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CN103086379A - A radiation intercepting device for a crucible for electron beam melting - Google Patents

A radiation intercepting device for a crucible for electron beam melting Download PDF

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CN103086379A
CN103086379A CN201310023866XA CN201310023866A CN103086379A CN 103086379 A CN103086379 A CN 103086379A CN 201310023866X A CN201310023866X A CN 201310023866XA CN 201310023866 A CN201310023866 A CN 201310023866A CN 103086379 A CN103086379 A CN 103086379A
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radiation
electron beam
crucible
furnace wall
interception cover
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CN103086379B (en
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谭毅
姜大川
石爽
温书涛
邹瑞洵
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Dalian University of Technology
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Dalian University of Technology
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Abstract

The invention belongs to the technical field of metallurgical smelting, and particularly relates to a special radiation interception device for electron beam smelting. In the device, a radiation interception cover is positioned above a smelting crucible and movably arranged at the top of a furnace wall through a sliding suspension rod, the radiation interception cover is movably connected with the sliding suspension rod through a suspension hinge buckle, the radiation interception cover is spherical, the concave surface of the radiation interception cover faces downwards, the focus point of the concave surface is positioned at the center of the smelting crucible, and an arc-shaped notch is formed in the radiation interception cover. The radiation interception cover has the advantages of simple structure, practical function and convenience in manufacture, and can intercept the heat radiation of the silicon melt and the electron beam reflected by the surface of the silicon melt and act on the surface of the silicon melt again, so that the energy utilization rate of the electron beam is greatly improved, and the amplitude is improved by 20-50%.

Description

一种电子束熔炼用坩埚的辐射拦截装置A radiation intercepting device for a crucible for electron beam melting

   the

技术领域 technical field

本发明属于冶金熔炼技术领域,特别涉及一种电子束熔炼用的辐射拦截专用装置。 The invention belongs to the technical field of metallurgical smelting, in particular to a radiation intercepting device for electron beam smelting.

背景技术 Background technique

目前,世界范围内制备太阳能电池用多晶硅材料已形成规模化生产,主要制备方法是改良西门子法,但其综合电耗高达170kW·h/kg,并且生产呈间断性,无法在Si的生产上形成连续作业,并且此法在流程的核心环节上采取了落后的热化学气相沉积,工艺流程的环节过多,一次转化率低,导致流程时间太长,增加了材耗、能耗成本。 At present, the preparation of polysilicon materials for solar cells has formed a large-scale production worldwide. The main preparation method is the improved Siemens method, but its comprehensive power consumption is as high as 170kW h/kg, and the production is intermittent, which cannot be formed in the production of Si. Continuous operation, and this method adopts backward thermal chemical vapor deposition in the core link of the process. There are too many links in the process flow, and the primary conversion rate is low, which leads to too long process time and increases material consumption and energy consumption costs.

为此,世界各国都在积极探索制备高纯硅材料的全新工艺方法,其中冶金法制备多晶硅由于具有生产周期短、污染小、成本低、工艺相对简单、规模大小可控等特点,被认为是最能有效地降低多晶硅生产成本的技术之一,目前已成为世界各国竞相研发的热点,电子束熔炼技术是冶金法制备太阳能级硅中重要的方法之一,它是利用高能量密度的电子束作为熔炼热源的工艺方法,可以有效降低多晶硅中的磷、铝、钙等蒸发性杂质,现有电子束熔炼过程中采用的坩埚多为水冷铜坩埚,这主要是由于其可重复利用,避免二次污染等优点。 For this reason, countries all over the world are actively exploring a new process for preparing high-purity silicon materials. Among them, the metallurgical method for preparing polysilicon is considered to be the most important technology due to its short production cycle, low pollution, low cost, relatively simple process, and controllable scale. One of the technologies that can most effectively reduce the production cost of polysilicon has become a hot spot in the research and development of countries all over the world. Electron beam melting technology is one of the important methods in the metallurgical preparation of solar-grade silicon. It uses electron beams with high energy density As a smelting heat source process, it can effectively reduce evaporative impurities such as phosphorus, aluminum, and calcium in polysilicon. Most of the crucibles used in the existing electron beam smelting process are water-cooled copper crucibles, mainly because they can be reused and avoid secondary Secondary pollution and other advantages.

