TW201226341A - Method for making quartz crucible for casting polycrystalline silicon ingot - Google Patents

Method for making quartz crucible for casting polycrystalline silicon ingot Download PDF

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TW201226341A
TW201226341A TW99146307A TW99146307A TW201226341A TW 201226341 A TW201226341 A TW 201226341A TW 99146307 A TW99146307 A TW 99146307A TW 99146307 A TW99146307 A TW 99146307A TW 201226341 A TW201226341 A TW 201226341A
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quartz
polycrystalline
slurry
quartz crucible
powder
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TW99146307A
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TWI415807B (en
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Yan-Cen Pan
Bao-Cai Chen
yu-zhen Huang
Kun-Min Zhang
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Sunward Refractories Co Ltd
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Abstract

A method for making a quartz crucible for casting polycrystalline silicon ingot comprises: (A) compounding a fine silicon powder with a particle size not greater than 500 μm, the crude silicon powder with an average particle size of 0.1 mm to 2 mm, a dispersant mainly containing the polycarbonate, a plasticizer mainly containing the alcohol polymer, and the water to form a slurry; (B) injecting the slurry under a normal pressure into a plaster mold and demolding after the slurry is cured to obtain a blank; and (C) sintering the blank after it is dried to obtain the quartz crucible. The quartz crucible made according to the present invention has a high density and a high anti-bending strength and is resistant to the impact. In addition, the present invention has a low production tolerance during fabrication, so it can provide better market competition edges.

Description

201226341 六、發明說明: 【發明所屬之技術領域】 本發明是有關於一種灌t成型(si ipcasting)的技術, 特別是指一種鑄造多晶矽晶錠用的石英坩堝的製作方法。 【先前技術】 多晶石夕太陽能電池的基礎物料之一是多晶矽晶圓 (P〇 1 y-si 1 icon waf er),多晶矽晶圓的品質優劣對於製作出201226341 VI. Description of the Invention: [Technical Field] The present invention relates to a technique of siping, and in particular to a method for producing a quartz crucible for casting a polycrystalline ingot. [Prior Art] One of the basic materials of the polycrystalline solar cell is a polysilicon wafer (P〇 1 y-si 1 icon waf er), and the quality of the polycrystalline silicon wafer is produced.

