200521082 五、發明說明（1) 【發明所屬之技術領域】 本發明是關於一種似球塑矽粗顆粒之製造方法及其# 置，特別是關於一種低成本之一種似球型矽粗顆粒之製造 方法及其裝置。 < 【先前技術】 矽的用途非常廣泛，尤其半導體、光電、微機電及奈 米等技術更是建築在石夕材料上的龐大產業。特別是半導體 產業所使用的矽單晶（Si Single Crystal)，基於其特殊 性質以及其原料矽砂（二氧化矽）於地表的含量豐富，在現 今的積體電路應用上扮演無可取代的關鍵角色。 從製造成本的考量上，目前絕大部份的積體電路用的 矽晶圓（Si 1 i con Wafer )，均由所謂的柴氏法 (Czochralski Method)成長矽單晶棒再加以裁切而成。 通常在矽單晶棒之長晶製程中，均需使用符合半導體業規 格之高純度矽晶材料作為原料。一般高純度矽晶材料生產 由矽砂開始，經由電弧爐的提煉還原成冶金級的矽，再經 由鹽酸氯化（Hydr0chlorinati〇n )、蒸餾 、 (Distillation)純化之後，透過慢速分解 (DisComposition )還原過程析出高純度多晶矽，再將此 析出之矽晶材料擊碎成塊狀（chunk)。然後將上述之 度塊狀矽晶材料置於柴氏（Cz〇chralski)長晶爐中加埶至 ，巧融再進行拉伸長晶，由於這些大塊狀㈣晶材料报 :^成大孔隙使得矽晶材料於長晶爐充填率报低造成 製程設備的空間浪費，嶋要一些較小的顆粒狀=200521082 V. Description of the invention (1) [Technical field to which the invention belongs] The present invention relates to a method for manufacturing spherical plastic-like silicon coarse particles and its arrangement, especially to a low-cost production of spherical-like silicon coarse particles. Method and device. < [Previous technology] Silicon has a wide range of uses, especially semiconductor, optoelectronics, micro-electromechanical and nano-technology, etc. is a huge industry built on Shixi materials. In particular, the silicon single crystal (Si Single Crystal) used in the semiconductor industry, based on its special properties and its rich content of silicon sand (silicon dioxide) on the ground, plays an irreplaceable key in today's integrated circuit applications. Roles. From the perspective of manufacturing cost, most silicon wafers used in integrated circuits (Si 1 i con Wafer) are grown by the so-called Czochralski Method and then cut. to make. Generally, in the process of growing a silicon single crystal rod, a high-purity silicon crystal material conforming to the specifications of the semiconductor industry is used as a raw material. Generally, the production of high-purity silicon crystal materials begins with silica sand, which is reduced to metallurgical silicon by refining in an electric arc furnace, and then purified by hydrochloric acid chloride (Hydrogen chloride), distillation, and (Distillation), and then through slow decomposition (DisComposition) During the reduction process, high-purity polycrystalline silicon is precipitated, and the precipitated silicon crystal material is crushed into chunks. Then the above-mentioned bulk silicon crystal material is placed in a Czochralski crystal growth furnace, and then the crystal is stretched. Since these large crystal materials are reported to form large pores As a result, the filling rate of the silicon crystal material in the crystal growth furnace is reported to be low, which causes a waste of space in the process equipment. Some smaller particles are required =