由于熔炼过程中,硅材料与水冷铜坩埚直接接触,其导热性能比较好,致使水冷系统带走的热量较多,以前的坩埚设计者主要从减少水冷系统带走的热量入手来提高电子束能量的利用率,例如:增加坩埚衬底等方式。该方式虽能提高电子束能量利用率,但是不能无限制提高电子束能量利用率,如若想继续提高坩埚的能量利用率,还需要从其它方面入手。 Since the silicon material is in direct contact with the water-cooled copper crucible during the smelting process, its thermal conductivity is relatively good, resulting in more heat taken away by the water-cooling system. Previous crucible designers mainly started with reducing the heat taken away by the water-cooling system to increase the energy of the electron beam. The utilization rate, such as: increasing the crucible substrate and so on. Although this method can improve the energy utilization rate of the electron beam, it cannot increase the energy utilization rate of the electron beam without limit. If we want to continue to improve the energy utilization rate of the crucible, we need to start from other aspects.

发明内容 Contents of the invention

本发明为克服上述不足问题,提供一种电子束熔炼用坩埚的辐射拦截装置。该装置结构简单,采用辐射拦截罩将反射的热辐射和电子束能量拦截后反射回熔炼坩埚中继续作用于熔体之中,提高了电子束能量的利用效率。 In order to overcome the above disadvantages, the present invention provides a radiation intercepting device for a crucible for electron beam smelting. The device has a simple structure, adopts a radiation intercepting cover to intercept reflected thermal radiation and electron beam energy, and then reflects back into the melting crucible to continue acting on the melt, thereby improving the utilization efficiency of the electron beam energy.

本发明为实现上述目的所采用的技术方案是:一种电子束熔炼用坩埚的辐射拦截装置,包括辐射拦截罩,滑动悬挂杆和真空熔炼装置,真空熔炼装置中,炉壁内部为熔炼室,炉壁上安装有炉门,水冷托盘固定安装于炉壁底部,水冷托盘上开有进水口和出水口,熔炼坩埚固定安装于水冷托盘之上,真空泵组固定安装于炉壁之上,电子枪固定安装于炉壁顶部,其特征是:辐射拦截罩位于熔炼坩埚上方,且通过滑动悬挂杆活动安装于炉壁的顶部,辐射拦截罩与滑动悬挂杆之间通过悬挂铰接扣活动连接。 The technical solution adopted by the present invention to achieve the above object is: a radiation intercepting device for a crucible for electron beam smelting, including a radiation intercepting cover, a sliding suspension rod and a vacuum smelting device. In the vacuum smelting device, the inside of the furnace wall is a melting chamber, Furnace door is installed on the furnace wall, the water-cooling tray is fixedly installed on the bottom of the furnace wall, the water inlet and outlet are opened on the water-cooling tray, the melting crucible is fixed on the water-cooling tray, the vacuum pump group is fixed on the furnace wall, and the electron gun is fixed Installed on the top of the furnace wall, it is characterized in that: the radiation intercepting cover is located above the melting crucible, and is movably installed on the top of the furnace wall through a sliding suspension rod, and the radiation intercepting cover and the sliding suspension rod are movably connected by a suspension hinge buckle.

所述辐射拦截罩为球面形状,其凹面朝下,凹面聚焦点位于熔炼坩埚中心,其上还开有一个圆弧形缺口。 The radiation intercepting shield is in the shape of a spherical surface, with its concave surface facing downwards, the focal point of the concave surface is located at the center of the melting crucible, and an arc-shaped gap is opened on it.

