CN202105819U - Cleaning device of cauliflower-shaped polysilicon material with oxide attached to surface - Google Patents

Cleaning device of cauliflower-shaped polysilicon material with oxide attached to surface Download PDF

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CN202105819U
CN202105819U CN2011202652270U CN201120265227U CN202105819U CN 202105819 U CN202105819 U CN 202105819U CN 2011202652270 U CN2011202652270 U CN 2011202652270U CN 201120265227 U CN201120265227 U CN 201120265227U CN 202105819 U CN202105819 U CN 202105819U
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cleaning
pool
overflow
cauliflower
ultrasonic
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周罗洪
李义
王达山
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YINGKOU JOLAR TECHNOLOGY Corp
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Abstract

本实用新型涉及一种菜花状及表面附氧化物的多晶硅原料的清洗装置,包括酸洗池、溢流池和超声波溢流清洗池,溢流池由至少一个隔板依次分隔成至少两个水池,每个水池的底部具有排水口,相邻的两个水池之间的隔板的上沿具有溢流开口;超声波清洗池包括清洗水池和设置在清洗水池内的超声波发生器,清洗水池内装有清洗液并具有循环补水装置,超声波发生器设置在清洗水池的两相对的侧壁和底部,还具有对清洗液加热的加热装置。本实用新型的菜花料及表面附氧化物的多晶硅原料的清洗装置,经清洗后原料的表面非常洁净,缝隙里不存在氧化物和其他杂质,充分去除菜花状原料,标准程序下能达到投炉铸锭或拉晶的生产要求。

The utility model relates to a cleaning device for cauliflower-like polysilicon raw materials with oxides attached on the surface, which comprises a pickling pool, an overflow pool and an ultrasonic overflow cleaning pool. The overflow pool is divided into at least two water pools in sequence by at least one partition , the bottom of each pool has a drainage port, and the upper edge of the partition between two adjacent pools has an overflow opening; the ultrasonic cleaning pool includes a cleaning pool and an ultrasonic generator arranged in the cleaning pool, and the cleaning pool is equipped with The cleaning liquid also has a circulating water supply device, and the ultrasonic generator is arranged on two opposite side walls and the bottom of the cleaning pool, and also has a heating device for heating the cleaning liquid. The utility model cleaning device for cauliflower material and polysilicon raw material with oxide attached on the surface, after cleaning, the surface of the raw material is very clean, there are no oxides and other impurities in the gap, and the cauliflower-like raw material can be fully removed. Production requirements for ingots or pulled crystals.

Description

菜花状及表面附氧化物的多晶硅原料的清洗装置Cleaning device for cauliflower-shaped polysilicon raw materials with oxides on the surface

技术领域 technical field

本实用新型涉及多晶硅原料清洗装置技术领域,尤其是一种菜花状及表面附氧化物的多晶硅原料的清洗装置。The utility model relates to the technical field of cleaning devices for polysilicon raw materials, in particular to a cleaning device for polysilicon raw materials in the shape of cauliflower and with oxides on the surface.

背景技术 Background technique

硅半导体耐高电压、耐高温、与其他半导体材料相比,体积小、效率高、寿命长、可靠性强、性能稳定,因而是最理想的太阳能电池材料,硅基太阳能电池占太阳能电池总量的80%以上。如果按照每生产1W太阳能电池需用硅材料17g计算,2010年全世界太阳能级硅材料需求达到8000吨。Silicon semiconductor is resistant to high voltage and high temperature. Compared with other semiconductor materials, it has small volume, high efficiency, long life, strong reliability and stable performance. Therefore, it is the most ideal solar cell material. Silicon-based solar cells account for the total amount of solar cells. More than 80% of. If it is calculated that 17g of silicon material is required to produce 1W of solar cells, the demand for solar-grade silicon materials in the world will reach 8,000 tons in 2010.

太阳能级硅料的纯度要求在6N左右,低于半导体工业用硅10-12N的纯度要求,所以太阳能级硅料主要来自于半导体工业硅的废料和次品。随着全球太阳能电池产业的迅猛发展,太阳能硅料的来源已经无法满足其日益增长的需求,太阳能级硅来源出现了巨大的缺口。The purity requirement of solar-grade silicon is about 6N, which is lower than the purity requirement of 10-12N for silicon used in the semiconductor industry, so solar-grade silicon mainly comes from the waste and defective products of silicon in the semiconductor industry. With the rapid development of the global solar cell industry, the source of solar silicon materials has been unable to meet its growing demand, and there has been a huge gap in the source of solar-grade silicon.

