201201928 六、發明說明： 【發明所屬之技術領域】 本發明係有關一種透明導電金屬氧化物粉末之方法，特別是指一 種以低溫共沉澱法來製作更精確的控制掺雜比例及提高導電性質之透 明導電金屬氧化物粉末。 【先前技術】 目前，金屬透明導電氧化物(transparent conductive oxide, TCO) 薄膜是指具有高導電性，以及對可見光具高透光率，和對紅外線具高 反射率的薄膜，因此被廣泛的運用於太陽能電池的透明電極平板顯 不器的驅動裝置和光偵測器、透明加熱元件、抗靜電膜、電磁波防護 膜等電子、光學與光電裝置上，尤其是液晶顯示器(LCD)的透明導電電 極材料。為獲得可見光區的透明性，TCO材料通常採用能隙寬度大於 可見光能量的半導體金屬氧化物，並在半導體金屬氧化物材料中摻雜 雜質增加導電性’例如：在氧化銦中加人少量錫形成氧化銦錫薄膜 (ITO)，或在氧化鋅中摻雜鋁的氧化銘鋅薄膜(AZ0);而TC〇薄膜的導 電特性除受製程方法及製程條件的影響外，摻雜金屬雜質的比例更是 影響TCO薄膜導電特性的關鍵因素。目前工業上製備TC〇薄膜的主 要方法為錢鍍法，而濺鍍法乃利用以TCO粉末所製備之TC0靶材， 利用真空磁控濺鍍的方法進行由於靶材中因原料的組成與粒徑分佈等 因素，使得不同氧化物混合的均勻程度有其極限，且氧化物中可能包 含有不純物，因而影響到薄膜的導電性、透光性以及與基板的附著二。 因此’在製備TCO透明導電薄膜過程中所使用的濺鍍靶材，及製備濺 鍍靶材所需之多成份金屬TCO粉末也越來越受重視。 然而，目前多成份金屬TC0粉末的製造方法，主要是以混合控制 比例之個別金屬氧化物粉末進行固態反應法及利用不同方式製備所需 成份比例之化學法為主。但因固態反應法所製備的氧化物粉末，可能 因原始粉末之粒徑過大、混合不均及研磨產生的雜質污染等問題，造 201201928 而使得製備氧化物靶材及濺 成瑕燒後所得之氧化物粉末性質上劣化， 鍍法鍍製的薄膜性質變差。 上量產潛力的方法"。料姆料，狀驗是最具工業 原料，在_:解= 、高溫_製得多成 == 法繼爾擦雜的多成份透明導電=二 研究團隊人員魏前驅溶液鑛_騎劑，如氨水錢氧化納，^ 麟’若財和反毅驗度錄，會造成職溶液的溫 度升兩，當其缝溫度大於5(rc，w分成份的金屬離子，如辞離子 t與沉賴化合JL獅成氧錄而錢氧化物；另外若最終沉殿的 酸鹼值太大’會麟部分錄錄會形成錯合㈣重新雜。在這些 狀況下均無賴騎需雜狀異質，减分均自之乡成份透^ 導電金屬氧化物奈米粉末。 因此，如何更精確的控制摻雜比例及製作均勻之奈米級粉末，以 達到高品質、高緻密度之性質是祕職的問題。 有鑑於此’本發明遂針對上述先前技術之缺失，提出一種以低溫 共>儿澱法製作透明導電金屬氧化物粉末之方法，以有效克服上述之該 等問題。 【發明内容】 本發明之主要目的在提供一種以低溫共沉澱法製作透明導電金屬 氧化物粉末之方法，係可提升多成份透明導電金屬氧化物粉末的性 質，以製造出擁有良好性質的濺鍍靶材和透明導電氧化物薄膜。 為達上述之目的，本發明提供一種以低溫共沉澱法製作透明導電 201201928 金屬氧化物粉末之方法，包括下列步驟1先，將一第一金屬與及一 第二金屬分別加入溶劑中進行溶解，以分別形成一第一金屬離子溶液 及-第二金屬離子溶液；混合第—金屬離子溶液及第二金屬離子溶液 以形成-前驅溶液，並_之；_在低於机之低溫溫度下，加入 -沉殿劑於前驅溶液中’並調至—第—酸難，使前驅溶液析出部分 沉殿物，據此產生-第-沉澱溶液，並進行—第—次陳化；控制在低 於45°C之低溫溫度下，再次加入沉澱劑於第一沉殿溶液中，並調至一 第一I驗值’使則驅溶液析出全部沉澱物，據此產生一第二沉澱溶液， 並進行-第二次陳化；過渡第二沉澱溶液，以取得一濾餅；以去離子 • 水來水洗_並加以獅錄後，再重複過it、水洗及獅分散之處 理程序’直至細中之陰離子的含量低於—允許值為止；對濾餅予以 乾燥處理’崎到-魏澱複合齡末；及將共職複合物粉末置入 一高溫爐進行煆燒處理，以獲得透明導電金屬氧化物粉末。 本發明除了可在共沉澱期間將合成及細化一併完成，同時也可精 確地控制粉末成份組成及粉末成份分佈均勻性，提高製程中所獲得的 透明導電氧化物粉末性質，也提高了後續以此粉末製作的透明導電氧 化物靶材及薄膜材料的性質。 底下藉由具體實施例詳加說明，當更容易瞭解本發明之目的、技 • 術内容、特點及其所達成之功效。 【實施方式】 如第1圖所示，首先如步驟S10所示，先將一第一金屬與及一第 二金屬分別加入一溶劑中進行溶解，其中溶劑係為硝酸或鹽酸之強酸 溶劑或者係為水、硝酸水溶液或鹽酸水溶液之水溶液溶劑，以分別形 成一第一金屬離子溶液及一第二金屬離子溶液，其中第一金屬與及第 二金屬係選自金屬銦、金屬鋅、金屬錫或金屬鹽類化合物，其中金屬 鹽類化合物係為硝酸銦、硝酸鋅、硝酸錫、硝酸鋁、氣化錮、氯化鋅、 氣化銘或氣化錫，且第一金屬及第一金屬之材料為相異者。再如步驟 201201928 S12所示，依所需比例充分混合第一金屬離子溶液及第二金屬離子溶 液後’以形絲定毅比例城分均自之—前驅雜，再洲餅機 將前驅溶賴拌舶。如步驟S14所示，㈣在低於45χ：之低溫溫度 下’可在麟前驅溶液時’快速地加人—職^於魏溶液中進行沉 殿反應，其中沉澱劑係為氫氧化錄、氫氧化鈉或氫氧化卸，並調至一 第-酸驗值（pH值），其中最適當的第一酸驗值範圍係為〇至4·5之 間，使前驅溶液難如额、g)频或複氧錄料分職物，據此 產生-第-臟溶液，並進行-第—次陳化，其中最佳第—次陳化時 間係為3至24小時。接續’如步驟S16所示，控制在低於做之低 溫溫度下’再:欠加人麟麟[沉澱驗巾進行職反應，並調至 -第-酸驗值（pH值）’其巾最適當的第二酸驗值範圍料6 〇至9.5 之間’使前驅溶液析出全部沉澱物，據此產生一第二沉殿溶液，並進 行-第二次陳化’其中最佳第二次陳化時間係為6至72小時。 經由上述步驟S14及步驟S16在低溫溫度你⑽件下進行兩階 段共沉澱與陳化過程’能使酸驗中和的熱反應及沉澱溫度獲得控制， 且可以抑織化物的生錢Α氧化物的再轉，躺驗先前技術因 前驅溶液與驗性臟劑進行職反麟，巾和反應放熱速度太快，造 成沉澱溶液的溫度過高’如溫度大於5(rc，使部分齡的金屬離子會 與沉澱劑化合直獅成氧化物，或是最終沉_ pH值太大，而使部 分氫氧化物形成錯合物而重新溶解，因而無法獲得所需摻雜特定成分 且成分均勻之粉末的問題。再如步驟S18所示，以離心過濾或壓力過 濾等過濾方式來過濾、第二;職溶液，以取得祕。如步驟S2〇所示， 以去離子水來水洗鑛，並加卩麟分織，再重複猶、水洗及擾 拌分散之處理程序，直至濾餅中之陰離子的含量低於一允許值為止， 其中滤餅中之陰離子的允許值係為含硕酸根離子之陰離子的含量低於 500 ppm，且含氣離子之陰離子的含量低於5〇〇 ppm。如步驟S22 所示，對濾餅予以喷霧乾燥或加熱乾燥等進行乾燥處理，且乾燥溫度 係小於80 °C，以得到一共沉殿複合物粉末。最後如步驟S24所示， 201201928 將共沉澱複合物粉末置人-高溫爐進行贱處理，其巾煅燒溫度範圍 為500 Ό至1200。(：之間，持溫時間為2_10小時，以獲得透明導電金 屬氧化物粉末，其巾透鱗電金魏化物粉末係為氧倾鋅、氧化嫁 鋅、氧化麵鋅或氧化銦錫。 、藉由上述製作步驟，本發明具有如下之優點：（1)設備簡單、設備 成本低廉、程序㈣、可大量生產、沉澱躺可將合成和細化一道完 成。