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CN118553594B - A graphite boat cleaning device and method based on straight rod antenna ICP - Google Patents

A graphite boat cleaning device and method based on straight rod antenna ICP Download PDF

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CN118553594B
CN118553594B CN202411012396.1A CN202411012396A CN118553594B CN 118553594 B CN118553594 B CN 118553594B CN 202411012396 A CN202411012396 A CN 202411012396A CN 118553594 B CN118553594 B CN 118553594B
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graphite boat
reaction chamber
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middle position
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CN118553594A (en
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卢旭
袁刚
汤芳
王超军
林娜
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China Science And Technology Ningbo Co ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/32009Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32082Radio frequency generated discharge
    • H01J37/321Radio frequency generated discharge the radio frequency energy being inductively coupled to the plasma
    • H01J37/3211Antennas, e.g. particular shapes of coils
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/32431Constructional details of the reactor
    • H01J37/3244Gas supply means
    • H01J37/32449Gas control, e.g. control of the gas flow
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/32431Constructional details of the reactor
    • H01J37/32458Vessel
    • H01J37/32513Sealing means, e.g. sealing between different parts of the vessel
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/32431Constructional details of the reactor
    • H01J37/32458Vessel
    • H01J37/32522Temperature
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/32431Constructional details of the reactor
    • H01J37/32532Electrodes
    • H01J37/32541Shape
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/32431Constructional details of the reactor
    • H01J37/32532Electrodes
    • H01J37/32559Protection means, e.g. coatings
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/32431Constructional details of the reactor
    • H01J37/32532Electrodes
    • H01J37/32568Relative arrangement or disposition of electrodes; moving means
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10FINORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F71/00Manufacture or treatment of devices covered by this subclass
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/32Processing objects by plasma generation
    • H01J2237/33Processing objects by plasma generation characterised by the type of processing
    • H01J2237/335Cleaning
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Drying Of Semiconductors (AREA)

Abstract

本发明提供一种基于直杆天线ICP的石墨舟清洗设备及方法,石墨舟清洗技术领域,以解决现有技术中ICP针对清洗石墨舟这种大面积、大体积的应用,若选用螺旋线圈或平面线圈两种形式,会导致线圈整体的电感量巨大,难以与主流射频电源相匹配的技术问题;一种基于直杆天线ICP的石墨舟清洗设备,包括反应室,反应室内设有反应腔,反应腔内设有偏压电极板,偏压电极板上设有用于放置石墨舟的绝缘块,反应室内连接有若干直杆电极,每根直杆电极的长度方向与石墨舟长度方向在空间上垂直,若干直杆电极并联呈单梳型、双梳型、U型、双梳型与U型相结合的其中一种布局;还涉及一种基于直杆天线ICP的石墨舟清洗方法,使用上述的石墨舟清洗设备。

The present invention provides a graphite boat cleaning device and method based on a straight-rod antenna ICP, in the field of graphite boat cleaning technology, to solve the technical problem that in the prior art, if a spiral coil or a planar coil is used for the large-area and large-volume application of ICP for cleaning a graphite boat, the overall inductance of the coil will be huge and it will be difficult to match the mainstream radio frequency power supply; a graphite boat cleaning device based on a straight-rod antenna ICP comprises a reaction chamber, a reaction cavity is provided in the reaction chamber, a bias electrode plate is provided in the reaction cavity, an insulating block for placing the graphite boat is provided on the bias electrode plate, a plurality of straight-rod electrodes are connected in the reaction chamber, the length direction of each straight-rod electrode is vertical to the length direction of the graphite boat in space, and the plurality of straight-rod electrodes are connected in parallel to form a single-comb type, a double-comb type, a U-type, or a combination of a double-comb type and a U-type layout; and also relates to a graphite boat cleaning method based on a straight-rod antenna ICP, using the above-mentioned graphite boat cleaning device.

Description

一种基于直杆天线ICP的石墨舟清洗设备及方法A graphite boat cleaning device and method based on straight rod antenna ICP

技术领域Technical Field

本发明涉及石墨舟清洗技术领域,具体讲是指一种基于直杆天线ICP的石墨舟清洗设备及方法。The invention relates to the technical field of graphite boat cleaning, and in particular to a graphite boat cleaning device and method based on a straight rod antenna ICP.

背景技术Background Art

在TOPCon太阳能电池生产过程中,其隧穿氧化层超薄氧化硅(SiOx)和高掺杂多晶硅(poly-Si)通常采用管式等离子体增强化学气相沉积设备(通常称为管式PECVD设备)制备,其中PECVD制备隧穿氧化层和高掺杂多晶硅的生长过程中,需要使用到承载晶硅电池片的承载物,通常称为石墨舟。在PECVD工艺制备过程中,石墨舟承载着晶硅电池片沉浸在PECVD反应腔体内,因此沉积反应在电池片上的隧穿氧化硅和掺杂非晶硅材料也会沉积在石墨舟的各个结构表面,当石墨舟上沉积的薄膜达到一定厚度后,由于高掺杂多晶硅的弱导电性,因此会影响石墨舟两片互为正负极的舟叶间电阻值,从而影响正常的PECVD沉积反应生长速率,从而影响电池片生产工艺的稳定性,因此,石墨舟在使用过一段时间后,需要对石墨舟做清洗处理,去除表面沉积的氧化硅和高掺杂多晶硅材料。In the production process of TOPCon solar cells, its tunneling oxide layer ultra-thin silicon oxide (SiOx) and highly doped polycrystalline silicon (poly-Si) are usually prepared by tubular plasma enhanced chemical vapor deposition equipment (commonly known as tubular PECVD equipment). In the process of PECVD preparation of tunneling oxide layer and highly doped polycrystalline silicon, a carrier for carrying crystalline silicon cells is required, usually called a graphite boat. In the PECVD process, the graphite boat carries the crystalline silicon cell and is immersed in the PECVD reaction chamber. Therefore, the tunneling silicon oxide and doped amorphous silicon materials deposited on the cell will also be deposited on the surface of each structure of the graphite boat. When the film deposited on the graphite boat reaches a certain thickness, due to the weak conductivity of highly doped polycrystalline silicon, it will affect the resistance value between the two boat leaves of the graphite boat, which are positive and negative electrodes to each other, thereby affecting the normal PECVD deposition reaction growth rate, thereby affecting the stability of the cell production process. Therefore, after the graphite boat has been used for a period of time, it is necessary to clean the graphite boat to remove the silicon oxide and highly doped polycrystalline silicon materials deposited on the surface.

湿法清洗是目前业界选用的主流石墨舟清洗方法,但是该方法存在清洗用时较长、效率低下、容易损坏石墨舟、清洗不足或清洗过度、污染环境的缺点。近年来,基于等离子体的石墨舟“干式”清洗设备不断涌现。目前石墨舟干式清洗设备大多采用容性耦合等离子体(CCP,Capacitively coupled plasma)作为等离子体源,CCP对石墨舟侧壁的刻蚀清洗效果往往不够理想,并且所要求的工作气压较高,电离率相对较低,为保证清洗效率不得不提高功率,然而这又可能会进一步导致局部过刻问题。此外,要实现对整个石墨舟的清洗,需要的电极面积巨大,增加了加工难度和成本。Wet cleaning is the mainstream graphite boat cleaning method currently used in the industry, but this method has the disadvantages of long cleaning time, low efficiency, easy damage to the graphite boat, insufficient or excessive cleaning, and environmental pollution. In recent years, plasma-based "dry" graphite boat cleaning equipment has continued to emerge. At present, most graphite boat dry cleaning equipment uses capacitively coupled plasma (CCP) as the plasma source. The etching and cleaning effect of CCP on the side wall of the graphite boat is often not ideal, and the required working gas pressure is high and the ionization rate is relatively low. In order to ensure the cleaning efficiency, the power has to be increased, which may further lead to local over-engraving problems. In addition, to achieve the cleaning of the entire graphite boat, a huge electrode area is required, which increases the processing difficulty and cost.