所述辐射拦截罩位于熔炼坩埚上方10-30cm,其正投影为圆形,半径为15-40cm。 The radiation intercepting shield is located 10-30 cm above the melting crucible, and its orthographic projection is a circle with a radius of 15-40 cm.

所述辐射拦截罩材质为石英、304不锈钢、石墨或铜。 The radiation intercepting shield is made of quartz, 304 stainless steel, graphite or copper.

所述滑动悬挂杆为3-5根,每根滑动悬挂杆安装有独立的驱动装置。 There are 3-5 sliding suspension rods, and each sliding suspension rod is equipped with an independent driving device.

所述圆弧形缺口的半径为5-10cm。 The radius of the arc-shaped notch is 5-10cm.

本发明设备结构简单,功能实用,该装置具有以下优点: The device of the present invention is simple in structure and practical in function, and the device has the following advantages:

1. 辐射拦截罩可对硅熔体的热辐射进行拦截,通过拦截硅液面的辐射,使辐射被反射重新作用于硅液面,有效的减少了由于热辐射损失的能量,提高了电子束设备的能量利用率。 1. The radiation intercepting cover can intercept the thermal radiation of the silicon melt. By intercepting the radiation of the silicon liquid surface, the radiation is reflected and re-acted on the silicon liquid surface, which effectively reduces the energy lost due to thermal radiation and improves the electron beam. Energy utilization of the equipment.

2. 辐射拦截罩不仅能够拦截由于硅熔体产生的辐射,而且能够拦截电子束反射的能量,前人的研究表明,电子束能量利用率只有75%左右,主要原因是由于电子束轰击硅熔体液面时有25%的能量被反射,辐射拦截罩可以将该反射能量进行拦截,用于硅熔体的熔炼。 2. The radiation intercepting shield can not only intercept the radiation generated by the silicon melt, but also intercept the energy reflected by the electron beam. Previous studies have shown that the energy utilization rate of the electron beam is only about 75%. The main reason is that the electron beam bombards the silicon melt. 25% of the energy is reflected at the surface of the body fluid, and the radiation intercepting shield can intercept the reflected energy for melting silicon melt.

综上,本发明提供一种电子束熔炼用坩埚的辐射拦截装置,具有制作方便的优点,该辐射拦截装置可将硅熔体的热辐射、被硅熔体表面反射的电子束束流拦截回来,重新作用于硅熔体表面,大大提高了电子束能量利用率,提高幅度达20~50%。 In summary, the present invention provides a radiation intercepting device for a crucible for electron beam smelting, which has the advantage of being easy to manufacture. The radiation intercepting device can intercept the thermal radiation of the silicon melt and the electron beam reflected by the surface of the silicon melt. , re-acting on the surface of the silicon melt, greatly improving the energy utilization rate of the electron beam by 20-50%.

附图说明 Description of drawings

图1为一种电子束熔炼用坩埚的辐射拦截装置的结构简图。 Fig. 1 is a schematic structural diagram of a radiation intercepting device for a crucible for electron beam melting.

图2为图1中辐射拦截罩的俯视结构图 Fig. 2 is a top view structure diagram of the radiation intercepting cover in Fig. 1

图中:1.真空泵组,2.滑动悬挂杆,3.电子枪,4.炉壁,5.电子束,6.辐射拦截罩,7.炉门,8.熔炼室,9.熔炼坩埚,10.熔融液体,11.进水口,12.出水口,13.水冷托盘,14.悬挂铰接扣,15.缺口 In the figure: 1. Vacuum pump group, 2. Sliding suspension rod, 3. Electron gun, 4. Furnace wall, 5. Electron beam, 6. Radiation intercepting cover, 7. Furnace door, 8. Melting chamber, 9. Melting crucible, 10 .Molten liquid, 11. Water inlet, 12. Water outlet, 13. Water cooling tray, 14. Hanging hinge buckle, 15. Notch

具体实施方式 Detailed ways

下面结合具体实施例及附图详细说明本发明,但本发明并不局限于具体实施例。 The present invention will be described in detail below in conjunction with specific embodiments and drawings, but the present invention is not limited to specific embodiments.