第6頁 200521082 五、發明說明⑵ 1 料作為空隙的有效添加料，以控制長晶爐内可達最大的長 晶量，亦即使製程效益達到最大，如此可大幅提升 言^ 備的有效使用率。 ' ° 因此’於矽晶材料的長經過程中需要一些較小的矽粗 顆粒來填補塊狀矽晶材料的空隙。這種次於大塊卻又須大 2 —般粉末狀的矽晶材料的成形問題，一直困擾高純度矽 曰曰材料生產者，因為不但要使矽粗顆粒的尺寸能適當的填 補於空隙，且矽粗顆粒的形狀又必須具備一定的流動性或 滾動性，才能在有效的充填於矽塊料之間而發揮其作用。 習知=做法大都使用流體床進行反應以取得矽粗顆粒，如 吴國第60 0 786 9號專利與美國第478 6477號專利中 =矽粗顆粒製程，藉由反應氣體形成流體 : # ^ ^ ^ 知末作為矽日日種。矽粉在流體床中 ^仃的才間中，同犄加熱反應氣體使其與矽粉產生沉積反 二：使:夕T成長成大顆粒，而達到粗顆· 狀 是使用流體床方法的成長速度太慢，使其成本 於美國第4532090號專利提及另一鍤古 的製造方法，其將石夕炫融液直接傾_ '、、、屯度石夕粗顆粒 iv制π λ. , 1丑按1貝倒（Ρ0 u r 1 n g)入液體中 以I付石夕粗顆粒。然而此簡單 寸大小與形狀。 門早方法很難控制矽粗顆粒之尺 【發明内容】 為改善以上所述習知技術的問 球型矽粗顆粒之製造方法及明扣供一種似 无及其衣置，以降低高純度矽粗顆Page 6 200521082 V. Description of the invention ⑵ 1 material as an effective additive for the void to control the maximum amount of crystals in the crystal growth furnace, and even if the process efficiency reaches the maximum, this can greatly improve the effective use of equipment . '° Therefore, some small coarse silicon particles are needed to fill the voids of the bulk silicon material during the long warping process of the silicon material. This problem of forming silicon powder materials, which are second to large but powdery, has always troubled the producers of high-purity silicon materials, because not only must the size of the coarse silicon particles be properly filled in the gaps, In addition, the shape of the coarse silicon particles must have certain fluidity or rolling properties, in order to effectively fill the silicon blocks and play their role. Conventional = most of the methods use a fluid bed to perform reactions to obtain coarse silicon particles, such as Wu Guo No. 60 0 786 9 and US Patent No. 478 6477. In the process of silicon coarse particles, a fluid is formed by a reaction gas: # ^ ^ ^ Zhi Mo as a Silicon Sun. When silicon powder is in the fluid bed, the reaction gas is heated to make it deposit with the silicon powder. The second is to make: Xi T grow into large particles, and the coarse particles are shaped. The growth is using the fluid bed method. The speed is too slow, making it cost in U.S. Patent No. 4532090 mentioning another ancient manufacturing method, which directly pours the Shi Xixuan melt _ ',,, Tundu Shi Xi coarse particles iv λ λ., 1 Ugly pour 1 ng (P0 ur 1 ng) into the liquid to give I Shi Xi coarse particles. However this simple size and shape. Early gate method is difficult to control the scale of silicon coarse particles [Abstract] In order to improve the above-mentioned conventional technology, a method for manufacturing spherical silicon coarse particles and an open button are provided to reduce the high-purity silicon. Coarse
ΗΊΗΊ
五、發明說明（3) 粒的製造成本；並且， ^ 調整石夕粗顆粒之尺+ I ;糟由叙置與製程參數的控制來 L ' T大小與形狀。 本發明係將矽原料熔融之 卻流體之腔體中，使石夕 更’直接將矽熔融液滴入冷 並由於表面張力而得刹^ :的過程中固化成粗顆粒狀， 的設計可以控制滴入^^形之粗顆粒矽。而透過裝置 徑、冷卻液體之液位古^ ^ $流入冷卻液體的流嘴口 步調整高溫矽熔融液滴 ^孔體£力，末進一 為達上述目的成形時之外型與粒徑大小。 " 的似球型矽粗顆粒之製造方、去之牛驟勹 含有··首A，提供容置冷卻液俨乂：衣：方法之步驟包 熔融狀態以形成矽熔融、夜·接供=_ #矽原料加熱至 吏夕^㈣液通過流嘴注入於冷卻液體 = 夕。由於石夕炫融液與冷卻液體接觸時， Γ 液 熱會導致劇烈的喷濺現象，其所產生之劇η ，切作用力將使㈣融液切割成小顆…經表面二 作用則使㈣融液在固化為粗秒顆粒的過程中形成近似球 狀的外型。然其矽粗顆粒之粒徑大小取決於矽熔融液盥冷 卻流體接觸時之液柱尺寸，可透過改變流嘴口徑與冷卻液 體之液面南度來加以控制。 配合以上之方法，本發明更包含一種似球型矽粗顆粒 之製造裝置，其包含盛料桶、流嘴以及腔體，盛料桶係用 以容置矽熔融液，腔體係容置冷卻液體，流嘴連接盛料桶 與腔體，使矽熔融液匯流至流嘴以進入腔體，並注二於冷 卻液體以固化成粗顆粒矽。 、~ 200521082 五、發明說明（4) 為使對本發明的目的、構造、特徵及其功能有進一步 的了解，茲配合圖示詳細說明如下·· 【實施方式】 請參考第1圖，其為本發明實施例之裝置示意圖，其 包含石英坩堝11 〇、高周波加熱器111、石墨發熱體1丨2、 流嘴1 2 0、加熱線圈丨2 1、腔體1 3 0及收集槽1 4 0。