（2)可精雜制各成份的含量，誤差範圍小於Q 5% ^⑶在沉搬過 程中，可以透過控制沉澱條件及沉澱物的暇燒，來㈣所得粉末的純 度、顆粒大小、分散性和她成，煅燒溫度低，慨穩定且重現性 好0 、此外，由於金屬鋅（Ζη)龜藏量豐富且廉價，同時無毒性，因此 被廣泛應用，在此’本發_金屬鋅作為主要成分金制第一金屬為 例，而最佳次要成分金屬係以金屬銘（Α|)、金屬鎵（Ga)'金屬銦⑽ 作為第二金屬’其最佳雜重量百分比為鎵：3〜5wt%，銘：， 銦2wt/〇 藉由上述第1圖之步驟流程，即可製作出多成份透明導 電金屬氧化物’如氧化銘鋅(a|umjnum_d〇ped Z丨nc 〇χ丨扣，WO)、氧化 鎵鋅(gallium-doped zinc oxide，GZ0)及氧化銦鋅(丨_m zinc _e IZO)的粉末^ ’ 如第2圖所示’本實施例將以奈米結晶性的氧化紹鋅粉末作為實 作範例其步驟如下.首先，如步驟326所示，先將以金屬鋅為第一 金屬溶解於俩水溶液中以形成金屬鋅離子溶液，再將摻雜金屬銘之 重量^分比為2wt% ’作純二金屬溶解於猶水雜巾鄉成金屬銘 離子;谷液如步驟S28所示，混合金屬辞離子溶液及金屬紹離子溶液 以配製濃度為G.25〜6M，域拌至形成澄清之前驅溶液^再如步驟 S30所不’蝴在低於蚊之低溫溫度的祕下，加人氫氧化納或氣 氧化钟之濃料_的沉澱劑，翻至第—酸祕為3，她（AH) 離子先沉澱，據此產生—第—職溶液，再進行第—次陳化，其時間 為6小時，使第—沉澱溶射的_金屬離子辦反應產生氫氧化銘 201201928 :殿。待陳化為6小時後，可使氫氧化物完全沉;殿，接下來如步 S3=所示，_在慨做之低溫溫度的條件下，再度添加入氣氧化 j氫氧化鉀之職劑於第-職溶液中，並調至第二值 =10，此產生一第二沉澱溶液，使辞（Zn+2)離子完全沉殿， 二第二次陳化’其時間為12小時。其中，選用此第二酸驗值範圍是因 為沉_之氫氧根離子_量未達當量值時鱗致職不完全， 前驅沉職的成份關發生偏折，但過高的氫氧根軒用量時，因為 t為兩性元素，會使職物重新溶解產生錯合物，導致最後粉末的成 分比例無法有效的控制，故在以〇H.作為沉殿劑的反應中沉殿溶液之 第二酸驗值馳制在-個適當的範圍，因此，在此第二酸驗範圍最 佳沉澱點約在值為8.1Q之間，才能使溶射的鋅離子均勻反應產 生氫氧化鋅職。再如步驟S34所示，以離心過渡或壓力過滤等過滤 方式來過濾第二沉澱溶液’以取得-贿。再如步驟S36所示，以^ 子水來水洗賴’並加_拌分紐，再重複職、水洗及授拌分散 之處理程序，直至滤餅中之陰離子的含量低於—允許值為止，其中渡 餅中之陰離子的允許值係為含硝酸根離子之陰離子的含量低於5〇〇 ppm，且含氣離子之陰離子的含量低於5〇〇 口口⑴。如步驟s38所示， 對溏餅予以喷霧乾燥或加熱乾燥等進行乾燥處理，且乾燥溫度係小於 80。〇’以制含氫氧化雜鋅之共職複合物粉末。最後如步驟S4〇 所示，將共沉澱複合物粉末置入一高溫爐進行煆燒處理，其中煆燒溫 度為600°C ’持溫時間為2小時，以獲得透明導電金屬氧化銘鋅粉末。 最後以相關材料性質檢測設備檢視粉末特性，如χ光繞射分析儀 (X-ray difftaction，XRD)及電子顯微鏡（Sca_g 日ectr〇n201201928 VI. Description of the Invention: [Technical Field] The present invention relates to a method for transparent conductive metal oxide powder, and more particularly to a method for producing a more precise control doping ratio and improving electrical conductivity by low temperature coprecipitation. Transparent conductive metal oxide powder. [Prior Art] At present, a transparent conductive oxide (TCO) film is a film which has high conductivity, high transmittance to visible light, and high reflectance to infrared light, and thus is widely used. A transparent conductive electrode material for a transparent electrode flat panel display device of a solar cell, and an electronic, optical and optoelectronic device such as a photodetector, a transparent heating element, an antistatic film, an electromagnetic wave protective film, etc., especially a liquid crystal display (LCD) . In order to obtain the transparency of the visible light region, the TCO material usually adopts a semiconductor metal oxide having a gap width larger than the visible light energy, and doping impurities in the semiconductor metal oxide material to increase conductivity 'for example: adding a small amount of tin to the indium oxide Indium tin oxide film (ITO), or oxidized zinc film (AZ0) doped with aluminum in zinc oxide; and the conductivity of TC〇 film is affected by the process method and process conditions, and the proportion of doped metal impurities is more It is a key factor affecting the electrical conductivity of TCO films. At present, the main method for preparing TC ruthenium film in the industry is the money plating method, and the sputtering method is to use the TC0 target prepared by TCO powder, and the method of vacuum magnetron sputtering is used for the composition of the raw material due to the target material. Factors such as the diameter distribution make the uniformity of the mixing of different oxides have their limits, and