston, 9 is an absorbing substance, 10 is a handle, and 11 is a working gas outlet.
具体实施方式 Detailed ways
本发明提出的基于耦合窗辐射的大体积微波等离子体发生装置,其结构如图1所示,包括矩形波导2、电感式耦合窗3、谐振腔外壳4、矩形石英玻璃框5、短路活塞8、吸收物质9和手柄10。矩形波导2通过电感式耦合窗3与谐振腔的一端连通,谐振腔外壳4上设有气压测量口6、工作气体进气口7和工作气体出气口11。矩形石英玻璃框5置于谐振腔内,矩形石英玻璃框5的两端部镶嵌在谐振腔的侧壁上,矩形石英玻璃框5与两侧的谐振腔侧壁形成封闭空间。短路活塞8置于谐振腔的另一端,短路活塞8与谐振腔外壳4成滑动配合。吸收物质9固定在短路活塞8的前端部,并位于谐振腔内。手柄10固定在短路活塞8的后端部,并位于谐振腔外。The large-volume microwave plasma generator based on coupling window radiation proposed by the present invention has a structure as shown in Figure 1, including a
本发明提出的等离子体发生装置,其中的矩形波导的型号为BJ22。其中的微波耦合器件由法兰、和电感式耦合窗依次焊接相连而成,并通过法兰与外部标准微波器件相连,这种微波耦合器件是基于电感式耦合窗,这种电感式耦合窗可以最大程度上使微波封闭在矩形谐振腔内部,使微波自由无障碍地馈入到矩形谐振腔中,当微波在矩形谐振腔内部谐振时,仅有极少量的微波能够通过耦合窗反射到微波源,其中耦合窗也可以设计为电容式或者谐振式耦合窗。矩形谐振腔由三部分组成,分别为矩形谐振腔外壳、圆角矩形石英玻璃框及焊接在矩形谐振腔前后铜板上的进、出气口及气压测量接口。矩形谐振腔本质上是一个长方体,其长度、宽度和高度均不同,它由六块铜板拼接而成,这样设计是为了可以方便的拆卸及安装,在矩形谐振腔前后铜板上开多个气孔,分别为工作气体进气口、出气和气压测量口。圆角矩形石英玻璃框镶嵌在矩形谐振腔内部,圆角矩形石英玻璃框仅有四个面,另外两个面是矩形谐振腔的前后铜板,这样的设计既能保证形成一个密封的工作气体空间,这个密封工作空间对产生不同气压或者不同工作气体的微波等离子体是极其重要的,又能方便工作气体的进出及测量圆角矩形石英玻璃框内的工作气体气压,圆角矩形石英玻璃框提供的一个密封空间在制备纳米材料和废气尾气处理中是至关重要的。矩形谐振腔与微波耦合器件以焊接或者螺丝固定的形式相连,微波通过电感式耦合窗馈入到矩形谐振腔内部并进一步辐射到圆角矩形石英玻璃框内部。谐振腔也可以设计为圆柱形谐振腔。可调式滑动短路活塞直接以滑动配合的方式插入矩形谐振腔的后端部铜板上,它可以在一定距离内自由滑动以调节矩形谐振腔的长度,使微波能够在矩形谐振腔内部产生良好的谐振,产生大体积的强电场区,进而在圆角矩形石英玻璃框里面产生大体积的微波等离子体,提高纳米材料制备和废气尾气处理的效率。In the plasma generating device proposed by the present invention, the model of the rectangular waveguide is BJ22. Among them, the microwave coupling device is welded and connected with the flange and the inductive coupling window in sequence, and is connected with the external standard microwave device through the flange. This microwave coupling device is based on the inductive coupling window, and the inductive coupling window can be The microwave is enclosed in the rectangular resonant cavity to the greatest extent, so that the microwave can be fed into the rectangular resonant cavity freely and unobstructed. When the microwave resonates inside the rectangular resonant cavity, only a very small amount of microwave can be reflected to the microwave source through the coupling window , where the coupling window can also be designed as a capacitive or resonant coupling window. The rectangular resonant cavity is composed of three parts, which are the rectangular resonant cavity shell, the rounded rectangular quartz glass frame, the air inlet and outlet ports and the air pressure measurement interface welded on the front and rear copper plates of the rectangular resonant cavity. The rectangular resonator is essentially a cuboid with different lengths, widths and heights. It is spliced by six copper plates. This design is for easy disassembly and installation. Multiple air holes are opened on the front and rear copper plates of the rectangular resonator. They are working gas inlet, outlet and air pressure measurement port respectively. The rounded rectangular quartz glass frame is inlaid inside the rectangular resonant