為避免雜 質摻入，本發明實施例係使用石英坩堝（quartz crucible)作為盛料桶。 如第1圖所示，塊狀矽（Si chunk)原料1 〇〇係置於石英 掛塌11 0 ’而高週波加熱爐111則加熱石英坩堝11 〇外圍之 腔體1 3 0係容置純水 石墨發熱體1 1 2以將矽原料丨〇 〇熔化 ____^一…^且心小 131以作為冷卻液體並且可通入保護氣氛於腔體13〇，流嘴 120〜連接石英坩堝11〇與腔體13〇，使矽原料1〇〇熔融產生之 矽熔融液101匯流至流嘴12〇以進入腔體13〇，並注入於純 固化形成粗矽顆粒102。為使流嘴12〇保持暢通，於 机觜1 2 0處裝設一組加熱線圈丨2】作為流嘴丨2 〇之加埶源 = “通過流嘴120之石夕熔融液101即進人腔體130並 ，=、、、屯水131中以進行固化，收集 〇則 底部以，集沉降之粗石夕顆粒1〇2產物。 體130之 _ _上述衣置，進彳于似球 參考第2圖，盆Α太恭日日無/生7租顆粒之策w方法，請 令·舌各 ......本I月貝施例之製造流程圖，步驟包 各·百先，於腔體内容置純水 (步驟2 1 0 )，並诵A _ >从* 便/、保持疋之液面尚度 料置於石英掛二為保護氣1 ;取3公斤塊狀石夕原 央掛堝（步驟220 );將矽原料加熱至熔融狀態以 200521082 五、發明說明（5) 熔融液（步驟230 )，將高週波感應爐加熱 1550度至1 700度，矽原料即開始熔化；使矽熔融氏 嘴注入於冷卻液體以固化开彡点 ’通過流 : = 將石夕粗顆粒取出進行烘乾程序(步驟25〇)腔， 本發明之矽粗顆粒之製造方法可達到高產率。 表不 由粗顆粒之粒徑大小取決於石夕 的士 f 寸以及矽熔融液喷濺時的溫度與作用六 :大小，目而可透過改變流嘴口徑 j 來加以控㈣，流嘴 ；η,液面而度 一公；？ 5 Λ、 丨/從篮之液面咼度的距離可為 的石々+兩么尺，調整其距離可應用於製作不同尺寸大’】、 开^顆粒，請參考附件！至附件5，其為各 球 ^粗顆粒照片，合流嘴口徑 = 不同距離來分別製作。 f體液面间度的 合加=，Γί㈣内之石夕溶融液的溫度及其流動性可配 由流嘴二 施例之高週波加熱器，來加以控制，並藉 内通控制石夕熔融單位時間的流入量，並於腔體 數的，：Γΐ 的表面氧* ’本發明可透過製程參 保護氣气：融液的溫度及其流動性、流嘴的口徑、 粒度計：部液體液面高低！，進行石夕粗顆粒的形狀與 計，於製程中=i:以透t:央坩堝和加熱器所組成的設 的似球形矽粗顆粒。 逆貝式地里產具有流動性V. Description of the invention (3) The manufacturing cost of the granules; and, ^ adjust the size of the coarse granules of Shi Xi + I; the size and shape of L'T are controlled by the setting and process parameters. The invention melts silicon raw materials into a fluid cavity, so that Shi Xigeng directly drops the molten silicon liquid into cold and brakes due to surface tension. The process can be solidified into coarse particles. The design can be controlled. Add ^^-shaped coarse particles of silicon. The diameter of the cooling device and the liquid level of the cooling liquid pass through the nozzle of the cooling liquid. The high-temperature silicon molten liquid droplets are adjusted step by step, and the shape and particle size of the molding are achieved to achieve the above purpose. " The manufacturing method of spherical silicon-like coarse particles contains the first A, which provides the cooling liquid. 衣: clothing: The steps of the method include the molten state to form the silicon melt. _ #The silicon raw material is heated to the official evening ^ liquid is injected into the cooling liquid through the nozzle = evening. When Shi Xixuan's molten liquid is in contact with the cooling liquid, Γ liquid heat will cause a violent splash phenomenon. The sharp force η produced by it will cut the ㈣ melt into small pieces ... The molten liquid forms an approximately spherical shape during the process of solidifying into coarse-second particles. However, the particle size of the coarse silicon particles depends on the size of the liquid column when the silicon molten liquid is in contact with the cooling fluid, which can be controlled by changing the orifice diameter and the south of the liquid surface of the cooling liquid. In conjunction with the above method, the present invention further includes a spherical silicon-like coarse particle manufacturing device, which includes a material bucket, a spout, and a cavity. The material bucket is