the oxide may contain impurities, thus affecting the conductivity, light transmittance and adhesion to the substrate. Therefore, the sputtering target used in the preparation of the TCO transparent conductive film and the multi-component metal TCO powder required for the preparation of the sputtering target are also receiving more and more attention. However, the current manufacturing method of the multi-component metal TC0 powder is mainly based on a solid-state reaction method in which a plurality of metal oxide powders are mixed and controlled, and a chemical method in which a ratio of a desired component is prepared in a different manner. However, the oxide powder prepared by the solid state reaction method may be caused by excessive particle size, uneven mixing, and impurity contamination caused by grinding, etc., and 201201928 is prepared to prepare an oxide target and splash it into a smoldering furnace. The oxide powder is deteriorated in nature, and the properties of the film plated by plating are deteriorated. The method of mass production potential". Material, the test is the most industrial raw material, in _: solution =, high temperature _ system is more == Fajier rubbing multi-component transparent conductive = two research team personnel Wei Qiansuo solution mine _ riding agent, such as Ammonia water oxidized sodium, ^ Lin 'ruo and anti-reputation test, will cause the temperature of the working solution to rise two, when the seam temperature is greater than 5 (rc, w sub-component metal ions, such as reciprocal ion t and Shen Lai JL lions are recorded as oxygen oxides; in addition, if the pH value of the final sinking hall is too large, the recordings of the Huilin section will form a mismatch (4) and re-mix. Under these conditions, the rogue rides require heterogeneous heterogeneity, and the scores are reduced. The self-contained ingredient is a conductive metal oxide nano powder. Therefore, how to control the doping ratio more accurately and produce a uniform nano-sized powder to achieve high quality and high density is a problem of secret service. In view of the fact that the present invention has been directed to the above-mentioned prior art, a method for producing a transparent conductive metal oxide powder by a low temperature method has been proposed to effectively overcome the above problems. [Summary of the Invention] The purpose is to provide a kind of low temperature co-precipitation The method for preparing a transparent conductive metal oxide powder by a layer method can improve the properties of the multi-component transparent conductive metal oxide powder to produce a sputtering target and a transparent conductive oxide film having good properties. The invention provides a method for preparing transparent conductive 201201928 metal oxide powder by low temperature coprecipitation method, comprising the following steps: first, adding a first metal and a second metal to a solvent to dissolve, respectively, to form a first a metal ion solution and a second metal ion solution; mixing the first metal ion solution and the second metal ion solution to form a precursor solution, and _; at a lower temperature than the machine, adding - sinking agent