1229141 經濟部智慧財產局員工消費合作社印製 A7 B7 五、發明說明（丨） < [技術領域] 本發明係關於一種濺鍍時之特性經時變化少的ITO濺 鍍革巴。 [背景技術] ITO (銦-錫之複合氧化物）膜係廣泛地被使用在以 液晶顯示器爲中心之顯示裝置的透明電極（膜）。形成該 ITO膜之方法方面，普通以真空蒸鍍法或濺鑛法等之一般 所謂的物理蒸鍍法之做法來進行。 特別地’磁控濺鍍法相較於不形成磁場之通常的濺鍍 法’由於膜之堆積速度（成膜速度）快，乃多採用作爲形 成ITO膜的方法。 以濺鍍法所進行之薄膜的形成，係讓Ar離子等之正 離子以物理方式衝撞設置於陰極之靶，以該衝撞能量釋放 出構成靶的材料，而在位於對面之陽極側之基板上積層出 與靶材料大致相同組成的膜。 、 採濺鏟法之被覆法係具有：可藉由調節處理時間或供 給電力等’以安定的成膜速度來形成從數nm之薄膜至數 十//m之厚膜之特徵。 如上述，ITO之濺鍍靶廣泛地使用在工業上之使用DC 電源之磁控濺鏟，而近年來開發出以DC電源來檢測電弧 放電的裝置，來一邊監視電弧放電一邊進行濺鑛。 該情況下，所檢測之電弧所釋放的能量大且持續時間 長，而稱爲強電弧(hard arc)。 3 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） --------------------訂---------線 (請先閱讀背面之注意事項再填寫本頁) 1229141 A7 B7 五、發明說明（/) (請先閱讀背面之注意事項再填寫本頁) 但是，在實際之濺鍰中，會發生許多較前述強電弧爲 小規模的電弧（一般稱爲「微電弧」）’並已知其會對膜 的品質造成大的影響。因此，在最近之裝置之高精細化製 程中，除了監視前述強電弧以外，監視微電弧並抑制其產 生乃爲重要的事。 又，一般使用濺鍍靶來形成ITO膜的情況下，除了上 述微電弧之產生外，尙有在濺鍍操作中’於絶腐蝕面產生 瘤塊（nodule，黑色之銦的低級氧化物）之問題。 瘤塊係隨著濺鍍累積電量之增加而急速地增加，其爲 招致成膜速度降低的一個原因。由於成膜速度變慢則理所 當然生產性降低，此時，係提高輸入濺鍍功率，防止成膜 速度之降低。然而，大幅地變更濺鍍條件（輸入濺鍍功率 )，由於恐怕會使薄膜性質產生變化，乃非所望。 而且，爲了提昇濺鍍ITO膜的性質，防止微電弧或瘤 塊之產生則特別地重要。 ‘ 一般而言，ITO濺鍍靶係使用將氧化錫粉末與氧化銦 粉末混合成既定之比例的粉末加以燒結來製造的方法。 上述所製造的靶係多使用含有1〇重量％之Sn〇2者。 經濟部智慧財產局員工消費合作社印制衣 其主要以提昇透明導電膜之導電率（降低比電阻）爲目的 〇 如此一來，ITO濺鍍靶不但有異常放電或瘤塊之產生 ，而且在瘤塊過度地增大的階段，一旦停止濺鍍操作，變 得必須有所謂洗淨靶的操作，從而成爲生產佳降低之原因 ，此爲目前的情況。 4 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） 1229141 A7 B7 五、發明說明（彡） 又，在上述習知ITO濺鍍靶中，難以顯著地降低濺鍍 時所產生之微電弧或形成於靶表面的瘤塊，不能達成根本 的解決。 另外，於ITO濺鍍膜之形成時，在靶密度低的情況下 、靶的粗糙度(Ra)大的情況下、或在靶之粒徑粗大的情況 下，特別會在ITO靶之腐蝕面上產生許多瘤塊（突起物） ，此將導致不規則之濺鎪，而造成異常放電或形成團狀（ 變成塊狀）之皮膜，成爲顯示裝置不良的原因，此爲問題 所在。 ； [發明之說明] 本發明之目的係提供一種ITO膜形成用濺鑛靶，不但 能抑制在濺鍍時所產生之微電弧，且可降低於靶表面所產 生之瘤塊，在整個靶壽命期間以安定、一定條件來進行濺 鍍操作。 爲了解決上述問題點之技術上的手段係調製ITO靶中 之Sn02組成於所限卑之範圍，藉以得到適於，ITO透明導 電膜等之形成的濺鍍靶。 基於上述見解，本發明係提供 一種ITO濺鍍靶，其特徵在於，靶中所含有之Sn02 組成在8·80〜9·40重量％之範圍。 一種ΙΤΟ濺鍍靶，其特徵在於，靶中所含有之Sn02 組成在8·90〜9·30重量％之範圍。 一種ΙΤΟ濺鑛靶，其特徵在於，靶中所含有之Sn02 5 ' 本紙張尺度適用中國國家標準(CNS)A4規格（210 X 297公釐） (請先閱讀背面之注意事項再填寫本頁) --------訂---------線· 經濟部智慧財產局員工消費合作社印製 1229141 A7 ____Β7 五、發明說明（k ) 組成在9.00〜9.20重量％之範圍。 上述1〜3所述之任一ITO濺鍍靶，其具備7.00g/cm3 以上之密度。 (請先閱讀背面之注意事項再填寫本頁) 上述1〜4所述之任一 ITO濺鍍靶，其靶之中心線平均 粗糙度Ra爲0.5//m以下。 上述1〜5所述之任一ITO濺鍍靶，其靶之平均粒徑未 滿 4 // m。 圖式之簡單說明 圖1係表示於ITO靶中讓Sn02在8.95〜10·83 (重量 °/〇 )變化的情況下，累積電量40WHr/cm2之微電弧產生次 數之圖。 圖2係表示於ITO靶中讓Sn02在8.95〜10·83 (重量 % )變化的情況下，累積電量80WHrVcm2之微電弧產生次 數之圖。 圖3係表示於ITO靶中讓Sn02在8.95〜1〇·83 (重量 °/〇 )變化的情況下，累積電量120WHr/cm2之微電弧產生 次數之圖。 ‘ 經濟部智慧財產局員工消費合作社印製 圖4係表示於ITO靶中讓Sn02在8·95〜1〇·83 (重量 % )變化的情況下，累積電量160WHr/cm2之微電弧產生 次數之圖。 圖5係表示於ITO靶中讓811〇2在8·95〜1〇·83 (重量 % )變化的情況下，累積電量40WHr7cm2之瘤塊被覆率之 圖。 6 , 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） !229141 A7 B7 五、發明說明（<) 圖6係表示於ITO靶中讓Sn02在8.95〜10.83 (重量 % )變化的情況下，累積電量80WHr/cm2之瘤塊被覆率之 圖。 圖7係表示於ITO靶中讓811〇2在8·95〜10.83 (重量 % )變化的情況下，累積電量12〇WHr/cm2之瘤塊被覆率 之圖。 圖8係表示於ΠΌ靶中讓811〇2在8.95〜10.S3 (重量 % )變化的情況下，累積電量16〇WHr/cm2之瘤塊被覆率 之圖。 圖9係表示於ITO靶中讓Sn02在8.95〜10.83 (重量 % )變化的情況下，累積電量80 WHr/cm2、120 WHr/cm2 、160 WHr/cm2之輸入濺鍍電功率密度(W/cm2)之圖。 [發明之實施形態] 在製造本發明之ITO濺鏟靶中，係使用例如平均粒徑 爲l//m以下之氧化銦粉末及大致相同粒徑之氧化錫粉末 作爲原料，於靶中成_既定之811〇2含有量來均勻地混合， 並於其中加入成形用黏結劑後充塡於模具中。 然後，對作爲充塡於該模具中之前述原料的混合粉末 ，以冷壓來施加50〜200MPa之壓力而得加壓成形體。 其次，將如此所得之成形體於lOOkPa (絕對壓）之純 氧環境氣氛下，以1550〜165(TC之溫度燒結3〜7小時，製 造ITO濺鐽靶燒結體。 