used to contain a silicon melt, and the cavity system contains a cooling liquid. The flow nozzle is connected to the tub and the cavity, so that the molten silicon liquid flows to the flow nozzle to enter the cavity, and is injected into the cooling liquid to solidify into coarse particles of silicon. ～ 200521082 V. Description of the invention (4) In order to further understand the purpose, structure, features and functions of the present invention, detailed descriptions are given in conjunction with the drawings as follows: [Embodiment] Please refer to Figure 1, which is based on The schematic diagram of the device of the embodiment of the invention includes a quartz crucible 110, a high-frequency heater 111, a graphite heating element 1 丨 2, a flow nozzle 1 2 0, a heating coil 21, a cavity 1 3 0, and a collecting tank 1 40. In order to avoid the inclusion of impurities, the embodiment of the present invention uses a quartz crucible as the container. As shown in Fig. 1, the bulk silicon (Si chunk) raw material 100 is placed in the quartz slump 11 0 ′, and the high frequency heating furnace 111 is used to heat the quartz crucible 11 〇 The outer cavity 1 30 is contained in pure Water graphite heating element 1 12 to melt the silicon raw material 丨 〇〇 ____ ^ 一 ... ^, and the small core 131 as a cooling liquid and can pass into a protective atmosphere in the cavity 13O, the nozzle 120 ~ connected to the quartz crucible 11〇 With the cavity 130, the silicon melt 101 generated by melting the silicon raw material 100 is converged to the flow nozzle 120 to enter the cavity 130, and injected into pure solidification to form coarse silicon particles 102. In order to keep the nozzle 12o unobstructed, a set of heating coils are installed at the machine 1200. 2] as the nozzle 丨 2 0 plus the source = "Enter the stone melt solution 101 through the nozzle 120 The cavity 130 is solidified in = ,,, and water 131, and the bottom is collected, and the sedimentary coarse stone particles 102 are collected. The product of the body 130 _ _ above is placed in a ball-like reference. Fig. 2, the method of basin A is too noble to produce / rent 7 particles every day, please order each tongue ... The manufacturing flow chart of this month's bebe example, the steps include each one hundred, Place pure water in the cavity (step 2 1 0), and chant A _ > from * 、 /, keep the liquid level of 疋 置于 material placed in the quartz hanging 2 as protective gas 1; take 3 kg of block stone eve The original central hanging pot (step 220); heating the silicon raw material to a molten state according to 200521082 V. Description of the invention (5) Melting liquid (step 230), heating the high frequency induction furnace 1550 degrees to 1 700 degrees, the silicon raw material begins to melt ; Inject the molten silicon mouth into the cooling liquid to solidify the opening and closing point 'through flow: = take out the Xixi coarse particles and perform the drying process (step 25) in the cavity. The production method can achieve