to the precursor In the solution, it is adjusted to - the first acid is difficult, so that the precursor solution precipitates part of the sinking material, thereby generating a -precipitating solution, and performing - first aging; controlling at a low temperature lower than 45 ° C , adding the precipitant to the first sinking solution again, and adjusting to a first I value, so that the solution is precipitated to precipitate all the precipitate, thereby generating a second precipitation solution, and Line - second aging; transition the second precipitation solution to obtain a filter cake; wash with deionized water • water and lion record, then repeat the it, wash and lion dispersion process 'until fine The content of the anion is lower than the allowable value; the filter cake is dried and treated; the Saki-Wei-Tuan compound age is finished; and the co-work compound powder is placed in a high-temperature furnace for calcination treatment to obtain transparent conductive metal oxidation. In addition to the synthesis and refinement during coprecipitation, the present invention can also accurately control the composition of the powder and the uniformity of distribution of the powder composition, and improve the properties of the transparent conductive oxide powder obtained in the process. The properties of the transparent conductive oxide target and the film material which are subsequently made of the powder are improved. The details of the present invention, the technical contents, the features and the efficacy. [Embodiment] As shown in Fig. 1, first, as shown in step S10, a first metal and a second metal are separately added to a solvent for dissolution, wherein the solvent is a strong acid solvent or a system of nitric acid or hydrochloric acid. An aqueous solution of water, an aqueous solution of nitric acid or an aqueous solution of hydrochloric acid to form a first metal ion solution and a second metal ion solution, wherein the first metal and the second metal are selected from the group consisting of metal indium, metallic zinc, metallic tin or a metal salt compound, wherein the metal salt compound is indium nitrate, zinc nitrate, tin nitrate, aluminum nitrate, bismuth gasification, zinc chloride, gasification or gasification tin, and the first metal and the first metal material For the difference. Then, as shown in step 201201928 S12, after the first metal ion solution and the second metal ion solution are sufficiently mixed according to the required ratio, the ratio of the shape of the wire is determined by the pre-existing impurity, and the pre-disintegration of the precursor cake is dissolved. Mix the ship. As shown in step S14, (4) at a low temperature of less than 45 χ: 'can be used in the lining precursor solution' to quickly add people---the solution in the Wei solution, the precipitant is hydrogen hydroxide, hydrogen Discharge from sodium oxide or hydroxide and adjust to a pH-value (pH). The most appropriate first acid range is between 〇 and 4.5, making the precursor solution difficult, g) The frequency or re-oxygen recording material is divided into two parts, thereby generating a -first-dirty solution, and performing a -first aging, wherein the optimum first aging time is 3 to 24 hours. Continued 'as shown in step S16, the control is lower than the temperature at which it is made. 