TW201240918A - Method for waste silicon slurry recovery and silicon ingot preparation - Google Patents

Method for waste silicon slurry recovery and silicon ingot preparation Download PDF

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TW201240918A
TW201240918A TW100111541A TW100111541A TW201240918A TW 201240918 A TW201240918 A TW 201240918A TW 100111541 A TW100111541 A TW 100111541A TW 100111541 A TW100111541 A TW 100111541A TW 201240918 A TW201240918 A TW 201240918A
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Taiwan
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silicon
waste
separation
crystal
mud
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TW100111541A
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Chinese (zh)
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Hong-Tai Cai
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Hong-Tai Cai
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Priority to TW100111541A priority Critical patent/TW201240918A/en
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  • Crystals, And After-Treatments Of Crystals (AREA)
  • Treatment Of Sludge (AREA)

Abstract

The present invention provides a method for waste silicon slurry recovery and silicon ingot preparation, including: a centrifugal separation step that carries out a centrifugal separation of the liquid in the waste silicon slurry; a drying step that carries out a drying treatment of the waste silicon slurry obtained from the aforementioned step so as to volatilize residual liquid; a grinding step that grinds the waste silicon slurry obtained from the aforementioned step to fine granular powder; a first blowing separation step that carries out a blowing separation of waste silicon slurry powder obtained from the aforementioned step so as to obtain metal substance, silicon carbide and silicon crystal having higher specific gravity; an electrostatic separation step that carries out an electrostatic separation of the metal substance, silicon carbide and silicon crystal obtained from the aforementioned step so as to obtain silicon carbide and silicon crystal; a second blowing separation step that carries out a blowing separation of silicon carbide and silicon crystal obtained from the aforementioned step so as to obtain silicon crystal; and a high temperature melting step that carries out a melting treatment of the silicon crystal obtained from the aforementioned step and then cooling down the same in a melting furnace to form high purity silicon ingot.

Description

201240918 六、發明說明: 【發明所屬之技術領域】 本發明係為一種廢矽泥回收及製造矽晶碇方法,尤指一種回 收過知更為簡單’不會對環境造成二次污染,而有助於降低廢石夕 泥回收處理成本及;^晶处產成本之射泥回收及製紗晶石定方 法。 【先前技術】 近年來由於再生能源受到重視,尤其太陽能產業快速的發 展,因此造成製造太陽能電池所需_原料供不應求,使得石夕原 料價格飆漲,嚴重影響太陽能產業的發展。 目前製造太陽能電池所需神補,係採自天财礦石少石, 再經提煉到純度99. 9_晶破,在提煉生絲晶碗之過程中,除 了需要技術、設似外’且製程繁㈣時及_雜極大的能源, 以致成本絲不下。因此,如何找尋到更多时原料來源,已為 產學界共通努力的方向。 曰然而’檢視目神晶销生產過程,其中在砍晶棒切割成石夕 晶片的過程中’因為切纖本身寬度的難,以致在切割的時候 會有_%的補耗’娜的销與切·、研練及切割線磨耗 的金屬混合在-起形射泥’而被當作廢棄物處莊棄;由是, 如果能將_泥中⑽有效的回收,再提供作為太陽能電池所需 的石夕補’那麼將成祕補供應的另—種來源,而可降低石夕礦 開採量與減少廢魏對環境辟,並可降低太陽能電池的生產成 201240918 本。 有關從廢矽泥中回收矽的技術,雖然在我國專利公報中已有 第095150091號「切割矽泥回收方法」(證書號數:1337983)專利 之核准及公開;惟查,該回收方法係包括有下列步驟: a、 離心清洗:加入清洗劑(例如丙嗣)去除矽泥中之雜質,並利用 離心處理分離液體,以去除石夕泥中之污水與潤滑油。 