实施例1 Example 1

如附图1和图2所示,一种电子束熔炼用坩埚的辐射拦截装置,包括辐射拦截罩,滑动悬挂杆和真空熔炼装置,真空熔炼装置中,炉壁4内部为熔炼室8,炉壁上安装有炉门7,水冷托盘13固定安装于炉壁4底部,水冷托盘上开有进水口11和出水口12,熔炼坩埚9固定安装于水冷托盘之上,真空泵组1固定安装于炉壁之上,电子枪3固定安装于炉壁顶部,辐射拦截罩6位于熔炼坩埚上方,且通过滑动悬挂杆2活动安装于炉壁的顶部,辐射拦截罩6与滑动悬挂杆2之间通过悬挂铰接扣活动连接。 As shown in Figure 1 and Figure 2, a radiation intercepting device for a crucible for electron beam melting includes a radiation intercepting cover, a sliding suspension rod and a vacuum melting device. In the vacuum melting device, the inside of the furnace wall 4 is a melting chamber 8, and the furnace Furnace door 7 is installed on the wall, water-cooling tray 13 is fixedly installed on the bottom of furnace wall 4, water inlet 11 and water outlet 12 are opened on the water-cooling tray, melting crucible 9 is fixedly installed on the water-cooling tray, vacuum pump group 1 is fixedly installed on the furnace On the wall, the electron gun 3 is fixedly installed on the top of the furnace wall, the radiation intercepting cover 6 is located above the melting crucible, and is movably installed on the top of the furnace wall through the sliding suspension rod 2, and the radiation intercepting cover 6 and the sliding suspension rod 2 are hinged by suspension Buckle activity connection.

辐射拦截罩为球面形状,其凹面朝下,凹面聚焦点位于熔炼坩埚中心,辐射拦截罩位于熔炼坩埚上方30cm,其正投影为圆形,半径为15cm,辐射拦截罩材质为铜。 The radiation intercepting shield is in the shape of a sphere, with its concave facing downwards. The focal point of the concave surface is located at the center of the melting crucible. The radiation intercepting shield is located 30cm above the melting crucible. Its orthographic projection is circular with a radius of 15cm. The radiation intercepting shield is made of copper.

辐射拦截罩上电子束直接辐射位置还开有一个圆弧形缺口15,圆弧形缺口的半径为5cm。 There is also an arc-shaped notch 15 at the direct radiation position of the electron beam on the radiation intercepting cover, and the radius of the arc-shaped notch is 5 cm.

圆弧形缺口主要是用来避开电子束的直接辐射,使得电子束的辐射直接作用于熔炼坩埚的熔体之中。 The arc-shaped notch is mainly used to avoid the direct radiation of the electron beam, so that the radiation of the electron beam directly acts on the melt of the melting crucible.

滑动悬挂杆为3根,每根滑动悬挂杆安装有独立的驱动装置,熔炼过程中通过调节滑动悬挂杆的升降,来调节辐射拦截罩的倾斜角度,使得辐射拦截罩反射回来的电子束和能量作用于熔炼坩埚的中心位置。 There are 3 sliding suspension rods, and each sliding suspension rod is equipped with an independent driving device. During the smelting process, the tilt angle of the radiation interception cover can be adjusted by adjusting the lifting of the sliding suspension rod, so that the electron beam and energy reflected by the radiation interception cover Acts on the central position of the melting crucible.