'Re: Adding people Lin Lin [precipitation test towel for occupational reaction, and adjusting to - acid-test value (pH)" Appropriate second acid test range from 6 〇 to 9.5 'pre-precipitate solution to precipitate all precipitates, according to which a second sinking solution is produced, and - second aging is carried out 'the best second Chen The time is from 6 to 72 hours. Through the above steps S14 and S16, you can carry out two-stage co-precipitation and aging process under low temperature (10) pieces, which can control the thermal reaction and precipitation temperature of the acid neutralization, and can suppress the granules of the granules. The re-transfer, lying before the previous technology due to the precursor solution and the test agent to carry on the anti-colon, the towel and the reaction exotherm too fast, causing the temperature of the precipitation solution to be too high 'such as temperature greater than 5 (rc, the metal ions of some age) Will combine with the precipitant to form a direct lion oxide, or the final sinking_pH value is too large, so that some of the hydroxide forms a complex and redissolves, thus failing to obtain the desired doping of specific components and uniform composition of the powder The problem is as shown in step S18, filtering by means of centrifugal filtration or pressure filtration, and the second; job solution to obtain the secret. As shown in step S2, washing the water with deionized water, and adding the unicorn Weaving, repeating the process of juicing, washing and dispersing until the content of anions in the filter cake is lower than a permissible value, wherein the allowable value of the anion in the filter cake is an anion containing a sour ion The content is less than 500 ppm, and the content of the anion containing gas ions is less than 5 〇〇 ppm. As shown in step S22, the filter cake is subjected to spray drying or heat drying to dry, and the drying temperature is less than 80 ° C. To obtain a total of the sinking complex powder. Finally, as shown in step S24, 201201928, the coprecipitated composite powder is placed in a high-temperature furnace for hydrazine treatment, and the calcination temperature of the towel ranges from 500 1200 to 1200. The heating time is 2-10 hours to obtain a transparent conductive metal oxide powder, and the towel-transparent electric gold-Wide powder is oxydop zinc, oxidized zinc, oxidized zinc or indium tin oxide. The invention has the following advantages: (1) simple equipment, low equipment cost, program (4), mass production, and sedimentation can be completed by synthesis and refinement. (2) content of each component of the miscellaneous miscellaneous, the error range is less than Q 5% ^(3) In the process of sinking, it can control the precipitation conditions and the smoldering of the precipitate. (4) The purity, particle size, dispersibility and purity of the obtained powder, low calcination temperature, stable and reproducible In addition, since the metal zinc (Ζη) is rich in minerals, inexpensive, and non-toxic, it is widely used. In this