於本發明中，靶中所含有之Sn02的組成爲8·80〜9.40 7 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） (請先閱讀背面之注意事項再填寫本頁) --------訂---------線 經濟部智慧財產局員Η消費合作社印製 1229141 A7 B7 經濟部智慧財產局員工消費合作社印製 五、發明說明（V) 重量％之範圍。以8.90〜9.30重量％爲佳，而更好以在 9.00〜9.20重量％之範圍爲佳。 上述Sn02的組成範圍可由調節原料氧化錫粉末之混合 比例與燒結溫度等之燒結條件而容易地達成。 以上述方式將ITO濺鍍靶中的Sn02組成調整於一定 範圍，可產生降低濺鑛時在靶表面所產生之微電弧與瘤塊 的效果。 過度使用靶的情況下，由於前述之瘤塊等的產生，在 同一濺鍍功率下，發現成膜速度較使用開始時有降低的現 象，於該情況下將輸入功率提高相當於速率降低之部分來 保持成膜速度一定是必要的。 然而，改變輸入濺鍍功率意味著實質上改變濺鍍條件 ，一旦該變化率大，則產生對於薄膜特性亦造成影響的問 題。 .； 而且，理所當然，輸入濺鎪功率固定，且變化率低者 ，對於靶的機能而言爲優異的，爲重要的靶評估項目之一 〇 即，在整個濺鍍操作中，爲了良好地維持ITO膜特性 ，必須讓該輸入濺鍍功率密度的變化小。 依照上述，本發明係可顯著地降低該等輸入濺鑛功率 密度之變化，而可於整個靶壽命中，以安定、大致固定之 條件下，進行濺鍍操作。 ； 於本發明中，更希望ITO濺鍍靶之密度爲7.00g/ cm3 以上、靶中心之中心線平均粗糙度Ra爲0.5/zm以下、靶 8 --------------------訂---------線 (請先閱讀背面之注意事項再填寫本頁) 尺度適用中國國家標準（CNS)A4規格(210 X 297公釐） 經濟部智慧財產局員工消費合作社印製 1229141 A7 B7 五、發明說明（飞） 之平均結晶粒徑未滿4 A m。 藉此，可更有效果地降低微電弧之產生與瘤塊，又可 在更長之時間中讓輸入濺鍍功率密度安定。 實施例與比較例 其次，就本發明之實施例來說明。還有，本實施例終 究爲一範例，本發明並不受限於該範例。即，在本發明之 技術觀念之範圍內，實施例以外之態樣或變形均包含在內 (實施例1〜5及比較例1〜6) 使用平均粒徑l//m以下之氧化銦粉末與同粒徑之氧 化錫粉末作爲ITO濺鍍靶之原材料，並以既定之比例均勻 地混合氧化錫粉末。 其次，將上述氧化銦-氧化錫混合粉末均勻地充塡於 模具中，以冷油壓壓力機施加80MPa之壓力而得加壓成形 體。 . ‘ 將如此所得之成形體在lOOkPa (絕對壓）之純氧環境 氣氛下，以1640°C之溫度來燒結4小時。將如此所得之燒 結體表面，以平面硏磨盤，使用400號鑽石硏磨粒來硏磨 ，更以鑽石切割器切斷側面，作爲ITO靶素材。 於上述靶製程中，藉由讓氧化錫之混合比例爲 9·00〜10·9〇重量％，而得到靶中之Sn02組成8.95〜10.83重 量％ 、密度7.08〜7·12 cm3、中心線平均粗糙度Ra 9 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） --------------------訂----------線 (請先閱讀背面之注意事項再填寫本頁) 1229141 A7 B7 五、發明說明（9 ) 0.30〜0.39//m、平均結晶粒徑3·15〜3.74/zm之ITO濺鍍靶 〇 靶中之Sn02組成在本發明之範圍內者以賣施例1〜5、 範圍外者以比較例1〜3示於表1。 然後，使用以上述實施例1〜5及比較例1〜3 (—部份 還有比較例4〜6)所得之濺鍍靶來濺鍍，對於每個靶中所 含有之Sn02組成，測定在各濺鑛累積電量中之微電弧發生 次數（次）、瘤塊覆蓋率（％)、輸入濺鎪功率密度（W/ cm2)。測定結果個別示於表2〜4。 還有，判定微電弧之條件係在檢測電壓100V以上、 釋放能量（電弧放電發生時之濺鍰電壓X濺虚電流X發生 時間）爲10mJ以下的情況，又瘤塊之覆蓋率，係以腐蝕 面積除以所產生之瘤塊面積的値。還有，僅瘤塊之覆蓋率 ，擴大所對應之Sn02組成範圍的幅度表示到比較例4〜6。 又，於後述之對應圖中，係更進一步擴大Sn02組成範圍之 幅度來顯示。 同樣地，該結果韦於表2〜表4。又，對應於表2〜表4 之圖則示於圖1〜圖9。 濺鏟條件係依照如下。 ‘ 靶尺寸 ：127X508 X 6.35mm 濺鍍氣體 ：氬氣+氧氣 濺鍍氣壓 ：0.5Pa1229141 Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs A7 B7 V. Description of the Invention (丨) [Technical Field] The present invention relates to an ITO sputtered leather with little change in characteristics over time. [Background Art] ITO (Indium-Tin Composite Oxide) films are widely used as transparent electrodes (films) in display devices centered on liquid crystal displays. The method for forming the ITO film is generally performed by a so-called physical vapor deposition method such as a vacuum vapor deposition method or a sputtering method. In particular, the 'magnetron sputtering method' is a method for forming an ITO film because a film deposition rate (film formation speed) is faster than a normal sputtering method in which a magnetic field is not formed. The formation of the thin film by the sputtering method is to allow positive ions such as Ar ions to physically collide with the target provided on the cathode, release the material constituting the target with the impact energy, and place the substrate on the opposite anode side. A film having approximately the same composition as the target material is laminated. The coating method of the shovel shovel method has the feature that the film can be formed from a thickness of several