的多晶矽太陽能電池的光電轉換效率有直接的影響;而由 於多晶矽晶圓是多晶矽晶錠(ing〇t)切割加工的產物也因 此,製作多晶矽晶錠時,會直接接觸到液體矽原料的『載體』 的品質,也對於之後製作出的多晶石夕太陽能電池的作動表』 現’有著十分關鍵的重要影響。 目前,製作多晶⑪晶鍵時用以盛裝液时原料的載體 批覆有氮切(Si3N4)的石英_,屬於—種__次性使用1 消耗品,無料次❹,且其品質大抵受限於各生產業者t 獨家生產過程而會有氣孔率較高、或抗折強度不夠帅 (一般而言,是以國外產製的石英㈣的出貨時例如& 羊、吸水率、體密度、抗㈣度的品質檢測結果作為石英土 =對樓準)。因此,如何以低製程成本生產高品, r二坩堝’疋目刚相關業者—個相當重要的課題。 【發明内容】 u此’本發明之目的 折強声古a# '即在提供一種生產氣孔率低、 的轉造多晶石夕晶鍵用的石英掛塥的製作方法。 ;疋本發明鏵造多晶石夕晶鍵用的石英掛堝的製作 201226341 法,包含三步驟。 首先將粒徑不大於5叫m的細石夕粉、平均粒徑是 二粗·主成分是聚軸 刀疋醇類4 口物的增塑劑,和水混練成—聚料。 :以常壓注聚方式將該浆料注入—石膏模具中,並在該 漿料硬化後脫模得到一坯體。 然後乾燥該&體後進行燒結,即可製得該石英掛禍。 較佳地’細矽粉、粗矽粉、分散劑、增塑劑和水的配比 是 1 : 〇. 22~1. 5 : 1. ixin 5x1〇-3 : i 1χ1〇_4」5χΐ〇_3 : 0.卜0. 5。 較佳地混練製作该衆料時還以粒徑2丽七關的錯球 進行球磨。 較佳地,使用的該石膏模具是以石膏粉與水以〇. 72 :工 的比例混合後成型得到。 較佳地,是在25°C〜10(TC自然乾燥該坯體,再將乾燥 後的坯體在80ITC〜1001TC燒結,而製得該石英坩堝。 本發明之功效在於:提供一種完整的製作方法以低生產 成本製作具有低氣孔率及高抗折強度的石英坩堝,且生產時 產生的容許生產公差尺寸低。 【實施方式】 有關本發明之前述及其他技術内容、特點與功效,在以 下配合參考圖式之一個較佳實施例的詳細說明中,將可清楚 的呈現。 在本發明被詳細描述之前,要注意的是,在以下的說明 201226341 内容中,類似的元件是以相同的編號來表示。 參閱圖1,本發明鑄造多晶矽晶錠用的石英坩堝的製作 方法的一較佳實施例,用於製作出具有低氣孔率及高抗折強 度的石英坩堝。 首先進行步驟11,將粒徑不大於500 "m的細矽粉、平 均粒徑是0. 的粗矽粉、主成分是聚碳酸酯類的分散The photoelectric conversion efficiency of the polycrystalline silicon solar cell has a direct influence; and since the polycrystalline germanium wafer is a product of polycrystalline germanium ingot cutting, the polycrystalline germanium ingot is directly contacted with the carrier of the liquid germanium raw material. The quality of the slate is also very important for the actuating table of the polycrystalline stone solar cell produced later. At present, when the polycrystalline 11 crystal bond is produced, the carrier for the raw material for the liquid is coated with nitrogen-cut (Si3N4) quartz _, which belongs to the __ sub-use 1 consumable, no material defects, and its quality is greatly limited. In the exclusive production process of each manufacturer, there will be a high porosity or a good flexural strength (generally, the shipment of quartz (4) made in foreign countries, for example, & sheep, water absorption, bulk density The quality test results of anti-(four) degrees are used as quartz soil = right. Therefore, how to produce high-quality products at low process costs is a very important issue. SUMMARY OF THE INVENTION The object of the present invention is to provide a method for producing a quartz enthalpy for converting a polycrystalline quartz crystal bond having a low porosity.疋 The production of the quartz entanglement for the production of polycrystalline stellite bonds in the present invention. The 201226341 method comprises three steps. First, the fine-grained powder with a particle size of not more than 5 m is used, and the average particle size is a plasticizer with a coarse particle and a main component of a polycyclic saponin, and is mixed with water to form a polymer. The slurry is injected into a gypsum mold by atmospheric pressure injection, and after the slurry is hardened, it is demolded to obtain a green body. Then, the & body is dried and then sintered to obtain the quartz. Preferably, the ratio of fine powder, coarse powder, dispersant, plasticizer and water is 1: 〇. 22~1. 5 : 1. ixin 5x1〇-3 : i 1χ1〇_4”5χΐ〇 _3 : 0. Bu 0. 5. Preferably, the ball is ground by a wrong ball having a particle size of 2 Liqiguan when the mass material is produced by kneading. Preferably, the gypsum mold used is formed by mixing gypsum powder and water in a ratio of 72. Preferably, the body is dried at 25 ° C to 10 (TC is naturally dried, and the dried body is sintered at 80 ITC to 1001 TC to obtain the quartz crucible. The effect of the present invention is to provide a complete production. The method produces a quartz crucible having a low porosity and a high bending strength at a low production cost, and has a production tolerance tolerance which is low in production. [Embodiment] The foregoing and other technical contents, features and effects of the present invention are as follows. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT OF THE PREFERRED EMBODIMENT OF THE PREFERRED EMBODIMENT OF THE PREFERRED EMBODIMENT OF THE PREFERRED EMBODIMENT Before the present invention is described in detail, it is noted that in the following description 201226341, similar elements are numbered the same. Referring to Fig. 1, a preferred embodiment of a method for producing a quartz crucible for casting a polycrystalline germanium ingot is used to produce a quartz crucible having a low porosity and a high flexural strength. First, step 11 is performed. Fine powder with a particle size of not more than 500 "m, coarse powder with an average particle size of 0. The main component is dispersion of polycarbonate