b、 酸洗,加人酸洗劑(如:硫酸、鹽酸或俩)絲魏中之金屬 物質’此時矽泥之主要為矽及碳化石夕。 c、 第二讀洗:轉類或鴨(例如闕與摘)進行第二次清 洗,將有機物完全移除,並再以清水清洗與乾燥,以確保所有 的溶劑都已清除。 分離,加人比重介树及碳切間之浮賴(如:演仿或四演 乙烧再經麟4理,將料碳切錄,並麵碳化石广 其中’該浮棚的比重可彻添加乙醇來調整,該分離步驟可 進-步進行碳切聚鮮驟後再進行離心處理,該碳化石夕聚集 步驟係力认義溶液,以改變其_,或加錢糊或界面、舌 性劑,而令碳切料,畔職可進—步加入去離 子水進行第三:欠清洗步驟,財除水巾特定的陽離子與陰離 子。 第三次清洗:以_或_沖洗並職去除浮選劑,此時 需要可再步歡再次清洗去除凝聚劑或界面活性劑可能帶 來之金屬污染物或有機物質。 201240918 卜乾燥:以真线财式’結溫狀況下麵水分,取得高純度 碎粉。 g、高溫分離··將觀後的魏放讀辦加熱至_雜以上, 但在碳化石夕的熔點以下,讓矽晶析出。 由上述所揭露的技術内容可知,該專利係以化學處理方式作為 從射泥中回收_手段,也就是在從廢魏中时_過程中 加入了很多的化學藥劑;因此,除了回㈣程手續繁複之外,且 過程中所遺留之化學_财造成二次污染疑慮,須再次回收處 理,而將徒增廢矽泥回收處理之成本。 【發明内容】 本發明之目的,即在於改善上述廢魏时方法所存在之問 崎’提供-種时過程更為簡單,不會對環境造成二次污染,而 有助於降低廢魏回收處理成本及抑4生產成本之射泥回收 及製造矽晶碇方法。 為達到上述目的,本發明之廢石夕泥回收及製造石夕晶破方法, 包含有: a. 離心分離:糊離心機將廢魏巾驗體分離; b. 乾燥.將上述步騎得之廢魏進行乾雜理,將剩餘的液 體揮發; ' / c. 研磨.將上述步騎得财泥進行研磨處理,將射泥形成 顆粒細小之粉末; d. 第_人風吹分離:將上述步驟所得之廢矽泥粉末進行風吹分 201240918 離處理’利用比重原理,將比重較輕之廢泥砂分離,留下比 重較重之金屬物質、碳化石夕及石夕晶體; e.靜電分離:將上述步驟所得之金屬物f、碳切及梦晶體進 行靜電分離處理’ _帶電荷量差異性原理,將金屬物質分 離’留下碳化妙與石夕晶體; f·第-★風人/7離·將上述步驟所得之碳切財晶體再次進 行風吹分離處理’利耻重原理,將碳化料離,留下石夕晶 體; 晶體進行熔融,然後置於熔 g.高溫熔融:將上述步驟所得之矽 晶碇成長出完整的結晶體,製造出高 爐内冷卻到常溫,使石夕 純度的發晶石定; 藉由上述步驟’提供一種回收過程更為簡單,不會對環境造 成二次污染,而有助於降低廢魏回收處理成本歸Μ生產成 本之廢矽泥回收及製造矽晶碇方法。 【實施方式】 有關本發明為達到目的所之技術手段及其構造,兹謹再 配合第-圖所示之流糊,詳細說明如下: 本發明之廢碎泥回收及製紗晶財法,包含有: &離:分離:利用離心機將廢魏中的液體(如:水分、切割油、 醇及研磨液)刀離,其中,該離心機以連續性的離心機(例 如:碟型離心機)為較佳,藉以連續性的進料及將液體分離的廢 矽泥送出。 201240918 b.乾燥.將上述步驟分離後之廢魏以乾馳關餘微量的 液體(如:水分、切割油、乙二醇及研磨液)揮發乾燥。 C.研磨.將上述步職驗之射如研雜磨成齡細小之粉 末。 d. 第-次財分離:將上述步騎得之廢魏粉末贿風機進行 風吹分離處理,利用比重原理,將比重較輕之廢泥石少分離,留 下比重較重之金屬物質、碳化矽及矽晶體。 e. 靜電分離:將上述步驟所得之金屬㈣、碳切砂晶體以靜 電分離器進行靜電分離處理,利用帶電荷量差異性原理,將金 屬物質分離,留下碳化矽與矽晶體。 f. 第二次風吹分離:將上述步驟所得之碳切射晶體再次以旋 風機進行敬處理,姻比重顧,將碳切分離,留下石夕晶 體。 =溫雜:將上述步驟所得之㈣體以_賴進行溶融,势 後置於掛_冷卻到常溫,使㈣料長“整的結晶體,名 _内成型為高純度_純,製造出具有方棚的石夕晶 :。其中1晶體在_内進㈣融過程中,可於_内加入 鐵度的氬氣⑹,以防切晶體在溶融過程 :二可於掛銷外圍加入非晶質一 nr與魏赵氧倾卿彡成二氧化碳⑽),以有效降 用…圍氧乳的含量’防止石夕晶體在炼融過程中產生氧化作 ,使㈣作出結晶性良好的梦純。又,其中_晶體在掛 201240918 鋼内炼融成魏液後,可利用溫度梯度控制(例如以_小 閉-組加熱器為-下降區隔),使石夕_在_内緩慢冷卻_ 溫,以利用由下往上層的溫差,製造出具有方向性垂直結晶的 矽晶錠,使矽晶碇成長出更完整的結晶體。 、 藉由上述綠,本發日神可对效时廢魏中⑽晶體, 再以鑄造(Casting)方式絲造高純度⑽故,啸供最理想結 構的太陽能發晶片原料’而可減少㈣開採#及降低開採石夕確對 環境之影響,增加石夕晶碗的貨源供應,且在回收處理的過程中, 由於係以物理方法分離取财晶體’因此讀過程鮮,不會對 環境造成二次污染,而有助於降低廢魏时處理成本及梦晶旋 生產成本。 由疋’本發明確可提供廢;^泥之时及製财純,且相較 於既有的技術具有㈣之進步性,並確為未t有過,誠已符合發 明專利之要件,爰依法提出專利申請,並祈賜專利為禱,至感德 便。 惟,以上所述’僅為本發明之較佳實施例,因此並不能以之 限疋本發明,舉凡依本發明說明書及申請專利翻所為之等效改 變,皆應屬本發明所涵蓋之保護範圍。 【圖式簡單說明】 第一圖係本發明之流程圖。 8201240918 VI. Description of the invention: [Technical field to which the invention pertains] The present invention relates to a method for recycling and manufacturing a silicon germanium, in particular, a recycling is simpler and does not cause secondary pollution to the environment, but Helps reduce the cost of waste rock recycling and processing; and the method of sludge recovery and yarn making. [Prior Art] In recent years, due to the importance of renewable energy, especially the rapid development of the solar industry, the demand for raw materials for solar cells is in short supply, which makes the price of Shixi raw materials soar, seriously affecting the development of the solar industry. At present, the solar cell is required to be made by the gods. It is extracted from Tiancai ore and is refined to a purity of 99. 