nm to a thickness of several tens of meters per meter at a stable film formation speed by adjusting processing time or power supply. As described above, the sputtering target of ITO is widely used in the industry, and a magnetron sputtering shovel using a DC power supply is developed. In recent years, a device for detecting an arc discharge using a DC power supply has been developed to perform arc sputtering while monitoring the arc discharge. In this case, the energy released by the detected arc is large and has a long duration, and is called a hard arc. 3 This paper size applies to China National Standard (CNS) A4 (210 X 297 mm) -------------------- Order --------- (Please read the precautions on the back before filling this page) 1229141 A7 B7 V. Description of the invention (/) (Please read the precautions on the back before filling this page) However, in actual splashing, many comparisons will occur. The aforementioned strong arc is a small-scale arc (commonly referred to as a "micro-arc") and is known to have a large effect on the quality of the film. Therefore, in recent high-definition processes of devices, it is important to monitor micro-arcs and suppress their generation in addition to the aforementioned strong arcs. In addition, in the case where a sputtering target is generally used to form an ITO film, in addition to the generation of the micro-arc described above, there are no "nodules (black lower oxides of indium) that are generated on the corrosion-resistant surface during the sputtering operation. problem. The nodule increases rapidly with the increase of the accumulated electric power of sputtering, which is one cause of the decrease in the film-forming speed. As the film-forming speed becomes slower, the productivity is naturally reduced. At this time, the input sputtering power is increased to prevent the film-forming speed from decreasing. However, drastically changing the sputtering conditions (input sputtering power) may cause changes in film properties, which is not desirable. Furthermore, in order to improve the properties of the sputtered ITO film, it is particularly important to prevent the generation of micro-arcs or nodules. ‘Generally, the ITO sputtering target is produced by mixing a powder of tin oxide and an powder of indium oxide into a predetermined ratio and sintering the powder. Most of the target systems produced above use 10% by weight of Sn02. The clothing printed by the employee's consumer cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs mainly aims to increase the conductivity (reduce specific resistance) of the transparent conductive film. As a result, the ITO sputtering target not only has abnormal discharges or tumor masses, but also In the stage where the mass is excessively increased, once the sputtering operation is stopped, it is necessary to have a so-called target cleaning operation, which causes a reduction in production. This is the current situation. 