劑、主成分是醇類聚合物的增塑劑,和水以1 : 0.22〜1 5: 11χ1(Γ4〜1·5χ1(Γ3: i 1χ1〇\15χ1(Γ3: 〇1 〇 5 的配比混 練成一漿料;較佳地,混練製作該漿料時還以粒徑2随〜丨〇随 的锆球進行球磨而使得各原料混合的更為均勻,球磨後筛取 出該些錯球。 根據多次的嘗試,當使用的細矽粉粒徑大於5〇〇 "出 時,燒結出的石英坩堝會因為細矽粉粒徑過大而強度低。粗 矽粉的粒徑大於2mm時,燒結出的石英坩堝 就是氣孔率高),結構也鬆散,同時,混練得到的;;2 易出現粗矽粉沉澱的狀況而較不均勻;但粗矽粉的粒徑小於 〇_ 1mm時’則燒結得到的石英_的結構因為缺乏較大顆粒 的存在也會讓整體結構強度降低。分散劑與增_用於輔助 所製作出的聚料混合的更均勻以及令後續製作出㈣體且 有較佳的塑性而不易產生裂痕’二者的添加比例分別大於配 比的上限值時,燒結㈣石英_易出現氣孔,同時結構強 Μ㈣’ 低於配比τ限時’各原料無法均勾分 散,而導致後續製作出的坯體易產生裂痕。 刀 執行完步驟11得到混練均勻的聚料後即實施步驟12, 201226341 以常壓注漿方式將該漿料注入一石膏模具中,並在該漿料硬 化後脫模得到一坯體;較佳地,使用的該石膏模具是以石膏 粉與水以0.72: 1的比例混合後成型得到,且在將漿料注入 石膏模具之前,先進行真空脫泡10〜20分鐘。 最後實施步驟13,乾燥該坯體後進行燒結,即可製得 該石英堆禍;較佳地,本步驟是在25〇c〜1〇(rc自然乾燥該 坯體5小時,再將乾燥後的坯體在800。〇1000。(:燒結3小 時,自然降溫後即製得該石英坩堝。另外需注意的是,配合 各組成的配比,燒結溫度低於80(TC時燒結出的石英坩堝強 度不足,但大於丨〇〇〇〇c時會產生過大的晶相變化而導致成 品出現裂痕。 【實驗例] 將粒佐不大於500 V m的細矽粉、平均粒徑是0. 1關〜2mm 的粗石夕粉、主成分是聚碳酸®旨類的分散劑、主成分是醇類聚 °物的增塑劑,和水以1 : G. 9 : 0. _91 : G. _52 : 0. 3 的:比U2mm〜l〇mm的鍅球球磨並混合攪拌加分鐘,球磨 姐…_出4。鍅球’传到混合均句的梁料;將混練均勻的漿 2行真空脫泡20分鐘後’用常壓注漿方式將漿料注入石 極# '中_並在襞料硬化後脫模得到远體;於自然乾 燥該述體5小時後,胳# μρ # “ 曼將乾燥後的柱體在901TC燒結3小時, 自一降溫後製得石英_實驗樣品。 得的石英_實驗樣品進行品測,其氣孔率 ' 料廠商出售的商品(以相同的儀器進行檢 201226341 測,《I孔率為11.2%、吸水率為5 8%、體密度192g/cm3、 抗折強度18. 9MPa)相較,氣孔率、吸水率均較低,且抗折 強度較高。 综上所述,本發明是自原料配比開始,提出一最適配比 的漿料,並配合石膏模具以注漿方式成型㈣體再配合適 當的乾燥與燒結過程,從而製作出氣孔率低、抗折強度高的 製作多晶W㈣的石英㈣,另外,本發明進行生產時產The main component is a plasticizer for the alcohol polymer, and the water is mixed with 1: 0.22~1 5:11χ1 (Γ4~1·5χ1 (Γ3: i 1χ1〇\15χ1 (Γ3: 〇1 〇5) Preferably, the slurry is prepared by kneading with a particle size of 2 with the zirconium ball of the crucible to make the mixing of the raw materials more uniform, and the ball is sieved to remove the wrong balls. In the second attempt, when the particle size of the fine powder used is greater than 5 〇〇, the sintered quartz crucible will have a low strength due to the excessive particle size of the fine powder. When the particle size of the coarse powder is greater than 2 mm, the sintering is performed. The quartz crucible is high in porosity, and the structure is loose, and at the same time, it is obtained by mixing; 2 is prone to the condition of coarse powder precipitation and is less uniform; but when the particle size of the coarse powder is less than 〇 1 mm, then sintering is obtained. The structure of quartz _ will also reduce the strength of the overall structure because of the lack of larger particles. The dispersant and the _ used to assist the mixing of the produced material more uniform and the subsequent production of (four) body and better Plasticity is not prone to cracks. When the ratio of addition is greater than the upper limit of the ratio, respectively Sintering (4) Quartz _ easy to appear pores, while the structure is strong (4) 'When the ratio is lower than the ratio τ', the