感性耦合等离子体(ICP,Inductively coupled plasma)是常见的低气压等离子体形式之一,其原理是交流电通过电极线圈在真空腔内产生诱导磁场,诱导磁场产生诱导电场,电子在诱导电场的加速下轰击气体分子产生等离子体。ICP具有工作气压低、电离率高、离子能量可调节范围大、电极和腔室分离不易被污染等优点,在集成电路制造等领域被广泛应用。然而,ICP针对清洗石墨舟这种大面积、大体积的应用,若选用螺旋线圈或平面线圈两种形式,则会导致线圈整体的电感量巨大,以致难以与主流射频电源相匹配,导致ICP在大面积、大体积的石墨舟清洗上应用受限。Inductively coupled plasma (ICP) is one of the common forms of low-pressure plasma. Its principle is that alternating current generates an induced magnetic field in a vacuum chamber through an electrode coil, and the induced magnetic field generates an induced electric field. Electrons bombard gas molecules under the acceleration of the induced electric field to generate plasma. ICP has the advantages of low working pressure, high ionization rate, large adjustable range of ion energy, separation of electrodes and chambers, and is not easily contaminated. It is widely used in fields such as integrated circuit manufacturing. However, for large-area and large-volume applications such as cleaning graphite boats, if spiral coils or planar coils are used, the overall inductance of the coil will be huge, making it difficult to match the mainstream RF power supply, resulting in limited application of ICP in cleaning large-area and large-volume graphite boats.

发明内容Summary of the invention

针对现有技术的不足,本发明的第一个目的在于提供一种基于直杆天线ICP的石墨舟清洗设备,以解决现有技术中ICP针对清洗石墨舟这种大面积、大体积的应用,若选用螺旋线圈或平面线圈两种形式,则会导致线圈整体的电感量巨大,以致难以与主流射频电源相匹配的技术问题。In view of the shortcomings of the prior art, the first purpose of the present invention is to provide a graphite boat cleaning equipment based on a straight rod antenna ICP, so as to solve the technical problem that in the prior art, if a spiral coil or a planar coil is used for the large-area and large-volume application of ICP for cleaning graphite boats, the overall inductance of the coil will be huge, making it difficult to match the mainstream RF power supply.

为解决上述技术问题,本发明提供了一种基于直杆天线ICP的石墨舟清洗设备,包括反应室,反应室内设有容纳石墨舟的反应腔,反应腔内设有偏压电极板,偏压电极板上设有用于放置石墨舟的绝缘块,反应室内连接有若干直杆电极,若干直杆电极水平设置且相互平行,当石墨舟放置在绝缘块上时,每根直杆电极均位于石墨舟上方且每根直杆电极的长度方向与石墨舟长度方向在空间上垂直设置,若干直杆电极并联呈单梳型、双梳型、U型、双梳型与U型相结合的其中一种布局。To solve the above technical problems, the present invention provides a graphite boat cleaning device based on straight rod antenna ICP, comprising a reaction chamber, a reaction cavity for accommodating a graphite boat is arranged in the reaction chamber, a bias electrode plate is arranged in the reaction cavity, an insulating block for placing the graphite boat is arranged on the bias electrode plate, a plurality of straight rod electrodes are connected in the reaction chamber, the plurality of straight rod electrodes are arranged horizontally and parallel to each other, when the graphite boat is placed on the insulating block, each straight rod electrode is located above the graphite boat and the length direction of each straight rod electrode is arranged vertically in space to the length direction of the graphite boat, and the plurality of straight rod electrodes are connected in parallel to form a single comb type, a double comb type, a U-type, or a combination of a double comb type and a U-type layout.

采用上述结构后,本发明中的一种基于直杆天线ICP的石墨舟清洗设备具有以下优点:将ICP中常规的螺旋线圈或平面线圈拆分成直杆电极并联形式,阻抗较低,便于控制整体阻抗,能够适配市面上主流射频电源及匹配器,通过增减直杆电极的数量还可适配不同尺寸的反应腔与石墨舟,无需定制化电极,材料及加工成本低,相比于CCP而言,电离率更高,清洗效果更好,工作气压更低,能够减少特气的使用;此外,单梳型的布局形式结构简单,双梳型通过电场调制能够进一步提高等离子体均匀性,适用于对清洗要求更高的场合,双梳型与U型相结合是在双梳型的基础上减小了射频电源和匹配器的使用,降低成本,适用于更大尺寸石墨舟的处理需求。After adopting the above structure, a graphite boat cleaning equipment based on the straight rod antenna ICP in the present invention has the following advantages: the conventional spiral coil or planar coil in the ICP is split into a parallel form of straight rod electrodes, the impedance is low, it is easy to control the overall impedance, and it can be adapted to the mainstream RF power supply and matching device on the market. By increasing or decreasing the number of straight rod electrodes, it can also be adapted to reaction chambers and graphite boats of different sizes. No customized electrodes are required, and the material and processing costs are low. Compared with CCP, the ionization rate is higher, the cleaning effect is better, the working gas pressure is lower, and the use of special gases can be reduced; in addition, the single-comb type has a simple layout structure, and the double-comb type can further improve the plasma uniformity through electric field modulation, which is suitable for occasions with higher cleaning requirements. The combination of the double-comb type and the U-type reduces the use of RF power supply and matching device on the basis of the double-comb type, reduces costs, and is suitable for the processing needs of larger-sized graphite boats.

作为改进,若干直杆电极呈单梳型布局并且馈入点和接地点呈对角分布;采用此种结构,馈入点和接地点对角设置使得每路产生的等离子体均一性好,成本低,适合小型、试验型石墨舟的清洗。As an improvement, several straight rod electrodes are arranged in a single comb shape and the feeding points and the grounding points are distributed diagonally. With this structure, the feeding points and the grounding points are arranged diagonally so that the plasma generated in each path has good uniformity and low cost, which is suitable for the cleaning of small, experimental graphite boats.

作为改进,直杆电极由内向外依次包括空心金属管、绝缘支架和绝缘套管,空心金属管外壁通过若干个沿空心金属管外壁周向设置的绝缘支架与绝缘套管内壁连接,空心金属管与绝缘套管同轴设置;采用此种结构,由绝缘套管对空心金属管进行保护防止其直接裸露而受到等离子体刻蚀,显著降低了设备故障率和维护成本,空心金属管在清洗过程中内部流通冷却用的超纯水,空心金属管和绝缘套管之间由绝缘支架连接保证了两者之间的大气压环境而防止击穿。As an improvement, the straight rod electrode includes a hollow metal tube, an insulating bracket and an insulating sleeve from the inside to the outside. The outer wall of the hollow metal tube is connected to the inner wall of the insulating sleeve through a plurality of insulating brackets arranged circumferentially along the outer wall of the hollow metal tube, and the hollow metal tube and the insulating sleeve are coaxially arranged. With this structure, the hollow metal tube is protected by the insulating sleeve to prevent it from being directly exposed and etched by plasma, which significantly reduces the equipment failure rate and maintenance cost. Ultrapure water for cooling circulates inside the hollow metal tube during the cleaning process. The hollow metal tube and the insulating sleeve are connected by the insulating bracket to ensure an atmospheric pressure environment between the two to prevent breakdown.

作为改进,反应室的两个相对侧壁上均设有若干通孔,直杆电极两端分别插接在相对的两个通孔内并通过密封圈密封;采用此种结构,提高直杆电极与反应室之间的密封性。As an improvement, a plurality of through holes are provided on two opposite side walls of the reaction chamber, and the two ends of the straight rod electrode are respectively inserted into the two opposite through holes and sealed by a sealing ring; this structure improves the sealing between the straight rod electrode and the reaction chamber.

作为改进,反应室内设有用于为石墨舟加热的加热管;采用此种结构,用于在清洗工艺开始前烘舟去除水汽,防止清洗过程中产生氢氟酸(HF)造成污染和安全隐患。As an improvement, a heating tube for heating the graphite boat is provided in the reaction chamber; this structure is used to dry the boat to remove water vapor before the cleaning process begins, thereby preventing the generation of hydrofluoric acid (HF) during the cleaning process from causing pollution and safety hazards.

作为改进,偏压电极板包括四块呈矩阵式分布的子电极板,相邻子电极板之间均通过绝缘隔块连接,子电极板的偏压能够独立控制通断;采用此种结构,分块偏压实现多种清洗模式,提高清洗效果的同时保证清洗效率。As an improvement, the bias electrode plate includes four sub-electrode plates distributed in a matrix. Adjacent sub-electrode plates are connected by insulating spacers, and the bias of the sub-electrode plates can be independently controlled on and off. With this structure, the block bias can realize multiple cleaning modes, improving the cleaning effect while ensuring the cleaning efficiency.