4 This paper size is in accordance with Chinese National Standard (CNS) A4 (210 X 297 mm) 1229141 A7 B7 V. Description of the invention (彡) In the conventional ITO sputtering target, it is difficult to significantly reduce the impact of sputtering. The resulting micro-arc or nodules formed on the target surface cannot reach a fundamental solution. In addition, when the ITO sputtering film is formed, when the target density is low, when the target roughness (Ra) is large, or when the target particle diameter is large, it is particularly on the corrosion surface of the ITO target. Many bumps (protrusions) are generated, which will cause irregular splashes, cause abnormal discharges or form lumps (become lumps), and become the cause of defective display devices. This is the problem. [Explanation of the invention] The object of the present invention is to provide an ITO sputtering target for ITO film formation, which can not only suppress the micro-arc generated during sputtering, but also reduce the nodules generated on the surface of the target over the entire target life. During the sputtering process, stable and certain conditions are performed. In order to solve the above-mentioned problems, the technical means is to modulate the composition of Sn02 in the ITO target to a limited range, thereby obtaining a sputtering target suitable for the formation of an ITO transparent conductive film. Based on the above findings, the present invention provides an ITO sputtering target, characterized in that the Sn02 composition contained in the target is in the range of 8.80 to 9.40% by weight. An ITO sputtering target is characterized in that the Sn02 composition contained in the target ranges from 8.90 to 9.30% by weight. An ITO sputtering target, characterized in that the Sn02 5 'contained in the target is in accordance with the Chinese National Standard (CNS) A4 specification (210 X 297 mm) (Please read the precautions on the back before filling this page) -------- Order --------- line · Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economy 1229141 A7 ____ Β7 V. Description of the invention (k) The composition ranges from 9.00 to 9.20% by weight. The ITO sputtering target according to any one of the above 1 to 3, has a density of 7.00 g / cm3 or more. (Please read the precautions on the back before filling out this page.) For any ITO sputtering target described in 1 to 4 above, the average centerline roughness Ra of the target is 0.5 // m or less. The ITO sputtering target of any one of the above 1 to 5 has an average particle diameter of the target less than 4 // m. Brief Description of the Drawings Figure 1 is a graph showing the number of micro-arc generation times of 40WHr / cm2 of accumulated power when Sn02 is changed in the ITO target from 8.95 to 10.83 (weight ° / 〇). Fig. 2 is a graph showing the number of micro-arc generation times with a cumulative electric power of 80 WHrVcm2 when Sn02 was changed in the ITO target from 8.95 to 10.83 (% by weight). Fig. 3 is a graph showing the number of micro-arc generations with a cumulative electric power of 120 WHr / cm2 when Sn02 was changed in an ITO target from 8.95 to 10.83 (weight ° / 〇). '' Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs, Figure 4 shows the number of micro-arc generation times of 160WHr / cm2 of accumulated electricity when Sn02 was changed from 8.95 to 10.83 (wt%) in the ITO target. Illustration. Fig. 5 is a graph showing the coverage rate of the nodules with a cumulative electric power of 40WHr7cm2 in the case where 81102 was changed from 8.95 to 10 · 83 (wt%) in the ITO target. 