为了节约硅原料,要把多晶硅废料处理后再利用。CN200610010654公开了一种冶金级硅的酸洗方法:1)、将粉碎好后的硅粉物料先使用浓度为1-6mol/l的盐酸进行酸浸处理,浸出温度40-80℃,浸出时间为0.5-2天,然后用蒸馏水清洗2-5次,再真空抽滤将硅粉与浸出液进行分离;2)、将分离出的硅粉物料用硝酸浓度为0.5-6mol/l,温度40-80℃,二次浸出0.5-2天,然后使用蒸馏水清洗2-5次后进行真空抽滤分离将硅粉与浸出液进行分离;3)、最后再采用浓度为1-5mol/l的氢氟酸,温度40-80℃,浸泡0.5-1天,然后用蒸馏水清洗3-8次后真空抽滤,将硅粉物料与浸出液进行分离。In order to save silicon raw materials, polysilicon waste should be processed and reused. CN200610010654 discloses a pickling method for metallurgical grade silicon: 1), first use hydrochloric acid with a concentration of 1-6mol/l to carry out pickling treatment with the pulverized silicon powder material, the leaching temperature is 40-80°C, and the leaching time is 0.5-2 days, then wash 2-5 times with distilled water, and then vacuum filter to separate the silicon powder from the leaching solution; ℃, secondary leaching for 0.5-2 days, and then use distilled water to wash 2-5 times, and then carry out vacuum filtration separation to separate the silicon powder from the leaching solution; 3), and finally use hydrofluoric acid with a concentration of 1-5mol/l, The temperature is 40-80°C, soaked for 0.5-1 day, then washed with distilled water for 3-8 times, and vacuum filtered to separate the silicon powder material from the leachate.

CN200910025729公开了一种多晶硅硅料的清洗方法:将多晶硅硅料置于混合酸液中进行避光浸泡1-10分钟,混合酸液的温度为30-35℃,后捞取,用纯水冲洗,再经超声冲洗、压缩空气鼓泡后烘干;混合酸液的配比为硝酸∶氢氟酸∶冰乙酸的溶液体积比为57∶18∶25,硝酸浓度为68-72%,氢氟酸浓度为38-41%,冰乙酸浓度为99.8-99.9%.CN200910025729 discloses a cleaning method for polysilicon material: put the polysilicon material in a mixed acid solution and soak it in the dark for 1-10 minutes. After ultrasonic washing, compressed air bubbling, drying; the proportion of the mixed acid solution is nitric acid: hydrofluoric acid: glacial acetic acid solution volume ratio is 57:18:25, the concentration of nitric acid is 68-72%, hydrofluoric acid The concentration is 38-41%, and the concentration of glacial acetic acid is 99.8-99.9%.

CN200610050725公开了一种硅料清洁方法:硅料沉浸于氢氟酸和硝酸混合酸溶液中;捞取浸渍后的硅料,用纯水多级冲洗;将冲洗后的硅料浸泡于纯水;测定纯水浸泡液的电导率;捞取硅料,烘干;氢氟酸的浓度为40%-49%,硝酸浓度为65-68%,体积比1∶8-12。CN200610050725 discloses a silicon material cleaning method: the silicon material is immersed in the mixed acid solution of hydrofluoric acid and nitric acid; The electrical conductivity of the pure water soaking solution; the silicon material is scooped out and dried; the concentration of hydrofluoric acid is 40%-49%, the concentration of nitric acid is 65-68%, and the volume ratio is 1:8-12.

为了节约硅原料,要把多晶硅废料处理后再利用。多晶硅沉积速度太快时,硅棒表面容易生长为菜花状,多晶硅料表面还附有氧化物,硅料缝隙深度较大时,后续的清洗工作非常困难,若要生产符合标准的太阳能级的硅片,必须将菜花料和氧化物清洗干净。原料需先经过酸洗,再漂洗去除残余酸,才能供后续操作使用,现有的设备不能完全去除残余酸。In order to save silicon raw materials, polysilicon waste should be processed and reused. When the polysilicon deposition rate is too fast, the surface of the silicon rod is easy to grow into a cauliflower shape, and the surface of the polysilicon material is also covered with oxides. When the gap depth of the silicon material is large, the follow-up cleaning work is very difficult. For slices, the cauliflower material and oxides must be cleaned. Raw materials need to be pickled first, and then rinsed to remove residual acid before they can be used in subsequent operations. Existing equipment cannot completely remove residual acid.