使用上述熔炼装置和传统熔炼装置进行电子束熔炼提纯多晶硅的对比实验: The comparison experiment of electron beam smelting and purification of polysilicon using the above smelting equipment and traditional smelting equipment:

(a)传统熔炼装置对0.5kg硅材料进行熔炼,固定电子束功率12kw,保证电子束坩埚中硅材料不能完全被熔融,当形成稳定熔池后,即刻关束。将硅锭取出在中心进行切割,腐蚀,进行断面形貌分析,标出熔池的形态,计算断面处的熔池面积,并记为A0; (a) The traditional smelting device melts 0.5kg of silicon material, and fixes the electron beam power at 12kw to ensure that the silicon material in the electron beam crucible cannot be completely melted. When a stable molten pool is formed, the beam is turned off immediately. Take out the silicon ingot and cut it in the center, corrode, analyze the cross-sectional morphology, mark the shape of the molten pool, calculate the area of the molten pool at the cross-section, and record it as A0;

b). 按照同样的熔炼参数,采用加有辐射拦截罩的装置进行熔炼,计算出断面处的熔池面积,记为A1; b). According to the same smelting parameters, use a device with a radiation intercepting cover for smelting, calculate the molten pool area at the section, and record it as A1;

c). 通过对比硅锭断面熔池面积A1和A0,发现A1-> A0,由此证明,加有辐射拦截的水冷铜坩埚能大幅提高电子束的能量利用率,电子束能量利用率提高20%。 c). By comparing the molten pool area A1 and A0 of the silicon ingot section, it is found that A1->A0, which proves that the water-cooled copper crucible with radiation interception can greatly improve the energy utilization rate of the electron beam, and the energy utilization rate of the electron beam can be increased by 20 %.

实施例2 Example 2

如图1和图2所示,一种电子束熔炼用坩埚的辐射拦截装置,装置中除了以下部件不同外,其他均与实施例1中装置相同: As shown in Figures 1 and 2, a radiation intercepting device for a crucible for electron beam smelting, the device is the same as the device in Example 1 except that the following components are different:

辐射拦截罩位于熔炼坩埚上方10cm,其正投影为圆形,半径为40cm,辐射拦截罩材质为石墨。 The radiation intercepting shield is located 10cm above the melting crucible, and its orthographic projection is a circle with a radius of 40cm. The radiation intercepting shield is made of graphite.

辐射拦截罩上电子束直接辐射位置还开有一个圆弧形缺口15,圆弧形缺口的半径为10cm,滑动悬挂杆为5根。 There is also an arc-shaped gap 15 at the direct radiation position of the electron beam on the radiation intercepting cover, the radius of the arc-shaped gap is 10cm, and there are 5 sliding suspension rods.

在进行如实施例1中的对比实验后得到,电子束能量利用率提高50%。 After performing the comparative experiment as in Example 1, the energy utilization rate of the electron beam was increased by 50%.

实施例3 Example 3

如图1和图2所示,一种电子束熔炼用坩埚的辐射拦截装置,装置中除了以下部件不同外,其他均与实施例1中装置相同: As shown in Figures 1 and 2, a radiation intercepting device for a crucible for electron beam smelting, the device is the same as the device in Example 1 except that the following components are different:

辐射拦截罩位于熔炼坩埚上方18cm,其正投影为圆形,半径为30cm,辐射拦截罩材质为石英。 The radiation intercepting shield is located 18cm above the melting crucible, and its orthographic projection is a circle with a radius of 30cm. The radiation intercepting shield is made of quartz.

辐射拦截罩上电子束直接辐射位置还开有一个圆弧形缺口15,圆弧形缺口的半径为8cm,滑动悬挂杆为4根。 There is also an arc-shaped gap 15 at the direct radiation position of the electron beam on the radiation intercepting cover, the radius of the arc-shaped gap is 8cm, and there are 4 sliding suspension rods.

在进行如实施例1中的对比实验后得到,电子束能量利用率提高42%。 After performing the comparative experiment as in Example 1, the energy utilization rate of the electron beam was increased by 42%.