6. This paper size is in accordance with Chinese National Standard (CNS) A4 specification (210 X 297 mm)! 229141 A7 B7 V. Description of the invention (<) Figure 6 shows the ITO target with Sn02 at 8.95 ~ 10.83 (% by weight) ) The graph of the coverage rate of the tumor mass with the accumulated power of 80WHr / cm2. Fig. 7 is a graph showing the coverage rate of the nodules with a cumulative electric power of 120 WHr / cm2 when 81102 was changed from 8.95 to 10.83 (wt%) in the ITO target. Fig. 8 is a graph showing the coverage rate of the tumor mass with a cumulative electric power of 160 WHr / cm2 in the case where the 811 target is changed from 8.95 to 10.S3 (% by weight). Fig. 9 shows the input sputtering power density (W / cm2) of the accumulated power of 80 WHr / cm2, 120 WHr / cm2, and 160 WHr / cm2 when the Sn02 was changed from 8.95 to 10.83 (% by weight) in the ITO target. Figure. [Embodiments of the Invention] In manufacturing the ITO sputtering target of the present invention, for example, indium oxide powder having an average particle diameter of 1 // m or less and tin oxide powder having approximately the same particle diameter are used as raw materials to form _ The predetermined content of 81102 is uniformly mixed, and a molding adhesive is added thereto, and then filled in a mold. Then, a mixed powder as the aforementioned raw material charged in the mold is subjected to cold pressing to a pressure of 50 to 200 MPa to obtain a press-molded body. Next, the formed body thus obtained was sintered at a temperature of 1550 to 165 (TC for 3 to 7 hours in a 100 kPa (absolute pressure) pure oxygen atmosphere. In the present invention, the target The composition of the contained Sn02 is 8.80 ~ 9.40 7 This paper size is applicable to China National Standard (CNS) A4 (210 X 297 mm) (Please read the precautions on the back before filling this page) ----- --- Order --------- Printed by members of the Intellectual Property Bureau of the Ministry of Economics and Consumer Cooperatives 1229141 A7 B7 Printed by the Consumer Cooperatives of Employees of the Intellectual Property Bureau of the Ministry of Economic Affairs 5. The scope of the invention (V) weight%. 8.90 to 9.30% by weight is preferred, and more preferably in the range of 9.00 to 9.20% by weight. The composition range of the above Sn02 can be easily achieved by adjusting the sintering conditions such as the mixing ratio of the raw material tin oxide powder and the sintering temperature. The above method adjusts the composition of Sn02 in the ITO sputtering target to a certain range, which can reduce the micro-arc and nodules generated on the target surface during sputtering. In the case of excessive use of the target, due to the aforementioned nodules, etc. Generated at the same sputtering power