作为改进,反应室内部底端连接有绝缘隔层,绝缘隔层上端面设有凹槽,偏压电极板连接在凹槽内并由绝缘隔层包覆偏压电极板周向的每个侧壁;采用此种结构,用于防止偏压电极板与反应室侧壁或底端之间击穿打火。As an improvement, an insulating barrier is connected to the bottom end of the interior of the reaction chamber, a groove is provided on the upper end surface of the insulating barrier, the bias electrode plate is connected in the groove and each circumferential side wall of the bias electrode plate is covered by the insulating barrier; this structure is used to prevent breakdown and sparking between the bias electrode plate and the side wall or bottom end of the reaction chamber.

作为改进,反应室前侧壁上设有主进气口,反应室左右侧壁上各设有一辅助进气口;采用此种结构,不同进气方式实现多种清洗模式,提高清洗效果的同时保证清洗效率。As an improvement, a main air inlet is provided on the front side wall of the reaction chamber, and an auxiliary air inlet is provided on each of the left and right side walls of the reaction chamber; with this structure, different air intake methods can achieve multiple cleaning modes, improving the cleaning effect while ensuring cleaning efficiency.

本发明的第二个目的在于提供一种基于直杆天线ICP的石墨舟清洗方法,使用上述的基于直杆天线ICP的石墨舟清洗设备,包括以下步骤:The second object of the present invention is to provide a graphite boat cleaning method based on straight rod antenna ICP, using the above-mentioned graphite boat cleaning device based on straight rod antenna ICP, comprising the following steps:

S1、将石墨舟送入反应腔内并置于设定位置;S1. Send the graphite boat into the reaction chamber and place it at a set position;

S2、对反应腔抽真空至设定的真空值并通过监控真空值来检测反应腔是否泄漏;若反应腔未泄漏,则进入下一步;S2, evacuating the reaction chamber to a set vacuum value and detecting whether the reaction chamber leaks by monitoring the vacuum value; if the reaction chamber does not leak, proceeding to the next step;

S3、利用设置于反应室内的加热管对石墨舟进行烘舟,持续300-600s;S3, using a heating tube disposed in the reaction chamber to dry the graphite boat for 300-600 seconds;

S4、利用干燥氮气吹扫反应腔内由烘舟产生的水蒸气;S4, using dry nitrogen to purge the water vapor generated by the drying boat in the reaction chamber;

S5、对反应腔抽真空至设定的真空值;S5, evacuating the reaction chamber to a set vacuum value;

S6、从设于反应室前侧壁上的主进气口通入Ar并调整反应腔压力至设定范围;S6, introducing Ar from the main air inlet provided on the front side wall of the reaction chamber and adjusting the pressure of the reaction chamber to a set range;

S7、开启射频电源并调节射频电源功率至额定功率的10%-30%,启辉后根据负载端电压电流及阻抗检测放电状态是否正常;若放电状态正常,则进入下一步;S7, turn on the RF power supply and adjust the RF power supply to 10%-30% of the rated power. After starting, check whether the discharge state is normal according to the voltage, current and impedance of the load end; if the discharge state is normal, proceed to the next step;

S8、从主进气口和设于反应室左右侧壁上的辅助进气口以线性增长的速率通入反应气体,同时以相同线性减小的速率逐渐减小Ar通入,此过程中维持反应腔内气压恒定;S8, introducing the reaction gas from the main gas inlet and the auxiliary gas inlets provided on the left and right side walls of the reaction chamber at a linearly increasing rate, and at the same time gradually reducing the Ar introduction at the same linearly decreasing rate, during which the gas pressure in the reaction chamber is maintained constant;

S9、将射频功率调整至额定功率的50%-90%,偏压电极板接通偏压开始清洗;S9, adjust the RF power to 50%-90% of the rated power, connect the bias electrode plate to the bias and start cleaning;

S10、关闭射频电源,偏压电极板断开偏压;S10, turning off the radio frequency power supply, and disconnecting the bias voltage of the bias electrode plate;

S11、对反应腔抽真空后通入氮气使得反应腔气压恢复大气压,循环若干次;S11, evacuate the reaction chamber and introduce nitrogen to return the pressure of the reaction chamber to atmospheric pressure, and repeat the cycle several times;

S12、清洗结束,取出石墨舟。S12. After cleaning is completed, the graphite boat is taken out.

采用上述方法后,本发明中的一种基于直杆天线ICP的石墨舟清洗方法具有以下优点:将ICP中常规的螺旋线圈或平面线圈拆分成直杆电极并联形式,阻抗较低,便于控制整体阻抗,能够适配市面上主流射频电源及匹配器,通过增减直杆电极的数量还可适配不同尺寸的反应腔与石墨舟,无需定制化电极,材料及加工成本低,相比于CCP而言,电离率更高,清洗效果更好,工作气压更低,能够减少特气的使用;此外,单梳型的布局形式结构简单,双梳型通过电场调制能够进一步提高等离子体均匀性,适用于对清洗要求更高的场合,双梳型与U型相结合是在双梳型的基础上减小了射频电源和匹配器的使用,降低成本,适用于更大尺寸石墨舟的处理需求;另外,步骤S3中烘舟去除水蒸气,防止清洗过程中产生氢氟酸(HF)造成污染和安全隐患;利用步骤S7排除故障,防止反应腔内部绝缘老化,或者电源、匹配器故障。After adopting the above method, a graphite boat cleaning method based on straight-rod antenna ICP in the present invention has the following advantages: the conventional spiral coil or planar coil in ICP is split into a parallel form of straight-rod electrodes, the impedance is low, it is easy to control the overall impedance, and it can be adapted to the mainstream RF power supply and matching device on the market. By increasing or decreasing the number of straight-rod electrodes, it can also be adapted to reaction chambers and graphite boats of different sizes, without the need for customized electrodes, and the material and processing costs are low. Compared with CCP, it has a higher ionization rate, better cleaning effect, and lower working gas pressure, which can reduce the use of special gases; in addition, the single-comb type has a simple layout structure, and the double-comb type can further improve the plasma uniformity through electric field modulation, which is suitable for occasions with higher cleaning requirements. The combination of the double-comb type and the U-type reduces the use of RF power supply and matching device on the basis of the double-comb type, reduces costs, and is suitable for the processing requirements of larger-sized graphite boats; in addition, the boat is baked in step S3 to remove water vapor to prevent the generation of hydrofluoric acid (HF) during the cleaning process from causing pollution and safety hazards; step S7 is used to troubleshoot to prevent insulation aging inside the reaction chamber, or power supply and matching device failure.

作为改进,步骤S9包括:As an improvement, step S9 includes:

S9-1、第一阶段清洗:偏压电极板中的四个子电极板均接通偏压,持续2-3h;S9-1, first stage cleaning: the four sub-electrode plates in the bias electrode plate are all connected to the bias for 2-3 hours;

S9-2、第二阶段清洗:关闭主进气口,同时左侧两块子电极板断开偏压,持续0.5-1h;S9-2, second stage cleaning: close the main air inlet and disconnect the bias voltage of the two left sub-electrode plates for 0.5-1h;

S9-3、第三阶段清洗:左侧两块子电极板接通偏压,右侧两块子电极板断开偏压,持续0.5-1h;S9-3, third stage cleaning: the two left sub-electrode plates are biased, and the two right sub-electrode plates are biased, which lasts for 0.5-1h;

S9-4、第四阶段清洗:以逆时针或顺时针方向依次使各个子电极板接通偏压,每个子电极板的接通时间持续10-30min;S9-4, fourth stage cleaning: connect the bias voltage to each sub-electrode plate in turn in a counterclockwise or clockwise direction, and the connection time of each sub-electrode plate lasts for 10-30 minutes;

S9-5、第五阶段清洗:辅助进气口关闭,保持反应腔内气体静止恒压,所有子电极板接通偏压,持续10-30min;采用此种方法,通过主进气口和辅助进气口及分块偏压的不同组合,实现多种清洗模式,在提高清洗效果的同时保证清洗效率。S9-5, fifth stage cleaning: the auxiliary air inlet is closed, the gas in the reaction chamber is kept at a static constant pressure, and all sub-electrode plates are connected to bias voltage for 10-30 minutes. By adopting this method, a variety of cleaning modes can be achieved through different combinations of main air inlet, auxiliary air inlet and block bias voltage, which can improve the cleaning effect while ensuring the cleaning efficiency.

附图说明BRIEF DESCRIPTION OF THE DRAWINGS

图1为本发明中石墨舟清洗设备的结构示意图。FIG. 1 is a schematic diagram of the structure of a graphite boat cleaning device according to the present invention.

图2为本发明中反应室的俯视图。FIG. 2 is a top view of the reaction chamber of the present invention.

图3为本发明中直杆电极的结构示意图。FIG. 3 is a schematic diagram of the structure of the straight rod electrode in the present invention.