实施例4 Example 4

如图1和图2所示,一种电子束熔炼用坩埚的辐射拦截装置,装置中除了以下部件不同外,其他均与实施例1中装置相同: As shown in Figures 1 and 2, a radiation intercepting device for a crucible for electron beam smelting, the device is the same as the device in Example 1 except that the following components are different:

辐射拦截罩位于熔炼坩埚上方22cm,其正投影为圆形,半径为25cm,辐射拦截罩材质为石墨。 The radiation intercepting shield is located 22cm above the melting crucible, and its orthographic projection is a circle with a radius of 25cm. The radiation intercepting shield is made of graphite.

辐射拦截罩上电子束直接辐射位置还开有一个圆弧形缺口15,圆弧形缺口的半径为6cm,滑动悬挂杆为4根。 There is also an arc-shaped gap 15 at the direct radiation position of the electron beam on the radiation intercepting cover, the radius of the arc-shaped gap is 6cm, and there are 4 sliding suspension rods.

在进行如实施例1中的对比实验后得到,电子束能量利用率提高32%。 After performing the comparative experiment as in Example 1, the energy utilization rate of the electron beam was increased by 32%.

Claims (6)

1. an electron beam melting is with the radiation blocking apparatus of crucible, comprise radiation interception cover, slip hanger bar and vacuum melting device, in the vacuum melting device, inside, furnace wall (4) is working chamber (8), fire door (7) is installed on the furnace wall, water-cooled pallet (13) is fixedly installed in bottom, furnace wall (4), have water-in (11) and water outlet (12) on the water-cooled pallet, smelting pot (9) is fixedly installed on the water-cooled pallet, vacuum pump group (1) is fixedly installed on the furnace wall, electron beam gun (3) is fixedly installed in the top, furnace wall, it is characterized in that: radiation interception cover (6) is positioned at above smelting pot, and be movably installed in the top of furnace wall by slip hanger bar (2), be flexibly connected by hanging kinge-joint knot between radiation interception cover (6) and slip hanger bar (2).
2. a kind of electron beam melting according to claim 1 is with the radiation blocking apparatus of crucible, it is characterized in that: described radiation interception cover is spherical shape, its concave surface down, the concave surface focus point is positioned at the smelting pot center, also has a circular arc cutaway (15) on it.
3. arbitrary described a kind of electron beam melting is with the radiation blocking apparatus of crucible according to claim 1 and 2, and it is characterized in that: described radiation interception cover is positioned at smelting pot top 10-30cm, and its orthographicprojection be circle, and radius is 15-40cm.
4. arbitrary described a kind of electron beam melting is with the radiation blocking apparatus of crucible according to claim 1 and 2, and it is characterized in that: described radiation interception cover material is quartz, 304 stainless steels, graphite or copper.
5. a kind of electron beam melting according to claim 1 is with the radiation blocking apparatus of crucible, and it is characterized in that: described slip hanger bar is the 3-5 root, and every slip hanger bar is equipped with independently drive unit.
6. a kind of electron beam melting according to claim 2 is with the radiation blocking apparatus of crucible, and it is characterized in that: the radius of described circular arc cutaway is 5-10cm.
CN201310023866.XA 2013-01-23 2013-01-23 A radiation intercepting device for a crucible for electron beam melting Expired - Fee Related CN103086379B (en)

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CN109157760A (en) * 2018-08-07 2019-01-08 中国原子能科学研究院 For the rotary line arresting gear in medical device

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CN201981012U (en) * 2011-01-29 2011-09-21 大连隆田科技有限公司 A device for efficiently purifying polysilicon powder by electron beam
CN202063730U (en) * 2011-05-16 2011-12-07 大连隆田科技有限公司 A kind of equipment for smelting and purifying polysilicon by electron beam and slag filtration

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JPH10273313A (en) * 1997-03-28 1998-10-13 Kawasaki Steel Corp Production of polycrystal silicon ingot
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CN109157760A (en) * 2018-08-07 2019-01-08 中国原子能科学研究院 For the rotary line arresting gear in medical device
CN109157760B (en) * 2018-08-07 2019-12-24 中国原子能科学研究院 Rotary beam blocker for use in medical devices

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