raw materials can not be dispersed, resulting in the subsequent production of the green body is prone to cracks. The knife is finished step 11 to get a uniform mixing of the material After step 12, 201226341, the slurry is injected into a gypsum mold by atmospheric pressure grouting, and demolded after the slurry is hardened to obtain a green body; preferably, the gypsum mold used is gypsum powder. It is obtained by mixing with water in a ratio of 0.72:1, and vacuum defoaming is performed for 10 to 20 minutes before injecting the slurry into the plaster mold. Finally, step 13 is performed, and the body is dried and then sintered to obtain a slurry. The quartz stacking fault; preferably, the step is 25 〇c~1 〇 (rc naturally drying the blank for 5 hours, and then drying the green body at 800 〇 1000. (: sintering for 3 hours, natural cooling) The quartz crucible is prepared afterwards. In addition, the sintering temperature is lower than 80 when the ratio of each composition is matched (the strength of the quartz crucible sintered at TC is insufficient, but it is too large when it is larger than 丨〇〇〇〇c). Crystal phase changes leading to finished product [Experimental example] The fine powder of the granules of not more than 500 V m, the average particle size is 0.1 to 2 mm of coarse stone powder, and the main component is a dispersing agent and a main component of polycarbonate®. It is a plasticizer for alcohols, and water is 1: G. 9 : 0. _91 : G. _52 : 0.3: 鍅 ball milling and mixing for more than U2mm~l〇mm, ball miller ..._出4. Ryukyu 'passed to the beam material of the mixed sentence; after degassing the mixed slurry 2 lines under vacuum for 20 minutes', the slurry was injected into the stone pole by the normal pressure grouting method. After the material was hardened, the mold was released to obtain a far body; after drying the body for 5 hours, the #μρ# “man was dried and sintered at 901TC for 3 hours, and a quartz_test sample was prepared after cooling. The obtained quartz _ experimental sample was tested and its porosity was measured by the manufacturer. (The same instrument was used to test 201226341, "I hole rate was 11.2%, water absorption rate was 5 8%, body density was 192 g/cm3, The flexural strength is 18. 9 MPa), the porosity and water absorption are lower, and the flexural strength is higher. In summary, the present invention starts from the ratio of raw materials, proposes a slurry with the most suitable ratio, and forms a (4) body with a gypsum mold to form a suitable drying and sintering process, thereby producing a low porosity. Polycrystalline W (four) quartz (four) with high flexural strength, in addition, the present invention is produced at the time of production