图4为本发明中直杆电极单梳型布局示意图。FIG. 4 is a schematic diagram of a single comb-type layout of straight-rod electrodes in the present invention.

图5为本发明中直杆电极另一种单梳型布局示意图。FIG. 5 is a schematic diagram of another single-comb layout of the straight rod electrodes in the present invention.

图6为本发明中直杆电极双梳型布局示意图。FIG. 6 is a schematic diagram of a double-comb layout of straight-rod electrodes in the present invention.

图7为本发明中直杆电极另一种双梳型布局示意图。FIG. 7 is a schematic diagram of another double-comb layout of the straight rod electrodes in the present invention.

图8为本发明中直杆电极U型布局示意图。FIG8 is a schematic diagram of a U-shaped layout of straight rod electrodes in the present invention.

图9为本发明中直杆电极双梳型与U型相结合的布局示意图。FIG. 9 is a schematic diagram of the layout of the straight rod electrode combining double comb type and U type in the present invention.

图10为本发明中直杆电极另一种双梳型与U型相结合的布局示意图。FIG. 10 is a schematic diagram of another layout of a double-comb type and a U-type straight rod electrode in the present invention.

附图标记:1、反应室;2、反应腔;3、偏压电极板;31、子电极板;4、绝缘块;5、直杆电极;51、空心金属管;52、绝缘支架;53、绝缘套管;6、加热管;7、绝缘隔块;8、绝缘隔层;9、凹槽;10、主进气口;11、辅助进气口;12、馈入点;13、接地点。Figure numerals: 1. reaction chamber; 2. reaction cavity; 3. bias electrode plate; 31. sub-electrode plate; 4. insulating block; 5. straight rod electrode; 51. hollow metal tube; 52. insulating bracket; 53. insulating sleeve; 6. heating tube; 7. insulating spacer; 8. insulating barrier; 9. groove; 10. main air inlet; 11. auxiliary air inlet; 12. feeding point; 13. grounding point.

具体实施方式DETAILED DESCRIPTION

下面结合附图对本发明一种基于直杆天线ICP的石墨舟清洗设备及方法作详细说明。The following is a detailed description of a graphite boat cleaning device and method based on straight rod antenna ICP of the present invention in conjunction with the accompanying drawings.

如图1至图10所示,一种基于直杆天线ICP的石墨舟清洗设备,包括反应室1,反应室1内设有容纳石墨舟的反应腔2,反应腔2内设有偏压电极板3,具体地,如图1所示,反应室1内部底端连接有绝缘隔层8,用于防止偏压电极板3与反应室1的侧壁或底端之间击穿打火,绝缘隔层8优选四氟、陶瓷等绝缘、耐高温材料。绝缘隔层8上端面设有凹槽9,偏压电极板3连接在凹槽9内并由绝缘隔层8包覆偏压电极板3周向的每个侧壁。As shown in Figures 1 to 10, a graphite boat cleaning device based on a straight rod antenna ICP includes a reaction chamber 1, a reaction chamber 2 for accommodating a graphite boat is provided in the reaction chamber 1, and a bias electrode plate 3 is provided in the reaction chamber 2. Specifically, as shown in Figure 1, an insulating barrier 8 is connected to the bottom end of the reaction chamber 1 to prevent the bias electrode plate 3 from breaking down and sparking with the side wall or bottom end of the reaction chamber 1. The insulating barrier 8 is preferably made of insulating and high temperature resistant materials such as polytetrafluoroethylene and ceramics. A groove 9 is provided on the upper end surface of the insulating barrier 8, and the bias electrode plate 3 is connected in the groove 9 and each side wall of the bias electrode plate 3 is covered by the insulating barrier 8.

如图2所示,偏压电极板3包括四块呈矩阵式分布的子电极板31,相邻子电极板31之间均通过绝缘隔块7连接,使得绝缘隔块7整体呈十字形。本实施例中,偏压电极板3材料选用不锈钢、铝合金等耐F等离子体刻蚀的材料,而绝缘隔块7采用四氟长条,子电极板31的偏压能够独立控制通断,给带电粒子施加水平方向的电场力,改善石墨舟侧壁的清洗效果,并且,偏压电极板3整体的面积大于石墨舟的面积,也就是说在竖直方向上的投影中,石墨舟落在偏压电极板3内,偏压可选用直流或交流偏压,通过偏压提高电子/离子温度及刻蚀速率,提高整体清洗均匀性。As shown in FIG2 , the bias electrode plate 3 includes four sub-electrode plates 31 distributed in a matrix, and adjacent sub-electrode plates 31 are connected by insulating spacers 7, so that the insulating spacers 7 are cross-shaped as a whole. In this embodiment, the bias electrode plate 3 is made of stainless steel, aluminum alloy and other materials resistant to F plasma etching, and the insulating spacers 7 are made of polytetrafluoroethylene strips. The bias of the sub-electrode plate 31 can be independently controlled to be turned on and off, and a horizontal electric field force is applied to the charged particles to improve the cleaning effect of the side wall of the graphite boat. In addition, the overall area of the bias electrode plate 3 is larger than the area of the graphite boat, that is, in the vertical projection, the graphite boat falls inside the bias electrode plate 3. The bias can be selected as a DC or AC bias, and the electron/ion temperature and etching rate are increased by the bias, thereby improving the overall cleaning uniformity.

如图1所示,偏压电极板3上设有用于放置石墨舟的绝缘块4,用于支撑固定石墨舟同时将石墨舟与下方偏压电极板3电隔绝,绝缘块4优选陶瓷、四氟等材料。As shown in FIG1 , an insulating block 4 for placing a graphite boat is provided on the bias electrode plate 3 to support and fix the graphite boat while electrically isolating the graphite boat from the bias electrode plate 3 below. The insulating block 4 is preferably made of ceramic, polytetrafluoroethylene or other materials.

反应室1内连接有若干直杆电极5,如图1所示的虚线框区域即直杆电极5的安装区域,其位于石墨舟的上方,若干直杆电极5水平设置且相互平行,每根直杆电极5的长度方向与石墨舟长度方向在空间上垂直设置,直杆电极5的数量根据石墨舟长度而定,并且直杆电极5两端在竖直方向上的投影均超出石墨舟,如图4至图10所示,若干直杆电极5并联呈单梳型、双梳型、U型、双梳型与U型相结合的其中一种布局;如图4所示为最基础的单梳型布局;如图5所示为单梳型布局并且馈入点12和接地点13呈对角分布,其优点是每路产生的等离子体均一性好,成本低,适合小型、试验型石墨舟的清洗;如图6和图7所示为两种双梳型布局,通过电场调制进一步提高等离子体均匀性,适用于对清洗要求更高的场合;如图9和图10所示为双梳型与U型相结合的布局,所谓双梳型与U型相结合就是指若干直杆电极5先布局呈U型的形式,然后在U型的基础上参考双梳型布局再连接一个射频电源,其优点是在双梳型的基础上减少射频电源和匹配器的使用,降低成本,适用于大尺寸石墨舟的处理需求。此外,需要说明的是,如图6、图7、图9、图10所示的具有两个射频电源的布局形式中,采用实线与虚线分别表示两个射频电源与接地的连线。A plurality of straight-rod electrodes 5 are connected in the reaction chamber 1. The dotted-line frame area shown in FIG1 is the installation area of the straight-rod electrodes 5, which is located above the graphite boat. The plurality of straight-rod electrodes 5 are arranged horizontally and parallel to each other. The length direction of each straight-rod electrode 5 is vertically arranged in space with the length direction of the graphite boat. The number of straight-rod electrodes 5 is determined according to the length of the graphite boat, and the projections of both ends of the straight-rod electrodes 5 in the vertical direction exceed the graphite boat. As shown in FIG4 to FIG10, the plurality of straight-rod electrodes 5 are connected in parallel to form a single-comb type, a double-comb type, a U-type, or a combination of a double-comb type and a U-type. FIG4 shows the most basic single-comb type layout; FIG5 shows a single-comb type layout and the feed point 12 and the connection point 12 are connected to the feed point 12. Location 13 is diagonally distributed, and its advantage is that the plasma generated in each path is uniform and low in cost, which is suitable for cleaning of small and experimental graphite boats; as shown in Figures 6 and 7, there are two double-comb layouts, which further improve the plasma uniformity through electric field modulation, and are suitable for occasions with higher cleaning requirements; as shown in Figures 9 and 10, there is a layout combining double-comb and U-type. The so-called combination of double-comb and U-type means that a number of straight rod electrodes 5 are first arranged in the form of a U-shape, and then a radio frequency power supply is connected based on the U-shape with reference to the double-comb layout. Its advantage is that the use of radio frequency power supply and matching device is reduced on the basis of the double-comb type, and the cost is reduced, which is suitable for the processing requirements of large-sized graphite boats. In addition, it should be noted that in the layout forms with two radio frequency power supplies shown in Figures 6, 7, 9, and 10, solid lines and dotted lines are used to represent the connection lines between the two radio frequency power supplies and the ground respectively.