It is found that the film formation speed is lower than that at the beginning of use. In this case, it is necessary to increase the input power equivalent to the rate reduction to maintain the film formation speed. However, changing the input sputtering power means a substantial change. Sputtering conditions, once the rate of change is large, will also affect the characteristics of the film. Also, as a matter of course, the input sputtering power is fixed and the rate of change is low, which is excellent for the performance of the target. One of the important target evaluation items is that in order to maintain the characteristics of the ITO film well during the entire sputtering operation, the input sputtering power density must be made small. According to the above, the present invention can significantly reduce these inputs. The change in the power density of the sputtering ore allows the sputtering operation to be performed under stable and approximately fixed conditions throughout the life of the target. In the present invention, it is more desirable that the density of the ITO sputtering target be more than 7.00 g / cm3, The centerline average roughness Ra of the center of the target is 0.5 / zm or less, target 8 -------------------- Order --------- line (please Read the notes on the back before filling Page) The scale applies to the Chinese National Standard (CNS) A4 specification (210 X 297 mm) Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs 1229141 A7 B7 V. Description of invention (flying) The average crystal grain size is less than 4 A m. Thereby, the generation of micro arcs and nodules can be reduced more effectively, and the input sputtering power density can be stabilized for a longer period of time. Examples and Comparative Examples Next, the examples of the present invention will be described. Also Yes, this embodiment is an example after all, and the present invention is not limited to this example. That is, within the scope of the technical concept of the present invention, all aspects and deformations other than the embodiment are included (Examples 1 to 5 And Comparative Examples 1 to 6) Indium oxide powder having an average particle diameter of 1 // m or less and tin oxide powder of the same particle diameter were used as raw materials of the ITO sputtering target, and the tin oxide powder was uniformly mixed at a predetermined ratio. Next, the above indium oxide-tin oxide mixed powder was uniformly filled in a mold, and a pressure of 80 MPa was applied with a cold hydraulic press to obtain a press-molded body. ‘The shaped body thus obtained was sintered at a temperature of 1640 ° C. for 4 hours under a pure oxygen atmosphere atmosphere of 100 kPa (absolute pressure). The surface of the sintered body thus obtained was honed with a flat honing disc using a 400-gauge diamond honing grain, and the side was cut with a diamond cutter as an ITO target material. In the above target manufacturing process, the Sn02 composition in the target was obtained by setting the mixing ratio of tin oxide to 9.00 to 10.90 wt%, with a density of 8.95 to 10.83 wt%, a