high yields. The size of the coarse particles depends on the size of the Shixi taxi and the temperature and effect of the molten silicon spray. The size can be controlled by changing the nozzle diameter j. ㈣, running mouth; η, the liquid level is equal to one degree; 5 Λ, 丨 / The distance from the liquid level of the basket can be equal to two stone feet + adjusting the distance can be used to make different sizes. ], To open the particles, please refer to the attachment! To the attachment 5, which is a photo of each ball ^ coarse particles, the diameter of the confluence mouth = different distances to make separately. The temperature and fluidity can be controlled by the high frequency heater of the second embodiment of the nozzle, and the inflow of the unit melting time of Shi Xi is controlled by the internal pass, and the surface oxygen of the number of cavities: Γΐ * 'The present invention can protect the gas through the process parameters: the temperature of the melt and its fluidity, the diameter of the nozzle, the particle size meter: the level of the liquid level of the liquid !, the shape and calculation of the coarse particles of Shi Xi, in the process = i: through t: central crucible and heater-like ball Coarse silicon particles. Belleville inverse yield a flowable ground
200521082 五、發明說明（6) 雖然本發明之較佳實施例揭露如上所述，然其並非用 以限定本發明，任何熟習相關技藝者，在不脫離本發明之 精神和範圍内，當可作些許之更動與潤飾，因此本發明之 專利保護範圍須視本說明書所附之申請專利範圍所界定者 為準。200521082 V. Description of the invention (6) Although the preferred embodiment of the present invention is disclosed as described above, it is not intended to limit the present invention. Any person skilled in the relevant arts may make the same without departing from the spirit and scope of the present invention. With some changes and retouching, the scope of patent protection of the present invention must be determined by the scope of the patent application attached to this specification.
第11頁 200521082 圖式簡單說明 第1圖為本發明實施例之裝置示意圖； 第2圖為本發明實施例之製造流種圖： 附件1至附件5，豆為久接斗夕 ’及 片 ”馬各種尺寸之似球 $矽粗顆粒照 圖式符號說明】 100 矽原料 101 梦炫融液 102 粗矽顆粒 110 石英掛禍 111 高周波加熱器 112 石墨發熱體 120 流嘴 121 加熱線圈 130 腔體 131 純水 140 收集槽 步驟2 1 〇 高度 於腔體内$ 步驟220 取3公斤塊 步驟230 將矽原料i 步驟2 4 〇 使矽熔融ί' 化形成矽粗顆粒 步驟25〇 烘乾程序 洩放腔體fPage 11 200521082 Brief description of the drawings. Figure 1 is a schematic diagram of the device according to the embodiment of the present invention. Figure 2 is a manufacturing flow chart of the embodiment of the present invention: Attachment 1 to Attachment 5. Beans are long time to fight. Horses of various sizes resembling balls $ Silica coarse particles according to diagrammatic symbols] 100 Silicon material 101 Mengxuan melt 102 Coarse silicon particles 110 Quartz hanging 111 High frequency heater 112 Graphite heating element 120 Flow nozzle 121 Heating coil 130 Cavity 131 Pure water 140 collection tank Step 2 1 0 Height in the cavity $ Step 220 Take 3 kg blocks Step 230 Melt the silicon raw material Step 2 4 〇 Melt the silicon to form silicon coarse particles Step 25 Bake out the cavity in the cavity Body f