如图3所示,直杆电极5由内向外依次包括空心金属管51、绝缘支架52和绝缘套管53,空心金属管51外壁通过若干个沿空心金属管51外壁周向设置的绝缘支架52与绝缘套管53内壁连接,空心金属管51与绝缘套管53同轴设置;其中,空心金属管51材料优选紫铜,也可选用不锈钢、铝合金等具有较高强度和耐腐蚀性的材料,空心金属管51外径10-15mm,壁厚2mm;绝缘支架52为镂空支架,材料优选为四氟、陶瓷等,绝缘支架52厚度2-10mm;绝缘套管53材料优选为氧化铝陶瓷,也可选用耐F等离子体刻蚀的其他绝缘材料,绝缘套管53外径15-30mm,壁厚2mm;空心金属管51内部在整个清洗过程中通入冷却用的超纯水(电阻率18MΩ·cm,电导率0.055μS/cm)。As shown in FIG3 , the straight rod electrode 5 includes a hollow metal tube 51, an insulating bracket 52 and an insulating sleeve 53 from the inside to the outside. The outer wall of the hollow metal tube 51 is connected to the inner wall of the insulating sleeve 53 through a plurality of insulating brackets 52 arranged circumferentially along the outer wall of the hollow metal tube 51, and the hollow metal tube 51 and the insulating sleeve 53 are arranged coaxially. The hollow metal tube 51 is preferably made of copper, and materials with high strength and corrosion resistance such as stainless steel and aluminum alloy can also be selected. The outer diameter of the hollow metal tube 51 is 10-15 mm and the wall thickness is 2 mm. The insulating bracket 52 is a hollow bracket, and the material is preferably polytetrafluoroethylene, ceramics, etc., and the thickness of the insulating bracket 52 is 2-10 mm. The material of the insulating sleeve 53 is preferably alumina ceramic, and other insulating materials resistant to F plasma etching can also be selected. The outer diameter of the insulating sleeve 53 is 15-30 mm and the wall thickness is 2 mm. Ultrapure water (resistivity 18 MΩ·cm, conductivity 0.055 μS/cm) for cooling is passed into the hollow metal tube 51 during the entire cleaning process.

如图1所示,反应室1内设有用于为石墨舟加热的加热管6,加热管6由另外设置的支架悬空架设,用于在清洗工艺开始前烘舟去除水汽,防止清洗过程中产生氢氟酸(HF)造成污染和安全隐患;加热管6外侧套管材料优选氧化铝陶瓷,也可选用耐F等离子体刻蚀的其他绝缘材料。As shown in FIG1 , a heating tube 6 for heating the graphite boat is provided in the reaction chamber 1. The heating tube 6 is suspended by a bracket provided separately and is used to remove water vapor from the boat before the cleaning process starts, so as to prevent the generation of hydrofluoric acid (HF) during the cleaning process from causing pollution and potential safety hazards. The outer sleeve material of the heating tube 6 is preferably alumina ceramic, and other insulating materials resistant to F plasma etching may also be selected.

反应室1采用长方体型设计或近似长方体型设计,反应腔2尺寸与石墨舟尺寸适配,可以完全容纳石墨舟,且具有等离子体发生所需空间及机械运动空间;反应室1包括可开关的前后两侧端盖、上下底板及左右侧板,反应室1一侧端盖为进舟侧,通过开启端盖以便于取放舟机构将石墨舟水平送入清洗反应腔2内;取放舟机构包含缓存平台,缓存平台上有一套针对石墨舟的快速定位装置,该定位装置通过以石墨舟底部及一侧端面的平面为基准面,通过定位块与基准面接触将石墨舟位置准确固定;取放舟机构包含一套传动机构,可以将石墨舟沿着清洗反应腔2水平进出传送,也可以将石墨舟在反应腔2外进行上下传送以传送至不同的反应腔2,也可以将石墨舟摆放至缓存平台以备其他工艺取放,取放舟机构的具体结构为现有技术,在此不再赘述。The reaction chamber 1 is designed in a rectangular shape or a design approximately similar to a rectangular shape. The size of the reaction chamber 2 is adapted to the size of the graphite boat, can completely accommodate the graphite boat, and has the space required for plasma generation and mechanical movement space; the reaction chamber 1 includes switchable front and rear end covers, upper and lower bottom plates, and left and right side plates. The end cover on one side of the reaction chamber 1 is the boat inlet side. By opening the end cover, the graphite boat can be horizontally sent into the cleaning reaction chamber 2 by the boat taking and placing mechanism; the boat taking and placing mechanism includes a cache platform, and a set of rapid positioning devices for the graphite boat is provided on the cache platform. The positioning device uses the plane of the bottom and one end face of the graphite boat as the reference surface, and accurately fixes the position of the graphite boat through the contact of the positioning block with the reference surface; the boat taking and placing mechanism includes a transmission mechanism, which can transport the graphite boat horizontally in and out along the cleaning reaction chamber 2, or can transport the graphite boat up and down outside the reaction chamber 2 to different reaction chambers 2, or can place the graphite boat on the cache platform for other process taking and placing. The specific structure of the boat taking and placing mechanism is the existing technology and will not be repeated here.

反应室1的两个相对侧壁上均设有若干通孔,具体来说,反应室1左右两侧壁靠上相对位置留有等大小、等间距通孔用于固定直杆电极5,直杆电极5两端分别插接在相对的两个通孔内并通过密封圈密封,反应室1外壁面通孔处设有45度圆台型密封槽用于直杆电极5与反应室1之间的密封,密封圈优选氟橡胶密封圈,具体密封结构均为现有技术,在此不再赘述。A plurality of through holes are provided on the two opposite side walls of the reaction chamber 1. Specifically, through holes of equal size and equal spacing are left at relative positions on the upper left and right side walls of the reaction chamber 1 for fixing the straight rod electrode 5. The two ends of the straight rod electrode 5 are respectively inserted into the two opposite through holes and sealed by a sealing ring. A 45-degree frustoconical sealing groove is provided at the through hole on the outer wall of the reaction chamber 1 for sealing between the straight rod electrode 5 and the reaction chamber 1. The sealing ring is preferably a fluororubber sealing ring. The specific sealing structure is all existing technology and will not be repeated here.

如图2所示,反应室1前侧壁上设有主进气口10,反应室1左右侧壁上各设有一辅助进气口11,而在反应室1后侧壁上则设有一出气口,左右侧壁的进气是为了补偿石墨舟侧面的清洗效果,因为前侧的进气是自前向后从石墨舟叶片之间穿过去的,对侧壁的作用较弱,辅助进气口11的气流对石墨舟侧壁有一个垂直方向的作用;优选地,辅助进气口11,位置要在中线偏前的位置,这样从前至后对石墨舟主要部分都有作用效果。As shown in FIG2 , a main air inlet 10 is provided on the front side wall of the reaction chamber 1, an auxiliary air inlet 11 is provided on the left and right side walls of the reaction chamber 1, and an air outlet is provided on the rear side wall of the reaction chamber 1. The air intake of the left and right side walls is to compensate for the cleaning effect of the side of the graphite boat, because the air intake on the front side passes through between the blades of the graphite boat from front to back, and the effect on the side wall is weaker. The airflow of the auxiliary air inlet 11 has a vertical effect on the side wall of the graphite boat; preferably, the auxiliary air inlet 11 is located in front of the center line, so that it has an effect on the main part of the graphite boat from front to back.