density of 7.08 to 7.12 cm3, and a centerline average. Roughness Ra 9 This paper size is applicable to China National Standard (CNS) A4 (210 X 297 mm) -------------------- Order ------ ---- Line (Please read the precautions on the back before filling this page) 1229141 A7 B7 V. Description of the invention (9) 0.30 ~ 0.39 // m, average crystal grain size 3.15 ~ 3.74 / zm ITO sputtering Table 1 shows the composition of Sn02 in the target 0 within the range of the present invention as Examples 1 to 5, and those outside the range as Comparative Examples 1 to 3. Then, sputtering targets obtained using the above-mentioned Examples 1 to 5 and Comparative Examples 1 to 3 (partially and Comparative Examples 4 to 6) were used for sputtering, and the composition of Sn02 contained in each target was measured. The number of micro-arc occurrences (times), the nodule coverage (%), and the input sputtering power density (W / cm2) in the accumulated power of each ore splash. The measurement results are shown individually in Tables 2 to 4. In addition, the conditions for judging the micro-arc are the case where the detection voltage is 100V or more, and the energy release (spatter voltage X when the arc discharge occurs X spurious current X occurrence time) is 10mJ or less, and the coverage rate of the nodules is based on corrosion The area divided by the area of the tumor mass generated. In addition, only the coverage ratio of the tumor block, and the width of the corresponding Sn02 composition range were expanded to Comparative Examples 4 to 6. In the corresponding maps described later, the range of the Sn02 composition range is further expanded and displayed. Similarly, the results are better than those in Tables 2 to 4. The drawings corresponding to Tables 2 to 4 are shown in FIGS. 1 to 9. The shovel conditions are as follows. ‘Target size: 127X508 X 6.35mm Sputtering gas: Argon + oxygen Sputtering gas pressure: 0.5Pa
濺鑛氣體流量 ：300SCCM 濺鑛氣體中之氧濃度：1體積％ 10 (請先閱讀背面之注意事項再填寫本頁) --------訂---------線 經濟部智慧財產局員工消費合作社印製 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） 1229141 A7 B7 五、發明說明（（])Flow rate of ore splashing gas: 300SCCM Oxygen concentration in ore splashing gas: 1% by volume 10 (Please read the precautions on the back before filling this page) -------- Order --------- Line Printed by the Consumers' Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs, the paper size is applicable to China National Standard (CNS) A4 (210 X 297 mm) 1229141 A7 B7 V. Description of Invention (())
漏磁密度 ：0.1T 輸入濺鍍功率密度：以〇.5W/cm2開始濺鍍，保持一定 成膜速度來上升 濺鍍累積電量 ：〜160WHr/Cm2 表1Magnetic flux leakage density: 0.1T Input sputtering power density: Start sputtering at 0.5W / cm2, maintain a certain film-forming speed to increase Sputtered cumulative power: ~ 160WHr / Cm2 Table 1