实用新型内容 Utility model content

本实用新型要解决的技术问题是:为了解决现有技术的不足,本实用新型提供一种菜花状及表面附氧化物的多晶硅原料的清洗装置,满足菜花状料及表面附有氧化物的多晶硅料的去除残余酸的清洗要求。The technical problem to be solved by the utility model is: in order to solve the deficiencies of the prior art, the utility model provides a cleaning device for cauliflower-shaped polysilicon raw materials with oxides on the surface, which meets the requirements of cauliflower-shaped materials and polysilicon materials with oxides on the surface. cleaning requirements for the removal of residual acid.

本实用新型解决其技术问题所采用的技术方案是:一种菜花状及表面附氧化物的多晶硅原料的清洗装置,包括酸洗池、溢流池和超声波溢流清洗池,所述的溢流池由至少一个隔板依次分隔成至少两个水池,每个水池的底部具有排水口,相邻的两个水池之间的隔板的上沿具有溢流开口;所述的超声波清洗池包括清洗水池和设置在清洗水池内的超声波发生器,清洗水池内装有清洗液并具有循环补水装置,所述的超声波发生器设置在清洗水池的两相对的侧壁和底部,还具有对清洗液加热的加热装置。The technical solution adopted by the utility model to solve the technical problems is: a cleaning device for cauliflower-shaped polysilicon raw materials with oxides on the surface, including a pickling pool, an overflow pool and an ultrasonic overflow cleaning pool. The pool is divided into at least two pools sequentially by at least one partition, each pool has a drain outlet at the bottom, and the upper edge of the partition between two adjacent pools has an overflow opening; the ultrasonic cleaning pool includes cleaning The pool and the ultrasonic generator set in the cleaning pool, the cleaning pool is equipped with cleaning liquid and has a circulating water replenishment device, the ultrasonic generator is set on the two opposite side walls and bottom of the cleaning pool, and also has a heating mechanism for the cleaning liquid heating equipment.

作为优选,所述的溢流池为由两个隔板依次分隔成的三个水池。Preferably, the overflow pool is three water pools separated by two partitions in turn.

为防止水池相互污染,所述的两个隔板上的溢流开口高度不同。In order to prevent mutual contamination of the pools, the heights of the overflow openings on the two partitions are different.

为实现自动恒温,所述的加热装置为由温控开关控制启闭的加热管。In order to realize automatic constant temperature, the heating device is a heating tube controlled to be turned on and off by a temperature control switch.

本实用新型的有益效果是,本实用新型的菜花状及表面附氧化物的多晶硅原料的清洗装置,经清洗后原料的表面非常洁净,缝隙里不存在氧化物和其他杂质,充分去除菜花状原料,标准程序下能达到投炉铸锭或拉晶的生产要求。The beneficial effect of the utility model is that the cleaning device of the utility model for cauliflower-shaped polysilicon raw materials with oxides on the surface, after cleaning, the surface of the raw materials is very clean, there are no oxides and other impurities in the gaps, and the cauliflower-shaped raw materials are fully removed , under the standard procedure, it can meet the production requirements of casting ingots or pulling crystals.

附图说明 Description of drawings

下面结合附图和实施例对本实用新型进一步说明。Below in conjunction with accompanying drawing and embodiment the utility model is further described.

图1是本实用新型的菜花状及表面附氧化物的多晶硅原料的清洗装置中所述溢流池的主视结构示意图;Fig. 1 is the front view structural representation of the overflow tank described in the cleaning device of the polysilicon raw material of cauliflower shape and surface oxide of the present utility model;

图2是本实用新型的菜花状及表面附氧化物的多晶硅原料的清洗装置中所述溢流池的立体结构示意图;Fig. 2 is the schematic diagram of the three-dimensional structure of the overflow tank described in the cleaning device of the cauliflower-shaped and surface-attached polysilicon raw materials of the present invention;

图3是本实用新型的菜花状及表面附氧化物的多晶硅原料的清洗装置中所述超声波溢流清洗池的俯视结构示意图;Fig. 3 is the top view structural representation of the ultrasonic overflow cleaning tank described in the cleaning device of the cauliflower-shaped and surface-attached polysilicon raw materials of the present invention;

图4是本实用新型的菜花状及表面附氧化物的多晶硅原料的清洗装置中所述超声波溢流清洗池的立体结构示意图;Fig. 4 is the schematic diagram of the three-dimensional structure of the ultrasonic overflow cleaning tank described in the cleaning device of the cauliflower-shaped and surface-attached polysilicon raw materials of the present invention;

图中:1.溢流池,11.隔板,12.排水口,13.溢流开口,2.超声波溢流清洗池,21.超声波发生器,22.侧壁,23.底部,24.加热装置。In the figure: 1. overflow tank, 11. clapboard, 12. drain, 13. overflow opening, 2. ultrasonic overflow cleaning tank, 21. ultrasonic generator, 22. side wall, 23. bottom, 24. heating equipment.