此外,本实施例中还涉及一种基于直杆天线ICP的石墨舟清洗方法,使用上述的基于直杆天线ICP的石墨舟清洗设备,包括以下步骤:In addition, this embodiment also relates to a graphite boat cleaning method based on the straight rod antenna ICP, using the above-mentioned graphite boat cleaning device based on the straight rod antenna ICP, comprising the following steps:

S1、将石墨舟送入反应腔2内并置于设定位置,具体来说是将待清洗的石墨舟放入取放舟机构的缓存平台上,通过缓存平台自定位作用对石墨舟位置进行定位,通过取放舟机构将将石墨舟送入等离子清洗反应腔2内设定的位置;S1, sending the graphite boat into the reaction chamber 2 and placing it at a set position, specifically, placing the graphite boat to be cleaned on the buffer platform of the boat-pick-up and -release mechanism, positioning the graphite boat through the self-positioning function of the buffer platform, and sending the graphite boat to the set position in the plasma cleaning reaction chamber 2 through the boat-pick-up and -release mechanism;

S2、对反应腔2抽真空至设定的真空值并通过监控真空值来检测反应腔2是否泄漏;若反应腔2未泄漏,则进入下一步;若反应腔2泄漏,则停止清洗程序,对反应腔2进行检查;S2, evacuating the reaction chamber 2 to a set vacuum value and detecting whether the reaction chamber 2 is leaking by monitoring the vacuum value; if the reaction chamber 2 is not leaking, proceeding to the next step; if the reaction chamber 2 is leaking, stopping the cleaning procedure and inspecting the reaction chamber 2;

S3、利用设置于反应室1内的加热管6对石墨舟进行烘舟,持续300-600s;S3, using the heating tube 6 disposed in the reaction chamber 1 to dry the graphite boat for 300-600 seconds;

S4、利用干燥氮气吹扫反应腔2内由烘舟产生的水蒸气,氮气吹扫持续三次;S4, using dry nitrogen to purge the water vapor generated by the drying boat in the reaction chamber 2, and the nitrogen purge is continued three times;

S5、对反应腔2抽真空至设定的真空值;S5, evacuating the reaction chamber 2 to a set vacuum value;

S6、从设于反应室1前侧壁上的主进气口10通入Ar并调整反应腔2压力至设定范围(1-50pa);S6, introducing Ar from the main air inlet 10 provided on the front side wall of the reaction chamber 1 and adjusting the pressure of the reaction chamber 2 to a set range (1-50 Pa);

S7、反应腔2压力稳定后,开启射频电源并调节射频电源功率至额定功率的10%-30%,启辉后根据负载端电压电流及阻抗检测放电状态是否正常;若放电状态正常,则进入下一步;若放电状态异常,则停止清洗程序并排除故障;其中,射频电源额定功率的选用根据要清洗的石墨舟而定,具体来说,石墨舟的尺寸越大,选定的射频电源额定功率也越高,具体选用功率需要根据实际清洗效果调试决定;S7. After the pressure of reaction chamber 2 is stable, turn on the RF power supply and adjust the RF power supply power to 10%-30% of the rated power. After starting, detect whether the discharge state is normal according to the voltage, current and impedance of the load end; if the discharge state is normal, proceed to the next step; if the discharge state is abnormal, stop the cleaning procedure and troubleshoot; the selection of the rated power of the RF power supply depends on the graphite boat to be cleaned. Specifically, the larger the size of the graphite boat, the higher the rated power of the selected RF power supply. The specific power selection needs to be determined according to the actual cleaning effect.

S8、从主进气口10和设于反应室1左右侧壁上的辅助进气口11以线性增长的速率通入反应气体,同时以相同线性减小的速率逐渐减小Ar通入,此过程中维持反应腔2内气压恒定,优选的反应气体包括以下气体中的任意一种:三氟化氮、四氟化碳、六氟化硫、六氟乙烷、八氟丙烷等,可选择氧气、二氧化碳中的任意一种进行混合;S8, introducing the reaction gas from the main gas inlet 10 and the auxiliary gas inlet 11 provided on the left and right side walls of the reaction chamber 1 at a linearly increasing rate, and gradually reducing the Ar introduced at the same linearly decreasing rate, during which the gas pressure in the reaction chamber 2 is maintained constant, and the preferred reaction gas includes any one of the following gases: nitrogen trifluoride, carbon tetrafluoride, sulfur hexafluoride, hexafluoroethane, octafluoropropane, etc., and any one of oxygen and carbon dioxide can be selected for mixing;

S9、将射频功率调整至额定功率的50%-90%,偏压电极板3接通偏压开始清洗;S9, adjusting the RF power to 50%-90% of the rated power, connecting the bias electrode plate 3 to the bias voltage and starting cleaning;

S10、关闭射频电源,偏压电极板3断开偏压;S10, turning off the radio frequency power supply, and disconnecting the bias voltage of the bias electrode plate 3;

S11、对反应腔2抽真空后通入氮气使得反应腔2气压恢复大气压,循环若干次;S11, after evacuating the reaction chamber 2, nitrogen is introduced to restore the pressure of the reaction chamber 2 to atmospheric pressure, and the cycle is repeated several times;

S12、清洗结束,取出石墨舟。S12. After cleaning is completed, the graphite boat is taken out.

其中,步骤S9包括:Wherein, step S9 comprises:

S9-1、第一阶段清洗:偏压电极板3中的四个子电极板31均接通偏压,持续2-3h;S9-1, first stage cleaning: the four sub-electrode plates 31 in the bias electrode plate 3 are all biased for 2-3 hours;

S9-2、第二阶段清洗:关闭主进气口10,同时左侧两块子电极板31断开偏压,持续0.5-1h;S9-2, second stage cleaning: close the main air inlet 10, and disconnect the bias voltage of the two left sub-electrode plates 31, for 0.5-1h;

S9-3、第三阶段清洗:左侧两块子电极板31接通偏压,右侧两块子电极板31断开偏压,持续0.5-1h;S9-3, third stage cleaning: the two left sub-electrode plates 31 are biased, and the two right sub-electrode plates 31 are biased, which lasts for 0.5-1h;

S9-4、第四阶段清洗:针对沉积物较厚、较难清理的舟角区域做局部加强清洗,以逆时针或顺时针方向依次使各个子电极板31接通偏压,每个子电极板31的接通时间持续10-30min,本实施例中以如图2所示中的标号为A的子电极板31开始以顺时针方向依次接通各个子电极板31;S9-4, fourth stage cleaning: local enhanced cleaning is performed on the corner area of the boat where the deposits are thick and difficult to clean, and each sub-electrode plate 31 is connected to the bias in a counterclockwise or clockwise direction in turn. The connection time of each sub-electrode plate 31 lasts for 10-30 minutes. In this embodiment, starting from the sub-electrode plate 31 labeled A in FIG. 2 , each sub-electrode plate 31 is connected in a clockwise direction in turn;

S9-5、第五阶段清洗:辅助进气口11关闭,保持反应腔2内气体静止恒压,所有子电极板31接通偏压,持续10-30min,针对前期清洗阶段中由于气流影响导致清洗不彻底的区域做补偿清洗。S9-5, fifth stage cleaning: the auxiliary air inlet 11 is closed, the gas in the reaction chamber 2 is kept static and at a constant pressure, all sub-electrode plates 31 are biased for 10-30 minutes, and compensation cleaning is performed for the areas that were not thoroughly cleaned due to the influence of airflow in the previous cleaning stage.

本发明采用基于等离子体的干式清洗法清除石墨舟上附着的poly材料,相比传统湿法清洗具有耗时短、污染小、步骤简便、无需拆解石墨舟等优点;采用ICP,相比CCP结构具有电离率高的优点,能产生更多F离子,对于以化学反应为主要过程的硅材料清洗而言能显著提高清洗效率;并且工作气压很低,相比CCP能减少特气的使用,降低成本;将ICP中常规的螺旋线圈或平面线圈拆分成直杆电极5并联形式,阻抗较低,便于控制整体阻抗,能够适配市面上主流射频电源及匹配器,通过增减直杆电极5的数量还可适配不同尺寸的反应腔2与石墨舟,无需定制化电极,材料及加工成本低;直杆电极5外套有绝缘套管53,避免了空心金属管51直接裸露而受到等离子体刻蚀,显著降低了设备故障率和维护成本;单梳型的布局形式结构简单,双梳型通过电场调制能够进一步提高等离子体均匀性,适用于对清洗要求更高的场合,双梳型与U型相结合是在双梳型的基础上减小了射频电源和匹配器的使用,降低成本,适用于更大尺寸石墨舟的处理需求;采用加热管6,在清洗之前先烘舟去除残余水分,避免清洗过程中产生HF造成污染和安全隐患;通过进气形式及分块偏压的不同组合,实现多种清洗模式,在提高清洗效果的同时保证清洗效率。The present invention adopts a plasma-based dry cleaning method to remove the poly material attached to the graphite boat. Compared with traditional wet cleaning, it has the advantages of short time consumption, low pollution, simple steps, and no need to disassemble the graphite boat. ICP is adopted, which has the advantage of high ionization rate compared with CCP structure and can produce more F ions. For silicon material cleaning with chemical reaction as the main process, it can significantly improve the cleaning efficiency. In addition, the working gas pressure is very low, which can reduce the use of special gases and reduce costs compared with CCP. The conventional spiral coil or planar coil in ICP is split into a parallel form of straight rod electrodes 5, which has low impedance and is easy to control the overall impedance. It can be adapted to mainstream radio frequency power supplies and matchers on the market. By increasing or decreasing the number of straight rod electrodes 5, it can also adapt to reaction chambers 2 and graphite boats of different sizes without the need for customized electrodes. , low material and processing costs; the straight rod electrode 5 is covered with an insulating sleeve 53, which prevents the hollow metal tube 51 from being directly exposed and etched by plasma, significantly reducing the equipment failure rate and maintenance cost; the single-comb type has a simple layout structure, and the double-comb type can further improve the plasma uniformity through electric field modulation, which is suitable for occasions with higher cleaning requirements. The combination of the double-comb type and the U-type reduces the use of RF power supply and matching device on the basis of the double-comb type, reduces costs, and is suitable for the processing requirements of larger-sized graphite boats; a heating tube 6 is used to dry the boat before cleaning to remove residual moisture, so as to avoid HF pollution and safety hazards during the cleaning process; a variety of cleaning modes are realized through different combinations of air intake forms and block bias voltages, which improves the cleaning effect while ensuring the cleaning efficiency.

