200821390 九、發明說明： 【發明所屬之技術領域】 本發明旨在提供一種濺鍍靶材回收之方法，尤適於應用在再生報 廢之氧化銦錫（ΙΤ0)濺鍍乾材或類似結構者。 【先前技術】 以賤鑛法將構成輕材的物質沉積到一基板上，係已廣泛的使用在 各類薄膜的製程上。以氧化銦錫（IT0)薄膜為例，因其具有高導電性，200821390 IX. Description of the Invention: [Technical Field] The present invention is directed to a method for recycling a sputtering target, which is particularly suitable for use in reclaiming indium tin oxide (ITO) sputter dry materials or the like. [Prior Art] The deposition of a material constituting a light material onto a substrate by a bismuth ore method has been widely used in the process of various types of films. Taking indium tin oxide (IT0) film as an example, because of its high conductivity,
以及對可見光具高透光率，和對紅外線具高反射率的特性，故常被運 用於電子光學、光電裝置上。 當濺鍍靶材報廢時，習知的靶材回收製程步驟如下： 1、 破碎：對廢靶外加應力使其粉碎。 2、 次出·加入酸液將廢乾中之銦及錫溶出。 、選擇性沉殿除錫：將步驟2之溶液用驗液加以調整冰值，使锡成 份沈澱析出，並過濾除去錫。 4置換於去除錫的之廢乾液内f入鋅片，讓銦辞進行置換，使廢 靶液中之銦離子還原成海綿銦。 5、電解：將海線銦由廢赠中取出，並將其加熱熔解以獲得粗姻， 再將粗銦賴轴陽極板，最齡人電解贿精鍊。 ^ 下之峨加_化，再騰融金屬注入 模具後冷卻成型，可回收精煉後之金屬銦。 再贺赫於上述製μ，產物並非氧化銦錫峡金屬錮，而由金屬銦 再製錄材尚需經過多道製程，無形中耗費過多資源，對於工業化量 5 200821390 . 錄為料彳’且電解後剩下的電練不聽理，對魏雨言也有-定 . 之影響。 &出種較節省資源、污染較小，且可有效並大量回收氧化 罐粉末的麟崎回收之方法，實為本發明之用意。 【發明内容】 本ι月之主要目的在提供一種可回收報廢乾材，以再生把材之濺 鍍把材回收之方法者。 • 本發㈤之次要目的在提供-種免於雜太乡獅，如免使用稀有 金屬銦礦’而可有效降低成本，高回收率及低污染之濺脉材回收之 方法者。 為達上述之目的，本發明之方法所採取之步驟係包括··一、清洗·· 利用酸液將廢紅之雜質溶解去除；二、粉碎··施力破碎廢把，破碎 後粉粒粒徑須小於300微米；三、溶解··利用溫度在5〇〜15〇〇c之間 的酸液加入攪拌而將粉碎後粉粒溶解；四、過濾：將溶解後之廢靶溶 ® 解液過渡，分離雜質；五、解膠··加入鹼液至廢靶溶解液中，控制ph 值，使原本澄清之溶液產生微粒懸浮沉澱物，並持續攪拌使其分散； 六、中和沉澱··將解膠後之溶液加入鹼液，調整ph值，使溶液產生完 全沉澱；七、水洗過濾··將上述溶液經過濾，並用純水重新打散濾餅， 此動作重複一遍以上，形成水洗後之懸浮液；八、乾燥：將水洗後的 - 懸浮液乾燥，得到白色之氫氧化錮錫（Indium Tin Hydroxide)粉末； 以及九、煆燒：將白色之氫氧化錮錫（In(iium Tin Hydroxide)粉末置 6 200821390 入高溫爐職，即可料魏之氧彳_(lndium Tin Gxide powder) 粉末；藉上述步驟，即可由練上回收氧化錮錫（Mi⑽Tin Oxide P〇Wder)粉末’帛U再錄仙錫靶材者。 本發3之其他特點及具體實施例可於以下配合 中，進一步瞭解。 【實施方式】 請參第1圖，本發明之製程係包括以下步驟： /月洗10 ·利用酸液將廢輕上之雜質溶解去除； 粉碎2 0 ·施力破碎廢耙，破碎後粉粒粒徑須小於5〇〇微米； /合解3 0 ·糊/JnL度在5G〜150 C之間的酸液加人辦:而將粉碎後粉粒 溶解； 過慮4 0 ·將溶解後之廢把溶解液過渡，分離雜質； 解膠5 0 :加人驗液至廢総液中，㈣⑪值，使原本澄清之溶液產 生微粒懸浮沉殺物，並持續攪拌使其分散； 中和沉澱6 0 :將解膠後之溶液加入鹼液，調整此值，使溶液產生完 全沉澱； 水洗過濾7 0 :將上述溶液經過濾，並用純水重新打散濾餅，此動作 重複一遍以上，形成水洗後之懸浮液； 乾燥8 0 :將水洗後的懸浮液乾燥，得到白色之氫氧化銦锡（IndiumTin Hydroxide)粉末;以及 煆燒9 0 :將白色之氫氧化錮鍚（Indium Tin Hydroxide)粉末置入高 溫爐煆燒，即可得黃綠色之氧化銦錫（Indium Tin 〇xide 200821390 ^ Powder)粉末者。 • 〃•騎時’錢_魏麟練社之雜質轉去除，利用 讀機械或其他應力破碎廢鞑，使破碎後粉粒粒徑小於咖微米，加 又在50 C〜150 C之含有較的酸液並加以麟將躲粉溶解， 唯有〇C 150C、/辰度為6〜15N之含_素的熱酸液可逹的.篇以上 的命解效率，將溶解之廢靶溶解液過濾、，分離雜質，加入濃度為⑼〜 15N的鹼液於廢把溶解液，控制ph值之範圍為η，並檀摔2〜^小 φ 彳予以解膠’並力认?農度為1Ν〜鹽的驗液至解膠後的廢乾溶液中， 調至適當ph值，該Ph值之調整範圍為3〜9，使原本澄清之溶液產生 沉澱，將上述溶液經過濾，並用純水重新打散濾餅，如此動作重複一 遍以上，形成水洗後的懸浮液，將懸浮液予以乾燥，得到白色之氫氧 化銦錫（Indium Tin Hydroxide)之粉末，將白色氫氧化錮錫(jndium Tin Hydroxide)之粉末置入高溫爐，以升溫速率1〜20°C/min，持溫 溫度為300°C〜1100°C，持溫時間為0· 5〜5小時，煆燒成黃綠色之氧 _ 化銦錫（Indium Tin Oxide powder)粉末，用以再生把材者。 本發明於溶解步驟中，使用50°C〜150°C、濃度為6〜15N之含_ 素的熱酸液溶解廢輕粉，令廢輕粉的溶解效率高逹99· 8%，並於廢乾 液中直接加入鹼液中和，故可直接再生濺鍍靶材而非回收金屬銦者。 , 綜上所述，本發明揭示一創新之濺鍍靶材回收之方法，有效改進 ^ 一般使用常溫酸液較無法溶解金屬氧化物之缺失’同時利用熱酸液以 高逹99· 8%的溶解效率來溶解廢靶粉之藏鍍靶材回收之方法，具有新 8 200821390 穎性，因不需使用銦礦，可以節省資源，有效降低成本，於產業上具 利用價值，爰依法提出發明專利申請。 以上所述者，僅為本發明之較佳實施例而已，舉凡依本發明申請 專利細圍所做之鱗設計變化，均絲本案之技術所涵蓋。 200821390 【圖式簡單說明】 第1圖係為本發明之製造流程圖 【主要元件符號說明】 10 清洗 2 0 粉碎 3 0 溶解 4 0 過濾 5 0 解膠 6 0 中和沉澱 70 水洗過渡 8 0 乾燥 9 0 煆燒As well as high transmittance for visible light and high reflectivity for infrared light, it is often used in electro-optical and optoelectronic devices. When the sputtering target is scrapped, the conventional target recycling process steps are as follows: 1. Crushing: external stress is applied to the waste target to cause pulverization. 2. The second time and the addition of acid solution dissolve the indium and tin in the waste. Selective sinking in the tin: The solution of step 2 is adjusted with the test solution to adjust the ice value, and the tin component is precipitated and filtered to remove the tin. 4 Displace the zinc in the waste dry liquid from which tin is removed, and replace the indium to reduce the indium ions in the waste target liquid to sponge indium. 