9_ crystal broken. In the process of refining the raw silk crystal bowl, in addition to the need for technology and design, the process is complicated. (4) Time and _ extremely large energy, so that the cost is not enough. Therefore, how to find more sources of raw materials has become a common direction for the industry and academia.曰 However, 'inspecting the production process of the crystal gods, in the process of cutting the ingot into a stone wafer, 'because the width of the fiber itself is difficult, so that there will be _% of the consumption when cutting. The metal that is cut, grounded, and cut by the cutting line is mixed in the shape of the squirting mud, and is discarded as waste; if it is, the _ mud (10) can be effectively recycled and then provided as a solar cell. The Shi Xibu's will become another source of the secret supply, which can reduce the mining volume of Shixi Mine and reduce the environmental impact of waste Wei, and can reduce the production of solar cells into 201240918. Regarding the technology for recovering strontium from waste mud, although the approval and disclosure of the patent No. 095150091 "Cleaning sludge removal method" (certificate number: 1337983) has been published in the Chinese Patent Gazette; There are the following steps: a. Centrifugal cleaning: Adding a cleaning agent (such as propionate) to remove impurities in the mud, and separating the liquid by centrifugation to remove the sewage and lubricating oil in the stone mud. b, pickling, add acid pickling agent (such as: sulfuric acid, hydrochloric acid or two) silk metal in the material substance 'At this time, the mud is mainly 矽 and carbonized stone eve. c. Second wash: Transfer or duck (such as picking and picking) for a second wash, remove the organics completely, and then rinse and dry with water to ensure that all solvents are removed. Separation, adding the proportion of the tree and the carbon-cutting between the two (such as: imitation or four-playing E-burning and then through the Lin 4, the carbon cut, and the surface of the carbonized stone in which the 'the proportion of the shed can be Adding ethanol to adjust, the separation step can further carry out the carbon cutting and concentrating step, and then carry out centrifugation, the carbonization day gathering step is to force the solution to change its _, or add money paste or interface, tongue The agent, and the carbon cut, the job can be added - step by adding deionized water for the third: under-cleaning step, the specific cation and anion of the water towel. The third cleaning: _ or _ rinse and remove the float In this case, you need to be able to clean again to remove the metal contaminants or organic substances that may be caused by the coagulant or surfactant. 201240918 Bu Dry: Take the water under the junction temperature condition and obtain high purity Powder g. High-temperature separation ············································································ Treatment method as a means of recycling from the mud, also It is in the process of waste Weizhong _ process added a lot of chemicals; therefore, in addition to the complicated (four) procedures, and the chemical chemistry left behind in the process caused secondary pollution doubts, must be recycled again, and will increase