上面结合附图对本发明的实施方式作了详细说明,但是本发明并不限于上述一种实施方式,本领域技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。The embodiments of the present invention are described in detail above in conjunction with the accompanying drawings, but the present invention is not limited to the above-mentioned one embodiment, and all other embodiments obtained by those skilled in the art without making any creative work are within the scope of protection of the present invention.

Claims (10)

1.一种基于直杆天线ICP的石墨舟清洗设备,其特征在于,包括反应室(1),所述反应室(1)内设有容纳石墨舟的反应腔(2),所述反应腔(2)内设有偏压电极板(3),所述偏压电极板(3)上设有用于放置石墨舟的绝缘块(4),所述反应室(1)内连接有若干直杆电极(5),若干所述直杆电极(5)水平设置且相互平行,当石墨舟放置在所述绝缘块(4)上时,每根所述直杆电极(5)均位于石墨舟上方且每根所述直杆电极(5)的长度方向与石墨舟长度方向在空间上垂直设置,若干所述直杆电极(5)并联呈单梳型、双梳型、U型、双梳型与U型相结合的其中一种布局;1. A graphite boat cleaning device based on straight-rod antenna ICP, characterized in that it comprises a reaction chamber (1), wherein the reaction chamber (1) is provided with a reaction cavity (2) for accommodating a graphite boat, wherein the reaction cavity (2) is provided with a bias electrode plate (3), wherein the bias electrode plate (3) is provided with an insulating block (4) for placing the graphite boat, wherein a plurality of straight-rod electrodes (5) are connected in the reaction chamber (1), wherein the plurality of straight-rod electrodes (5) are arranged horizontally and parallel to each other, wherein when the graphite boat is placed on the insulating block (4), each of the straight-rod electrodes (5) is located above the graphite boat and the length direction of each of the straight-rod electrodes (5) is arranged vertically in space with the length direction of the graphite boat, wherein the plurality of straight-rod electrodes (5) are connected in parallel to form a single comb type, a double comb type, a U-type, or a combination of the double comb type and the U-type; 单梳型布局为若干所述直杆电极(5)平行等间距布置,其中一端并联后连接射频电源,另一端并联后接地;The single comb type layout is that a plurality of straight rod electrodes (5) are arranged in parallel with equal spacing, one end of which is connected in parallel and connected to a radio frequency power supply, and the other end of which is connected in parallel and grounded; 双梳型布局为两组相同数量的所述直杆电极(5)平行等间距布置,其中一组自左侧并联后中间位置连接射频电源,自右侧并联后中间位置接地,另一组置于该组直杆电极(5)中间,自右侧并联后中间位置连接射频电源,自左侧并联后中间位置接地;或双梳型布局为两组直杆电极(5)采用相互间隔设置的形式平行等间距布置,其中一组自左侧并联后中间位置连接射频电源,自右侧并联后中间位置接地,另一组自右侧并联后中间位置连接射频电源,自左侧并联后中间位置接地;The double comb-type layout is that two groups of the same number of straight rod electrodes (5) are arranged in parallel and at equal intervals, one group is connected to the radio frequency power supply at the middle position after being connected in parallel on the left side, and is grounded at the middle position after being connected in parallel on the right side, and the other group is placed in the middle of the group of straight rod electrodes (5), is connected to the radio frequency power supply at the middle position after being connected in parallel on the right side, and is grounded at the middle position after being connected in parallel on the left side; or the double comb-type layout is that two groups of straight rod electrodes (5) are arranged in parallel and at equal intervals in the form of being set at a distance from each other, one group is connected to the radio frequency power supply at the middle position after being connected in parallel on the left side, and is grounded at the middle position after being connected in parallel on the right side, and the other group is connected to the radio frequency power supply at the middle position after being connected in parallel on the right side, and is grounded at the middle position after being connected in parallel on the left side; U型布局为两组相同数量的所述直杆电极(5)平行等间距布置,其中一组所述直杆电极(5)置于另一组的上方,位于上方的一组所述直杆电极(5)左侧并联后于中间位置连接射频电源,位于下方的一组所述直杆电极(5)左侧并联后中间位置接地,位于上方的一组所述直杆电极(5)右侧并联中间位置与位于下方的所述直杆电极(5)右侧并联中间位置连通;The U-shaped layout is that two groups of the same number of straight-rod electrodes (5) are arranged in parallel and at equal intervals, one group of the straight-rod electrodes (5) is placed above the other group, the left sides of the group of straight-rod electrodes (5) located above are connected in parallel and then connected to a radio frequency power supply at the middle position, the left sides of the group of straight-rod electrodes (5) located below are connected in parallel and then grounded at the middle position, and the middle position of the right sides of the group of straight-rod electrodes (5) located above are connected in parallel and are connected to the middle position of the right sides of the straight-rod electrodes (5) located below; 双梳型与U型相结合布局为两组相同数量的所述直杆电极(5)平行等间距布置,其中一组自上方左侧并联中间位置连接射频电源,自下方左侧并联中间位置接地,另一组自上方右侧并联中间位置连接射频电源,自下方右侧并联中间位置接地;或者双梳型与U型相结合布局为两组相同数量的所述直杆电极(5)平行等间距布置,其中一组自上方左侧并联中间位置连接射频电源,自下方左侧并联中间位置接地,另一组自下方左侧并联中间位置连接射频电源,自上方左侧并联中间位置接地。The double comb type and U type combined layout is that two groups of the same number of straight rod electrodes (5) are arranged in parallel and at equal intervals, one group is connected to the RF power supply from the middle position of the upper left parallel connection and is grounded from the middle position of the lower left parallel connection, and the other group is connected to the RF power supply from the middle position of the upper right parallel connection and is grounded from the middle position of the lower right parallel connection; or the double comb type and U type combined layout is that two groups of the same number of straight rod electrodes (5) are arranged in parallel and at equal intervals, one group is connected to the RF power supply from the middle position of the upper left parallel connection and is grounded from the middle position of the lower left parallel connection, and the other group is connected to the RF power supply from the middle position of the lower left parallel connection and is grounded from the middle position of the upper left parallel connection. 2.根据权利要求1所述的基于直杆天线ICP的石墨舟清洗设备,其特征在于,若干所述直杆电极(5)呈单梳型布局并且馈入点(12)和接地点(13)呈对角分布。2. The graphite boat cleaning device based on straight rod antenna ICP according to claim 1 is characterized in that the plurality of straight rod electrodes (5) are arranged in a single comb type and the feeding point (12) and the grounding point (13) are distributed diagonally. 3.根据权利要求1所述的基于直杆天线ICP的石墨舟清洗设备,其特征在于,所述直杆电极(5)由内向外依次包括空心金属管(51)、绝缘支架(52)和绝缘套管(53),所述空心金属管(51)外壁通过若干个沿所述空心金属管(51)外壁周向设置的绝缘支架(52)与所述绝缘套管(53)内壁连接,所述空心金属管(51)与所述绝缘套管(53)同轴设置。