case, the first metal of gold, which is the main component of the metal, is the best. The composition of the metal is based on metal (Α|), metal gallium (Ga) 'metal indium (10) as the second metal', the optimum impurity percentage is gallium: 3~5wt%, Ming:, indium 2wt / 〇 by the above In the step of the figure, a multi-component transparent conductive metal oxide such as oxidized zinc (a|umjnum_d〇ped Z丨nc ,, WO), gallium-doped zinc oxide (GZ0) can be produced. And powder of indium zinc oxide (丨_m zinc _e IZO) ^' as shown in Fig. 2 'This embodiment will take nanocrystalline crystalline zinc oxide powder as an example of implementation. The steps are as follows. First, as steps As shown in 326, the first metal is dissolved in the two aqueous solutions to form a metal zinc ion solution, and then the weight ratio of the doping metal is 2 wt%, and the pure metal is dissolved in the water. Metal-forming ions; as shown in step S28, the mixed metal ionic solution and metal The sub-solution is prepared at a concentration of G.25~6M, and the domain is mixed until a clarification solution is formed. Then, as in step S30, it is not under the secret of the low temperature of the mosquito, and the sodium hydroxide or gas oxidation clock is added. Concentrate_precipitant, turn to the first - acid secret is 3, her (AH) ions are precipitated first, according to which - the first - working solution, and then the first - aging, the time is 6 hours, so that - Precipitation-solubilized _ metal ions do react to produce oxidized water 201201928: Temple. After 6 hours of aging, the hydroxide can be completely sunk; the temple, as shown in step S3 =, _ under the condition of low temperature, add the gas to the oxidation of potassium hydroxide In the first-position solution, and adjusted to the second value = 10, this produces a second precipitation solution, so that the (Zn + 2) ions completely sink the temple, and the second time aging - the time is 12 hours. Among them, the second acid test range is selected because the sinker's hydroxide ion _ is less than the equivalent value, the scale is not complete, the predecessor's component is deflected, but the too high hydroxide When Xu is used, because t is an amphoteric element, it will re-dissolve the complex to produce a complex compound, which will result in the inability to effectively control the proportion of the final powder. Therefore, in the reaction of 沉H. The diacid test is performed in a suitable range. Therefore, in this second acid test range, the optimum precipitation point is between about 8.1Q, so that the dissolved zinc ions can be uniformly reacted to produce zinc hydroxide. Further, as shown in step S34, the second precipitation solution is filtered by means of filtration such as centrifugation or pressure filtration to obtain a bribe. Further, as shown in step S36, the water is washed with water, and the process is repeated until the content of the anion in the filter cake is lower than the allowable value. The allowable value of the anion in the cake is that the content of the anion containing nitrate ions is less than 5 〇〇 ppm, and the content of the anion containing gas ions is less than 5 〇〇 mouth (1). As shown in step s38, the crepe cake is subjected to a drying treatment by spray drying or heat drying, and the drying temperature is less than 80. 