具体实施方式 Detailed ways

现在结合附图对本实用新型作进一步详细的说明。这些附图均为简化的示意图,仅以示意方式说明本实用新型的基本结构,因此其仅显示与本实用新型有关的构成。Now in conjunction with accompanying drawing, the utility model is described in further detail. These drawings are all simplified schematic diagrams, and only schematically illustrate the basic structure of the utility model, so they only show the configurations related to the utility model.

图1图2图3图4是本实用新型一种菜花状及表面附氧化物的多晶硅原料的清洗装置,包括酸洗池、溢流池1和超声波溢流清洗池2,溢流池1为由两个隔板11依次分隔成的三个水池,每个水池的底部具有排水口12,相邻的两个水池之间的隔板11的上沿具有溢流开口13,两个隔板11上的溢流开口13高度不同;超声波清洗池2包括清洗水池和设置在清洗水池内的超声波发生器21,清洗水池内装有清洗液并具有循环补水装置,超声波发生器21设置在清洗水池的两相对的侧壁22和底部23,还具有对清洗液加热的加热装置24。Fig. 1 Fig. 2 Fig. 3 Fig. 4 is the cleaning device of a kind of cauliflower shape and the polysilicon raw material with oxide on the surface of the utility model, including pickling pool, overflow pool 1 and ultrasonic overflow cleaning pool 2, overflow pool 1 is Three pools are separated by two partitions 11 in turn, each pool has a drain outlet 12 at the bottom, and the upper edge of the partition 11 between two adjacent pools has an overflow opening 13, and the two partitions 11 The height of the overflow opening 13 on the top is different; the ultrasonic cleaning pool 2 includes a cleaning pool and an ultrasonic generator 21 arranged in the cleaning pool. The cleaning liquid is housed in the cleaning pool and has a circulating water supply device. The ultrasonic generator 21 is arranged on both sides of the cleaning pool. The opposite side wall 22 and bottom 23 also have a heating device 24 for heating the cleaning liquid.

加热装置24为由温控开关控制启闭的加热管。The heating device 24 is a heating tube controlled on and off by a temperature control switch.

菜花状料及表面附有氧化物的多晶硅料经酸洗池清洗后采用溢流池1和超声波清洗池2去除酸洗时残留的酸液。After the cauliflower-like material and the polysilicon material with oxides on the surface are cleaned by the pickling tank, the overflow tank 1 and the ultrasonic cleaning tank 2 are used to remove the residual acid during pickling.

使用溢流池1溢流漂洗原料时,向三个水池中溢流开口13最高(即水位最高)的水池中通入纯水,注满后不停的向旁边的水池溢流,清洗原料时先放入水位低的水池清洗,再逐步用高水位水池清洗。达到充分清洗原料酸液的目的,并能节省宝贵水资源。When using the overflow tank 1 to overflow and rinse raw materials, feed pure water into the pool with the highest overflow opening 13 (i.e. the highest water level) in the three pools, and overflow to the pool next to it after filling, when cleaning the raw materials Put it into a pool with a low water level for cleaning first, and then gradually use a pool with a high water level for cleaning. The purpose of fully cleaning the raw acid solution can be achieved, and precious water resources can be saved.

使用超声波清洗池2时,清洗水池内通入纯水,并不停补充新的纯水,将用溢流池1漂洗后的原料放入超声波清洗池2,两侧壁22和底部23的超声波发生器21同时工作,去除原料中的残余酸,加热装置24对清洗液加热,控制清洗液温度为60℃±5℃,在这个温度环境下,维持2小时左右清洗效果最好。When using the ultrasonic cleaning tank 2, pure water is introduced into the cleaning tank, and new pure water is constantly replenished, and the raw materials rinsed with the overflow tank 1 are put into the ultrasonic cleaning tank 2, and the ultrasonic waves on the side walls 22 and the bottom 23 The generator 21 works at the same time to remove the residual acid in the raw material, and the heating device 24 heats the cleaning solution to control the temperature of the cleaning solution at 60°C±5°C. Under this temperature environment, the cleaning effect is best if it is maintained for about 2 hours.