The cost of the waste mud recovery treatment. SUMMARY OF THE INVENTION The object of the present invention is to improve the above-mentioned waste-time method, and to provide a simple process without causing secondary pollution to the environment. The invention relates to a method for recovering waste mud recovery and manufacturing a silicon wafer by reducing the waste treatment cost and the production cost of the waste. In order to achieve the above object, the waste stone recovery and manufacture method of the waste stone of the present invention comprises: a Centrifugal separation: the paste centrifuge separates the waste Wei towel; b. Dry. The waste from the above step is dry and sterilized, and the remaining liquid is volatilized; ' / c. Grinding. The mud is ground and the fine particles are formed into a fine powder; d. The first person is blown off by the wind: the waste mud powder obtained in the above step is subjected to wind blowing, 201240918, and the specific gravity principle is adopted. Separation of waste mud sand, leaving a heavier-weight metal material, carbon stone and stone crystal; e. Electrostatic separation: the metal material f, carbon cut and dream crystal obtained in the above step are subjected to electrostatic separation treatment _ _ charge difference Sexual principle, the separation of metal materials 'leave the carbonization and the stone crystals; f · the first - ★ wind people / 7 away · the carbon cut crystals obtained in the above steps are again subjected to wind blow separation process 'shadow weight principle, carbonization The material is separated, leaving the crystal of the stone; the crystal is melted, and then placed in the melt. High temperature melting: the crystallized crucible obtained in the above step is grown into a complete crystal, and the cooling in the blast furnace is cooled to normal temperature to make the purity of the stone The above steps 'provide a recycling process that is simpler, does not cause secondary pollution to the environment, and helps to reduce the waste recycling cost of the waste. The waste sludge is recovered and manufactured. method. [Embodiment] The technical means and structure of the present invention for achieving the object are described in detail with the flow paste shown in the drawings, and the following is a detailed description of the waste sludge recovery and yarn making method of the present invention, including There are: & separation: separation: using a centrifuge to remove the liquid in the waste Wei (such as: moisture, cutting oil, alcohol and grinding fluid), wherein the centrifuge is a continuous centrifuge (for example: disc type centrifugation) Preferably, the continuous feed and the waste mud separating the liquid are sent out. 201240918 b. Drying. The waste Wei separated by the above steps is evaporated and dried by a small amount of liquid (such as moisture, cutting oil, ethylene glycol and grinding liquid). C. Grinding. The above-mentioned step-by-step test is carried out by grinding into a fine powder of age. d. Separation of the first-secondary fiscal: the wind-blown separation process of the waste-wei powder brigade fan of the above step is