5, electrolysis: the sea line indium is taken out of the waste gift, and it is heated and melted to obtain the crude marriage, and then the crude indium anode shaft plate, the oldest person electrolysis and refining. ^ The next step is to add _, and then melt the metal into the mold and then cool it to recover the refined metal indium. In addition to the above-mentioned system μ, the product is not indium tin oxide gab metal, but the metal indium re-recording material still needs to go through multiple processes, invisibly consume too much resources, for the industrialization amount 5 200821390. Recorded as material and electrolysis After the remaining electric training is not reasonable, Wei Yuyan also has a certain effect. & It is the intention of the present invention to produce a method of recycling the arsenic which is more resource-saving, less polluting, and which can effectively and efficiently recover the oxidation can powder. SUMMARY OF THE INVENTION The main purpose of this month is to provide a method for recovering waste materials that can be recycled to regenerate the sputtered materials of the materials. • The secondary purpose of this (5) is to provide a method for the reduction of cost, high recovery and low pollution of recycled veins, which is free from the use of rare metal indium mines. In order to achieve the above purpose, the steps taken by the method of the present invention include: 1. cleaning, using acid to dissolve impurities of waste red; second, crushing, applying force to break the waste, and crushing the powder The diameter must be less than 300 microns; 3. Dissolve · Use the acid solution with a temperature between 5〇~15〇〇c to stir and dissolve the pulverized powder; 4. Filter: Dissolve the dissolved target solution solution Transition, separation of impurities; 5, degumming · Add lye to the waste target solution, control the pH value, so that the original clarified solution produces a particle suspension precipitate, and continue to stir to disperse; 6. Neutralization precipitation · Add the solution after degumming to the alkali solution, adjust the pH value to make the solution completely precipitated; 7. Wash the water filter. · Filter the above solution and re-disperse the filter cake with pure water. This action is repeated more than once to form a water wash. Suspension; VIII. Drying: The washed-suspension is dried to obtain a white Indium Tin Hydroxide powder; and ninth, simmering: white tin strontium hydroxide (In(iium Tin Hydroxide) ) powder set 6 200821390 Into the high temperature furnace, you can use the lndium Tin Gxide powder. By the above steps, you can recover the tin oxide (Mi(10)Tin Oxide P〇Wder) powder. Other features and specific embodiments of the present invention can be further understood in the following aspects. [Embodiment] Referring to Figure 1, the process of the present invention includes the following steps: / month wash 10 · use of acid to waste Dissolve and remove impurities on the light; pulverize 2 0 · apply force to break the waste sputum, the particle size of the granules must be less than 5 〇〇 micron after crushing; / 3 3 · paste / JnL degree between 5G~150 C Adding people to do: and dissolving the pulverized powder; over-treating 4 0 · Dissolving the dissolved waste to dissolve the solution, separating impurities; Dissolving 50: Adding the test to the waste sputum, (4) 11 value, so that the original clarification The solution produces a particulate suspension sinker and