、奋許生產a差尺寸也較低’而具有較高的市場競爭優 ,故確實能達成本發明之目的。 〜权1主^施例而已,當不合匕 以此限定本發明實施之鈴簡 月匕 及發明說明内容所作之簡單的等:本發明申請專利範圍 明專利涵蓋之範圍内早的等效變化與修飾,皆仍屬本發 【圖式簡單說明】The production size of the production is also low, and the market competition is excellent, so the object of the present invention can be achieved. ~ 权1 主^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^ Modifications are still in the hair [simplified description]

圖1是一流程圖,說明本發明鑄 坩堝的製作方法的一較佳實施例。 造多晶石夕晶鍵用 的石英 201226341 【主要元件符號說明】 11 .....步驟 13.....步驟 12 .....步驟BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a flow chart showing a preferred embodiment of the method of fabricating the cast strand of the present invention. Quartz for making polycrystalline quartz crystal bonds 201226341 [Description of main components] 11 .....Steps 13.....Step 12 .....

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Claims (1)

201226341 七、申請專利範圍: 1 . 一種鎮造多晶石夕晶錠用的石說m a 4丨 叩刃石央坩堝的製作方法,包含: (Α)將粒徑不大於500 ,, M , h β m的細矽粉、平均粒徑是 0· lmm〜2mm的粗石夕伞、 .,N Q 私、主成分疋聚碳酸酯類的分散 劑、主成分是醇類平人Az_ u ^ 呢頰t合物的增塑劑,和水混練成一 漿料;201226341 VII. Patent application scope: 1. A method for making a stone for the production of polycrystalline stone ingots, said ma 4 丨叩 石 , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , β m fine powder, average particle size is 0·lmm~2mm coarse stone umbrella, ., NQ private, main component 疋 polycarbonate dispersant, the main component is alcohol flat Az_ u ^ cheek a plasticizer of the t compound, mixed with water to form a slurry; ⑴以常壓注漿方式將Μ料注人―石膏模具中,並在 該漿料硬化後脫模得到一坯體;及 (C)乾燥該㈣後進行燒結,製得該石英掛禍。 2·依據申請專利範圍第μ所述之缚造多晶石夕晶鍵用的石英 掛禍的製作方法,其中,細石夕粉、粗石夕粉、分散劑、增塑 劑和水的配比是1 : 0.22〜1.5: UxHM.mo-3: hlx 10—M. 5xl(T3 : 〇.卜〇 5。 3·依據申5月專利範圍第2項所述之鑄造多晶矽晶錠用的石英 掛禍的製作方法’其中,該步驟(Α)還以粒徑2mm〜10mm 的鍅球進行球磨。 4.依據申請專利範圍第3項所述之鑄造多晶矽晶錠用的石英 掛禍的製作方法,其中,該步驟(B)使用的石膏模具是 以石膏粉與水以〇 · 7 2 : 1的比例混合後成型得到。 •依據申睛專利範圍第4項所述之鑄造多晶矽晶錠用的石英 掛禍的製作方法,其中,該步驟(C)是在25。(: ~1〇〇。(:自 然乾燥該域體後,將乾燥後的坯體在8〇〇<=c 〜1〇〇0°c燒結, 製得該石英坩堝。(1) The crucible is injected into a gypsum mold by a normal pressure grouting method, and after the slurry is hardened, the mold is released to obtain a green body; and (C) the (4) is dried and then sintered to obtain the quartz. 2. The method for preparing a quartz crucible for binding a polycrystalline quartz crystal bond according to the scope of the patent application, wherein the ratio of fine stone powder, coarse stone powder, dispersant, plasticizer and water It is 1: 0.22~1.5: UxHM.mo-3: hlx 10—M. 5xl (T3: 〇. 〇 〇 5. 3. According to the patent of the May patent scope, the quartz hang for the polycrystalline bismuth ingot The production method of the disaster, wherein the step (Α) is also ball-milled with a 鍅 ball having a particle diameter of 2 mm to 10 mm. 4. A method for producing a quartz smash for casting a polycrystalline yttrium ingot according to claim 3 of the patent application scope, Wherein, the gypsum mold used in the step (B) is formed by mixing gypsum powder and water in a ratio of 〇· 7 2 : 1. • Quartz for casting polycrystalline niobium ingot according to claim 4 of the patent scope The manufacturing method of the catastrophe, wherein the step (C) is at 25. (: ~1 〇〇. (: After drying the domain naturally, the dried body is at 8 〇〇 <=c 〜1〇 The quartz crucible was obtained by sintering at 0 ° C.
TW99146307A 2010-12-28 2010-12-28 Method for making quartz crucible for casting polycrystalline silicon ingot TW201226341A (en)

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FR2858611B1 (en) * 2003-08-07 2006-11-24 Saint Gobain Ct Recherches PROCESS FOR MANUFACTURING A SINTERED AMORPHOUS SILICA PIECE, MOLD AND BARBOTIN IMPLEMENTED IN SAID METHOD

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