used, and the principle of specific gravity is used to separate the waste rock with a relatively small specific gravity, leaving a relatively heavy metal material and strontium carbide. And 矽 crystal. e. Electrostatic separation: The metal (4) and carbon-cut sand crystals obtained in the above steps are electrostatically separated by an electrostatic separator, and the metal substance is separated by the principle of charge difference difference, leaving tantalum carbide and tantalum crystal. f. The second wind blow separation: the carbon cut crystal obtained in the above step is treated again by a rotary fan, and the carbon is separated and the carbon crystal is separated to leave the stone crystal. = Wen Miscellaneous: The (4) body obtained in the above step is melted by _ 赖, and then placed in a hanging _ cooling to normal temperature, so that (4) the material length is "the whole crystal, the name _ is formed into a high purity _ pure, and has a square Shi Xijing of the shed: In the process of _inward (four) melting, argon (6) of iron can be added to the _ to prevent the crystal from being melted: second, the amorphous one can be added to the periphery of the hanging pin. Nr and Wei Zhao oxygen dumping into carbon dioxide (10)), in order to effectively reduce the content of ... oxygenated milk to prevent the formation of oxidation in the process of smelting, so that (4) to make a good crystal purity of the pure. _The crystal can be tempered into the Wei liquid in 201240918 steel, and can be controlled by temperature gradient (for example, _ small closed-group heater is used as the descending interval), so that Shi Xi _ slowly cools in _ _ to use From the temperature difference from the lower layer to the upper layer, a twin crystal ingot with directional vertical crystals is produced, so that the twin crystal grains grow into a more complete crystal body. With the above green color, the Japanese god can treat the Weizhong (10) crystal when it is effective. The high-purity (10) is made by casting (Casting), so the most ideal structure of solar energy Sending wafer raw materials' can reduce (4) mining # and reduce the impact of mining on the environment, increase the supply of Shi Xijing bowl, and in the process of recycling, due to the physical separation of the fortune crystals The process is fresh, it will not cause secondary pollution to the environment, and it will help to reduce the waste processing cost and the production cost of the dream crystal spine. Since the invention can provide waste; the time of the mud and the pure wealth, and the phase Compared with the existing technology, it has the progress of (4), and it is indeed unsuccessful. Cheng has already met the requirements of the invention patent, and has filed a patent application according to law, and prayed for the patent as a prayer, to the sense of virtue. The description of the present invention is not intended to limit the invention, and the invention is not limited thereto, and the equivalents of the invention and the equivalents of the invention are all covered by the invention. BRIEF DESCRIPTION OF THE DRAWINGS The first figure is a flow chart of the present invention.