cavity. The rounded rectangular quartz glass frame has only four sides, and the other two sides are the front and rear copper plates of the rectangular resonant cavity. This design can not only ensure the formation of a sealed working gas space , this sealed working space is extremely important for generating microwave plasma with different pressures or different working gases, and it can also facilitate the entry and exit of working gases and measure the pressure of working gases in the rounded rectangular quartz glass frame. The rounded rectangular quartz glass frame provides A sealed space is crucial in the preparation of nanomaterials and exhaust gas treatment. The rectangular resonant cavity is connected with the microwave coupling device in the form of welding or screw fixing, and the microwave is fed into the rectangular resonant cavity through the inductive coupling window and further radiated into the rounded rectangular quartz glass frame. The resonator can also be designed as a cylindrical resonator. The adjustable sliding short-circuit piston is directly inserted into the copper plate at the rear end of the rectangular resonant cavity in a sliding fit. It can slide freely within a certain distance to adjust the length of the rectangular resonant cavity, so that the microwave can generate good resonance inside the rectangular resonant cavity. , generate a large-volume strong electric field area, and then generate a large-volume microwave plasma in the rounded rectangular quartz glass frame, improving the efficiency of nanomaterial preparation and exhaust gas treatment.
以下结合附图,详细介绍本发明装置的工作原理:Below in conjunction with accompanying drawing, introduce the working principle of the device of the present invention in detail:
本发明涉及的用于制备纳米材料和处理工业废气及汽车尾气的微波等离子体发生装置,包括微波耦合器件、矩形谐振腔和可调式滑动短路活塞。法兰1、BJ22矩形波导2与电感式耦合窗3依次焊接在一起,然后电感式耦合窗与矩形谐振腔4的左边铜板焊接在一起,六块铜板通过螺丝紧固形成矩形谐振腔4,可调式滑动短路活塞直接插入矩形谐振腔4的右边铜板的正中间,圆角矩形石英玻璃框镶嵌在矩形谐振腔4的前后面铜板中以形成封闭空间,气压测量接口6、工作气体的进气口7、工作气体的出气口11分别焊接在矩形谐振腔4的前后铜板上。整个微波等离子体发生装置通过法兰1与外部标准微波器件以螺丝相连。The invention relates to a microwave plasma generating device for preparing nanometer materials and treating industrial waste gas and automobile exhaust gas, comprising a microwave coupling device, a rectangular resonant cavity and an adjustable sliding short-circuit piston. Flange 1, BJ22
微波通过BJ22矩形波导2传输,经过电感式耦合窗3耦合到矩形谐振腔4内部,由于圆角矩形石英玻璃框5对微波的传输基本没有影响,微波能够馈入到圆角矩形石英玻璃框5内部,通过调节可调式滑动短路活塞的位置可以改变矩形谐振腔4的长度,使微波在矩形谐振腔4内部谐振,并在圆角矩形石英玻璃框5内部形成大体积的强微波电场,等离子体发生装置的剖面电场分布如图4、5所示,微波强电场使圆角矩形石英玻璃框5内部的工作气体电离产生大体积微波等离子体。Microwaves are transmitted through the BJ22
对于制备纳米材料,进气口7通入反应混合气体,出气口11接入用户自定的材料收集器,气压测量接口6接入气压表以测量圆角矩形石英玻璃框内部的工作气体气压,反应混合气体通过微波等离子体后形成的纳米材料可以通过气流由出气口11进入收集器。通过调节工作气体的气压大小和微波功率,可以用来制备特性不同的纳米材料。对于处理工业废气和汽车尾气,进气口7通入废气或尾气,出气口11接入下一步处理程序的装置或者直接与大气相连,废气或尾气通过微波等离子体处理后由出气口11进入下步处理程序或者直接通入大气中,不同的废气或尾气的气压和微波功率对应着不同的废气或尾气的处理效率。For the preparation of nanomaterials, the
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