以上述依据本实用新型的理想实施例为启示,通过上述的说明内容,相关工作人员完全可以在不偏离本项实用新型技术思想的范围内,进行多样的变更以及修改。本项实用新型的技术性范围并不局限于说明书上的内容,必须要根据权利要求范围来确定其技术性范围。Inspired by the above ideal embodiment according to the utility model, through the above description content, relevant staff can completely make various changes and modifications within the scope of not deviating from the technical idea of the utility model. The technical scope of this utility model is not limited to the content in the description, but must be determined according to the scope of the claims.

Claims (4)

1.一种菜花状及表面附氧化物的多晶硅原料的清洗装置,包括酸洗池、溢流池(1)和超声波溢流清洗池(2),其特征在于:所述的溢流池(1)由至少一个隔板(11)依次分隔成至少两个水池,每个水池的底部具有排水口(12),相邻的两个水池之间的隔板(11)的上沿具有溢流开口(13);1. a kind of cleaning device of the polysilicon raw material of cauliflower shape and surface attached oxide, comprises pickling tank, overflow tank (1) and ultrasonic overflow cleaning tank (2), it is characterized in that: described overflow tank ( 1) At least two pools are divided in turn by at least one partition (11), each pool has a drain outlet (12) at the bottom, and the upper edge of the partition (11) between two adjacent pools has an overflow opening (13); 所述的超声波清洗池(2)包括清洗水池和设置在清洗水池内的超声波发生器(21),清洗水池内装有清洗液并具有循环补水装置,所述的超声波发生器(21)设置在清洗水池的两相对的侧壁(22)和底部(23),还具有对清洗液加热的加热装置(24)。The ultrasonic cleaning pool (2) comprises a cleaning pool and an ultrasonic generator (21) arranged in the cleaning pool. The cleaning fluid is housed in the cleaning pool and has a circulating water supply device. The ultrasonic generator (21) is arranged in the cleaning pool. The two opposite side walls (22) and the bottom (23) of the pool also have a heating device (24) for heating the cleaning liquid. 2.如权利要求1所述的菜花状及表面附氧化物的多晶硅原料的清洗装置其特征是:所述的溢流池(1)为由两个隔板(11)依次分隔成的三个水池。2. The cleaning device of cauliflower-shaped and surface-attached oxide polysilicon raw materials as claimed in claim 1 is characterized in that: the overflow pool (1) is divided into three successively by two dividing plates (11). pool. 3.如权利要求2所述的菜花状及表面附氧化物的多晶硅原料的清洗装置其特征是:所述的两个隔板(11)上的溢流开口(13)高度不同。3. The cleaning device for cauliflower-shaped polysilicon raw materials with oxides on the surface as claimed in claim 2, characterized in that: the overflow openings (13) on the two partitions (11) are of different heights. 4.如权利要求1所述的菜花状及表面附氧化物的多晶硅原料的清洗装置其特征是:所述的加热装置(24)为由温控开关控制启闭的加热管。4. The cleaning device for cauliflower-shaped polysilicon raw materials with oxides on the surface as claimed in claim 1, characterized in that: the heating device (24) is a heating tube controlled by a temperature control switch.
CN2011202652270U 2011-07-25 2011-07-25 Cleaning device of cauliflower-shaped polysilicon material with oxide attached to surface Expired - Fee Related CN202105819U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102266859A (en) * 2011-07-25 2011-12-07 营口晶晶光电科技有限公司 Method and device for cleaning cauliflower-shaped polycrystalline silicon raw material with oxides on surface thereof
CN103157622A (en) * 2013-04-03 2013-06-19 沈陈益 Washing device
CN104550091A (en) * 2014-12-31 2015-04-29 东莞市华荣涂装设备有限公司 Water circulation system and circulation method for spray treatment before coating

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102266859A (en) * 2011-07-25 2011-12-07 营口晶晶光电科技有限公司 Method and device for cleaning cauliflower-shaped polycrystalline silicon raw material with oxides on surface thereof
CN103157622A (en) * 2013-04-03 2013-06-19 沈陈益 Washing device
CN104550091A (en) * 2014-12-31 2015-04-29 东莞市华荣涂装设备有限公司 Water circulation system and circulation method for spray treatment before coating

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