〇' to produce a composite powder containing a mixed zinc hydroxide. Finally, as shown in step S4, the coprecipitated composite powder was placed in a high temperature furnace for calcination treatment, wherein the calcination temperature was 600 ° C. The holding temperature was 2 hours to obtain a transparent conductive metal oxide zinc powder. Finally, the powder properties such as X-ray difftaction (XRD) and electron microscopy (Sca_g day ectr〇n) are examined with relevant material property testing equipment.
Microscope，SEM) ’請同時參閱第3圖及第4圖’分別為χ光繞射分 析圖譜與電子顯微鏡所分析的結果，證明使用本發明製作方式可生產 具有奈米級結晶性的透明導電金屬氧化鋁鋅粉末。而利用此法製備之 AZ0粉末經過研磨、配方、造粒、成型、αρ強化、脫蠟及高溫燒結 等程序，可獲得密度為5.575g/cm3、敏密度為99.575%(AZO之理論 201201928 密度設為5.60 g/cm3)及電阻係數為5們㈣训之奶_乾材， 而，用此乾進行即磁控賤鐘，可得電阻係數約3 〇*1〇%咖且可 光平均穿透率大於80%之AZO透明導電薄膜。 由上述可得知，本發明除了可在共沉助間將合成及細化一併 f，同時也可精確地控制粉末成份組成及粉末成份分佈均勾性 獲得的透明導電氧化物粉末性質，當然也相對提高了後續以 末製作為-賴狀透轉電氧⑽純及薄赌料的性質。 發明上^述者僅為本㈣之較佳實闕而已，麟用來限定本 ^圍。故即凡依本發明申請範圍所述之特徵及精神所為之 均等變化或修飾，均應包括於本㈣之巾請專利範圍内。 【圖式簡單說明】 第1圖為本發明之步驟流程圖。 ^ 製作透明導電金屬氧化鋁鋅粉末之步驟流程圖。 第3圓為f據本發衝製得之透料電金屬氧她鋅粉末之X光繞射 示意圖。 第4圖為根據本發明所製得之透金屬氧化轉 子 鏡照相圖。 【主要元件符號說明】Microscope, SEM) 'Please refer to Fig. 3 and Fig. 4' respectively for the results of the analysis of the diffraction profile and electron microscope, which proves that the transparent conductive metal with nanometer crystallinity can be produced by the method of the invention. Alumina zinc powder. The AZ0 powder prepared by this method can obtain a density of 5.575g/cm3 and a density of 99.575% after grinding, formulation, granulation, molding, αρ strengthening, dewaxing and high-temperature sintering, etc. (AZO theory 201201928 density setting) It is 5.60 g/cm3) and the resistivity is 5 (four) training milk _ dry material, and, with this dry, that is, the magnetic control 贱 clock, can obtain a resistivity of about 3 〇 * 1 〇% coffee and light average penetration AZO transparent conductive film with a rate greater than 80%. From the above, it can be known that the present invention can synthesize and refine the f together in the co-sinking, and at the same time, can precisely control the properties of the transparent conductive oxide powder obtained by powder composition and powder composition distribution, of course. It is also relatively improved in the subsequent production of the oxidized oxygen (10) pure and thin smear. The invention is only a better example of this (4), and Lin is used to define this. Therefore, any changes or modifications to the features and spirits described in the scope of the present application should be included in the scope of the patent application of this (4). BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a flow chart showing the steps of the present invention. ^ Flow chart of the steps for preparing transparent conductive metal aluminum oxide zinc powder. The third circle is a schematic diagram of the X-ray diffraction of the transparent metal oxide zinc powder according to the present invention. Figure 4 is a photomicrograph of a metal oxidized rotor made in accordance with the present invention. [Main component symbol description]