3. The graphite boat cleaning device based on straight rod antenna ICP according to claim 1 is characterized in that the straight rod electrode (5) comprises a hollow metal tube (51), an insulating bracket (52) and an insulating sleeve (53) from the inside to the outside, the outer wall of the hollow metal tube (51) is connected to the inner wall of the insulating sleeve (53) through a plurality of insulating brackets (52) arranged circumferentially along the outer wall of the hollow metal tube (51), and the hollow metal tube (51) and the insulating sleeve (53) are coaxially arranged. 4.根据权利要求1所述的基于直杆天线ICP的石墨舟清洗设备,其特征在于,所述反应室(1)的两个相对侧壁上均设有若干通孔,所述直杆电极(5)两端分别插接在相对的两个所述通孔内并通过密封圈密封。4. The graphite boat cleaning device based on straight rod antenna ICP according to claim 1 is characterized in that a plurality of through holes are provided on two opposite side walls of the reaction chamber (1), and two ends of the straight rod electrode (5) are respectively inserted into the two opposite through holes and sealed by sealing rings. 5.根据权利要求1所述的基于直杆天线ICP的石墨舟清洗设备,其特征在于,所述反应室(1)内设有用于为石墨舟加热的加热管(6)。5. The graphite boat cleaning device based on straight rod antenna ICP according to claim 1, characterized in that a heating tube (6) for heating the graphite boat is provided in the reaction chamber (1). 6.根据权利要求1所述的基于直杆天线ICP的石墨舟清洗设备,其特征在于,所述偏压电极板(3)包括四块呈矩阵式分布的子电极板(31),相邻所述子电极板(31)之间均通过绝缘隔块(7)连接,所述子电极板(31)的偏压能够独立控制通断。6. The graphite boat cleaning equipment based on straight rod antenna ICP according to claim 1 is characterized in that the bias electrode plate (3) includes four sub-electrode plates (31) distributed in a matrix, and adjacent sub-electrode plates (31) are connected by insulating spacers (7), and the bias of the sub-electrode plates (31) can be independently controlled on and off. 7.根据权利要求1所述的基于直杆天线ICP的石墨舟清洗设备,其特征在于,所述反应室(1)内部底端连接有绝缘隔层(8),所述绝缘隔层(8)上端面设有凹槽(9),所述偏压电极板(3)连接在所述凹槽(9)内并由所述绝缘隔层(8)包覆所述偏压电极板(3)周向的每个侧壁。7. The graphite boat cleaning device based on straight rod antenna ICP according to claim 1 is characterized in that an insulating barrier (8) is connected to the bottom of the reaction chamber (1), and a groove (9) is provided on the upper end surface of the insulating barrier (8), and the bias electrode plate (3) is connected in the groove (9) and each circumferential side wall of the bias electrode plate (3) is covered by the insulating barrier (8). 8.根据权利要求1所述的基于直杆天线ICP的石墨舟清洗设备,其特征在于,所述反应室(1)前侧壁上设有主进气口(10),所述反应室(1)左右侧壁上各设有一辅助进气口(11)。8. The graphite boat cleaning device based on straight rod antenna ICP according to claim 1 is characterized in that a main air inlet (10) is provided on the front side wall of the reaction chamber (1), and an auxiliary air inlet (11) is provided on each of the left and right side walls of the reaction chamber (1). 9.一种基于直杆天线ICP的石墨舟清洗方法,其特征在于,使用权利要求1至8任意一项所述的基于直杆天线ICP的石墨舟清洗设备,包括以下步骤:9. A graphite boat cleaning method based on straight rod antenna ICP, characterized in that the graphite boat cleaning device based on straight rod antenna ICP according to any one of claims 1 to 8 is used, comprising the following steps: S1、将石墨舟送入所述反应腔(2)内并置于设定位置;S1, sending a graphite boat into the reaction chamber (2) and placing it at a set position; S2、对所述反应腔(2)抽真空至设定的真空值并通过监控真空值来检测反应腔(2)是否泄漏;若所述反应腔(2)未泄漏,则进入下一步;S2, evacuating the reaction chamber (2) to a set vacuum value and detecting whether the reaction chamber (2) is leaking by monitoring the vacuum value; if the reaction chamber (2) is not leaking, proceeding to the next step; S3、利用设置于所述反应室(1)内的加热管(6)对石墨舟进行烘舟,持续300-600s;S3, using a heating tube (6) disposed in the reaction chamber (1) to dry the graphite boat for 300-600 seconds; S4、利用干燥氮气吹扫所述反应腔(2)内由烘舟产生的水蒸气;S4, using dry nitrogen to purge the water vapor generated by the drying boat in the reaction chamber (2); S5、对反应腔(2)抽真空至设定的真空值;S5, evacuating the reaction chamber (2) to a set vacuum value; S6、从设于所述反应室(1)前侧壁上的主进气口(10)通入Ar并调整所述反应腔(2)压力至设定范围;S6, introducing Ar from a main air inlet (10) provided on the front side wall of the reaction chamber (1) and adjusting the pressure of the reaction chamber (2) to a set range; S7、开启射频电源并调节射频电源功率至额定功率的10%-30%,启辉后根据负载端电压电流及阻抗检测放电状态是否正常;若放电状态正常,则进入下一步;S7, turn on the RF power supply and adjust the RF power supply to 10%-30% of the rated power. After starting, check whether the discharge state is normal according to the voltage, current and impedance of the load end; if the discharge state is normal, proceed to the next step; S8、从主进气口(10)和设于所述反应室(1)左右侧壁上的辅助进气口(11)以线性增长的速率通入反应气体,同时以相同线性减小的速率逐渐减小Ar通入,此过程中维持所述反应腔(2)内气压恒定;S8, introducing the reaction gas from the main gas inlet (10) and the auxiliary gas inlet (11) provided on the left and right side walls of the reaction chamber (1) at a linearly increasing rate, and at the same time gradually reducing the Ar introduction at the same linearly decreasing rate, during which the gas pressure in the reaction chamber (2) is maintained constant; S9、将射频功率调整至额定功率的50%-90%,所述偏压电极板(3)接通偏压开始清洗;S9, adjusting the radio frequency power to 50%-90% of the rated power, and connecting the bias electrode plate (3) to the bias to start cleaning; S10、关闭射频电源,偏压电极板(3)断开偏压;S10, turning off the radio frequency power supply, and disconnecting the bias voltage of the bias electrode plate (3); S11、对所述反应腔(2)抽真空后通入氮气使得所述反应腔(2)气压恢复大气压,循环若干次;S11, evacuating the reaction chamber (2) and introducing nitrogen gas so that the pressure of the reaction chamber (2) returns to atmospheric pressure, and repeating the cycle several times; S12、清洗结束,取出石墨舟。S12. After cleaning is completed, the graphite boat is taken out. 10.根据权利要求9所述的基于直杆天线ICP的石墨舟清洗方法,其特征在于,步骤S9包括:10. The graphite boat cleaning method based on straight rod antenna ICP according to claim 9, characterized in that step S9 comprises: S9-1、第一阶段清洗:所述偏压电极板(3)中的四个子电极板(31)均接通偏压,持续2-3h;S9-1, first stage cleaning: the four sub-electrode plates (31) in the bias electrode plate (3) are all connected to bias for 2-3 hours; S9-2、第二阶段清洗:关闭主进气口(10),同时左侧两块子电极板(31)断开偏压,持续0.5-1h;S9-2, second stage cleaning: close the main air inlet (10) and disconnect the bias voltage of the two left sub-electrode plates (31) for 0.5-1h; S9-3、第三阶段清洗:左侧两块子电极板(31)接通偏压,右侧两块子电极板(31)断开偏压,持续0.5-1h;S9-3, third stage cleaning: the two left sub-electrode plates (31) are biased, and the two right sub-electrode plates (31) are biased, for 0.5-1 h; S9-4、第四阶段清洗:以逆时针或顺时针方向依次使各个子电极板(31)接通偏压,每个子电极板(31)的接通时间持续10-30min;S9-4, fourth stage cleaning: connecting the bias voltage to each sub-electrode plate (31) in turn in a counterclockwise or clockwise direction, and the connection time of each sub-electrode plate (31) lasts for 10-30 minutes; S9-5、第五阶段清洗:辅助进气口(11)关闭,保持所述反应腔(2)内气体静止恒压,所有子电极板(31)接通偏压,持续10-30min。S9-5, fifth stage cleaning: the auxiliary air inlet (11) is closed, the gas in the reaction chamber (2) is kept at a static constant pressure, and all sub-electrode plates (31) are connected to bias voltage for 10-30 minutes.
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