continues to stir to disperse; neutralize the precipitate 60: the solution after degumming is added to the alkali solution, and the value is adjusted to completely precipitate the solution; the water is washed and filtered. Filtered and re-dispersed the filter cake with pure water. This action is repeated more than once. Forming a water-washed suspension; drying 80: drying the washed suspension to obtain a white Indium Tin Hydroxide powder; and calcining 90: whitening yttrium hydroxide (Indium Tin Hydroxide) The powder is placed in a high-temperature furnace and burned to obtain yellow-green indium tin oxide (Indium Tin 〇xide 200821390 ^ Powder) powder. • 骑• riding time 'money _ Wei Lin Lianshe's impurities are removed, using reading machinery or other stress Breaking the waste mites, so that the particle size after crushing is less than that of the coffee micron, and adding the acid in the 50 C~150 C and the lining will dissolve the hiding powder, only the 150C 150C, / Chen degree is 6~15N The thermal acid solution containing _ 逹 can be used for the above-mentioned prosperous solution efficiency, the dissolved waste target solution is filtered, and the impurities are separated, and the lye at a concentration of (9) to 15N is added to the waste solution to control the pH value. The range is η, and the sandal fall 2~^ small φ 彳 is degummed 'and the strength is recognized? The agricultural degree is 1Ν~ salt test liquid to the decontaminated waste dry solution, adjusted to the appropriate pH value, the Ph value The adjustment range is 3 to 9, so that the originally clarified solution is precipitated, and the above solution is passed. And re-disperse the filter cake with pure water, repeating this action more than once, forming a water-washed suspension, and drying the suspension to obtain a white powder of Indium Tin Hydroxide, white tin strontium hydroxide (jndium Tin Hydroxide) powder is placed in a high temperature furnace at a heating rate of 1 to 20 ° C / min, holding temperature of 300 ° C ~ 1100 ° C, holding temperature of 0 · 5 ~ 5 hours, simmering into yellow Green Oxygen _ Indium Tin Oxide powder is used to regenerate the material. In the dissolving step, the dissolving waste light powder is prepared by using a hot acid solution containing 50% to 150° C. and having a concentration of 6 to 15 N, so that the dissolving efficiency of the waste light powder is higher than 99·8%, and The waste liquid is directly neutralized by the alkali solution, so that the sputtering target can be directly regenerated instead of recovering the metal indium. In summary, the present invention discloses an innovative method for recycling a sputtering target, which is effective for improving the general use of a normal temperature acid solution which is incapable of dissolving the absence of metal oxides while using a hot acid solution at a high level of 99.8%. The method of dissolving efficiency to dissolve the target of the target of the waste target powder has the novelty of 200821390. Because it does not need to use indium ore, it can save resources, effectively reduce the cost, and has the use value in the industry. Application. The above description is only the preferred embodiment of the present invention, and the scale design changes made by the patent application according to the present invention are covered by the technology of the present invention. 200821390 [Simple description of the drawings] Fig. 1 is a manufacturing flow chart of the present invention [Major component symbol description] 10 Cleaning 2 0 Crushing 3 0 Dissolving 4 0 Filtration 5 0 Dissolving 6 0 Neutralizing precipitate 70 Washing transition 8 0 Drying 9 0 煆烧