Claims (1)

201240918 七、申請專利範圍: 1. 一種廢矽泥回收及製造矽晶 足万法,包含古. a.離心分離:利用離心機將矽廢泥 頁. b·乾燥:將上述步驟所得之廢二、的液體分離; 發; 泥進行乾燥,將剩餘的液體揮 c. 研磨:將上述步驟所得之轉 顆粒細小之粉末; 4丁研磨’將石夕廢泥研磨成 d. 第一次風吹分離:將上述步 .]m _ 〃斤件之廢矽泥粉末進行風吹分 離處理,利用比重原理,將 ^ ^ 、重較輕之廢泥砂分離,留下比 重車乂重之金屬物質、碳切及發晶體; e. 靜電分離:將上述步驟所提 行靜雷八齡 、麵㈣、碳化似碎晶體進 订電刀離處理,利用帶電荷 離,留下碳化石夕與石夕晶體;、’原理’將金屬物質分 f. 第=風吹分離:_步_之碳切_體再次進 Γ人爾理,利用比重原理,將碳切分離,留下石夕晶 純度的石夕晶石定。 2.如宇請專觀猶叙射泥时”紗騎 ^亥石夕晶體麵输助進行制過程t,可於_内加入盧 就(Ar) ’以防止石夕晶體在炫融過程中產生氧化作用。 虱 201240918 3·如申請專利範圍第丨項所述之 dp-kirjrH B SA Λ. /(〇。收及製造石夕晶旋方法,其 中以夕曰曰體在掛鍋熔爐内進行炫融過程中,可於賴外圍加入 非晶質碳粉’叫切晶巾產生氧化作用。 4.如申料她圍第丨項所述之射泥时及製妙喊方法,其 中該石夕晶體在掛鋼内熔融成石夕熔液後,可利用溫度梯度控制, 使矽熔液在坩鍋内緩慢冷卻到常溫,以利用由下往上層的溫 差’製ig~出具有方向性垂亩結晶的碎晶旋〇201240918 VII. Patent application scope: 1. A method for recycling and manufacturing waste mud and mud, including ancient. a. Centrifugal separation: using a centrifuge to remove waste mud. b. Drying: the waste obtained from the above steps The liquid is separated; the hair is dried, and the remaining liquid is c. Grinding: the powder obtained by the above steps is finely powdered; 4 Ding grinding 'grinding the Shixi waste mud into d. The first wind blowing separation: The above-mentioned step.]m _ 〃 件 之 矽 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 进行 粉末 粉末 粉末 粉末 粉末 粉末 粉末 粉末 粉末 粉末 比重 比重 比重 比重 比重 比重 比重Crystal; e. Electrostatic separation: the above-mentioned steps are carried out in the static eight-year-old, surface (four), carbonized and broken crystals, and the electrosurgical knife is removed, and the charged ion is used to leave the carbonized stone and the stone crystal; 'The metal material is divided into f. The first = wind blow separation: _ step _ carbon cut _ body again into the 尔 尔 , , 利用 利用 , , , , , , , , , , , , , , , , , , , , , , 比重 比重 比重 比重 比重 比重2. If you want to look at the mud when you are looking at the mud, you can use the yarn to ride the 亥 石 夕 夕 夕 夕 夕 夕 晶体 晶体 晶体 晶体 晶体 晶体 晶体 晶体 晶体 晶体 晶体 晶体 晶体 晶体 加入 加入 加入 加入 加入 加入 加入 加入 加入 加入 加入 加入 加入 加入Oxidation. 虱201240918 3· dp-kirjrH B SA Λ. / (〇. Receipt and manufacture of Shi Xijing spinning method, in which the 曰曰 曰曰 body is used in the furnace of the hanging pot During the melting process, amorphous carbon powder can be added to the periphery of the ray, which is called a crystallized towel to produce oxidation. 4. As for the method of spraying the mud as described in the article 丨 围 及 及 及 及 制 制 制 制 制 制After melting into the molten iron in the steel, the temperature gradient control can be used to slowly cool the crucible in the crucible to the normal temperature, so as to use the temperature difference from the bottom to the upper layer to make the directional aging crystal. Broken crystal
TW100111541A 2011-04-01 2011-04-01 Method for waste silicon slurry recovery and silicon ingot preparation TW201240918A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI481559B (en) * 2013-06-13 2015-04-21 Chung Wen Lan Method for recycling and purifying silicon particles from silicon slurry
CN108383122A (en) * 2018-05-04 2018-08-10 河南润祥新材料科技有限公司 A kind of ultra-fine pSi powder recycling method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI481559B (en) * 2013-06-13 2015-04-21 Chung Wen Lan Method for recycling and purifying silicon particles from silicon slurry
CN108383122A (en) * 2018-05-04 2018-08-10 河南润祥新材料科技有限公司 A kind of ultra-fine pSi powder recycling method

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