Sn02組成 密度 表面粗糙度Ra 平均結晶粒徑 (雷量％ ) (g/cm2) (//m) (//m) 比較例1 10.83 7.11 0.39 3.53 比較例2 10.46 7.12 0.30 3.27 比較例3 9.97 7.10 0.32 3.74 實施例1 9.30 7.11 0.36 3.41 實施例2 9.19 7.12 0.35 3.15 實施例3 9.09 7.10 0.36 3.24 實施例4 9.02 7.09 0.33 3.68 實施例5 8.95 7.08 0.37 3.25 11 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） (請先閱讀背面之注意事項再填寫本頁) ----- 訂---------線· 經濟部智慧財產局員工消費合作社印製 1229141 A7 B7 五、發明說明) 表2 經濟部智慧財產局員工消費合作社印製 微電弧產生次數（次） Sn02組成 累積電量(WHr/cm2) (重量％ ) 40 80 120 160 比較例1 10.83 16次 104 538 3359 比較例2 10.46 13 60 404 1761 比較例3 9.97 2 24 163 804 實施例1 9.30 0 17 69 647 實施例2 9.19 2 17 32 144 實施例3 9.09 0 13 27、 121 實施例4 9.02 1 20 33 169 實施例5 8.95 1 22 52 473 12 (請先閱讀背面之注意事項再填寫本頁) ---------訂---------線. 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） 1229141 A7 B7 五、發明說明（\\) 表3 經濟部智慧財產局員工消費合作社印製 瘤塊被覆率（％) Sn02組成 累積電量(WHr/cm2) (雷量％ ) 40 80 120 160 比較例1 10.83 0.33% 3.42 23.71 78.37 比較例2 10.46 0.24 2.71 20.08 40.29 比較例3 9.97 0.06 1.21 4.58 18.77 比較例4 9.60 0.13 0.44 1.93 5.80 比較例5 9.55 0.07 0.16 1.05 3.02 比較例6 7.89 0.00 0.06 0.16 0.35 實施例1 9.30 0.05 0.64 2.49 9.31 實施例2 9.19 0.02 0.03 0.03 0.04 實施例3 9.09 0.02 0.02 0·02; 0.03 實施例4 9.02 0.02 0.03 0.04 0.05 實施例5 8.95 0.04 0.68 2.65 9.89 13 (請先閱讀背面之注意事項再填寫本頁) # 訂---------線- 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） 1229141 經濟部智慧財產局員工消費合作社印製 A7 B7 五、發明說明（/) 表4 輸入濺鍍功率密度（W/cm2) Sn02組成 累積電量(WHr/cm2) (重量％ ) 40 80 120; 160 比較例1 10.83 0.50 0.54 0.57 0.64 比較例2 10.46 0.50 0.52 0.55 0.58 比較例3 9.97 0.50 0.52 0.54 0.56 實施例1 9.30 0.50 0.52 0.53 0.53 實施例2 9.19 0.50 0.50 0.50 0.53 實施例3 9.09 0.50 0.50 .0.50 0.52 實施例4 9.02 0.50 0.50 0.52 0.53 實施例5 8.95 0.50 0.52 0.54 0.55 (請先閱讀背面之注意事項再填寫本頁) 费 訂---------線. 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） 1229141 A7 B7 經濟部智慧財產局員工消費合作社印製 五、發明說明（θ) ' 於上述表2及圖1〜4中，顯示ΙΤΟ耙中讓Sn02組成 變化於8.95〜10.83 (重量％ )之情況下，濺鍍累積電量40 、80、120、160 W/cm2中微電弧產生次數。 在本發明之範圍（％02之組成爲8.80〜9.40重量％之 範圍）內的實施例1〜5之Sn028.95〜9.30重量％中，即使 增加累積電量，微電弧產生次數也不會過度的增加。 然而，在本發明範圍外之超出Sn02 9·40‘重量％之範 圍（比較例1〜3)中，發現微電弧產生次數會急速地增加 〇 特別是本發明之情況下，在Sn02之組成爲8·90〜9.30 重量％之範圍，更在Sn02之組成爲9.00〜9·20重量％之範 圍（實施例2〜4)中，發現微電弧產生次數之增加被顯著 地抑制。 如實施例1〜5所示，ΙΤΟ靶中之本發明範圍之Sn02組 成之存在，於微電弧之抑制上極爲有效。 < 於上述表3及圖5〜圖8中，顯示ITO靶中之Sn02組 成在8.95〜9·30 (重量％ )範圍變化之情況下，濺鑛累積電 量4〇、8〇、12〇、16〇 W/cm2中瘤塊覆蓋率。 在本發明之範圍（Sn02之組成爲8.80〜9.40重量％之 範圍）內的實施例1〜5之Sn028.95〜9·30重量％中，即使 增加累積電量，瘤塊覆蓋率也不會過度的增加。 然而，在本發明範圍外之超出Sn02 9.40重量％之範 圍（比較例1〜6)中，雖然有或多或少的變，但是瘤塊 15 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） --------------------丨訂---------線 (請先閲讀背面之注意事項再填寫本頁) 1229141 A7 B7 五、發明說明（A) 覆蓋率係急速地增加。 (請先閱讀背面之注意事項再填寫本頁) 特別是本發明之情況下，在Sn02之組成爲8.90〜9.30 重量％之範圍，更在Sn022組成爲9·00〜9.20重量％之範 圍（實施例2〜4)中，瘤塊覆蓋率幾乎不增加，顯著地被 抑制住。 如實施例1〜5所示，ΙΤΟ靶中之本發明範圍之Sn02組 成之存在，對於瘤塊之抑制極爲有效。 於上述表4及圖9中，顯示ITO靶中之Sn02組成在 8.95〜10.83 (重量％ )範圍變化之情況下，濺鍍累積電量 80、120、160 W/cm2之輸入濺鍍功率密度（W/cm2)(還 有，由於在濺鑛累積電量40 W/cm2無差異存在乃省略之） 〇 在本發明之範圍（Sn022組成爲8.80〜9.40重量％之 範圍）內的實施例1〜5之Sn028.95〜9.30重量％中，即使 增加累積電量，輸入濺鑛功率密度也不會過度的變化。 然而，在本發明範圍外之超出Sn02 9.40重量％之範 圍（比較例1〜3)中，發現爲了使成膜速度一定，必須變 化（提高）輸入濺鍍功率密度。 ， 經濟部智慧財產局員Η消費合作社印製 特別是本發明之情況下，在Sn02之組成爲8·90〜9.30 重量％之範圍，更在Sn02之組成爲9.00〜9.20重量％之範 圍（實施例2〜4)中，幾乎沒有必要變化輸入濺鑛功率密 度。 如實施例1〜5所示，ITO靶中之本發明範圍之Sn02組 成之存在，對於輸入濺鍍功率密度之變化之抑制極爲有效 16 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） A7 1229141 ____B7__ 五、發明說明（A) 。還有，於實施例中，雖然顯示測定Sn02組成爲 8.90〜9.30重量％範圍之微電弧、瘤塊之產生、輸入濺鍍功 率密度之變化的結果，但在本發明、即在Sn02組成爲 8.80〜9.40重量％之範圍中，同樣地得到良好的效果。 又，如表1所示，ITO濺鍰靶之密度爲i〇0 g/cm3以 上、靶之中心線平均粗糙度Ra爲0.5//m以下、靶之平均 結晶粒徑未滿4//m之條件下均可得良好的結果。 (實施例6、7及比較例7、8) 其次，使用Sn02組成不同之靶來進行成膜，測定所得 之ITO膜之電阻係數及可見光範圍之透過率來進行比較。 其結果示於表5。包含於本發明之範圍的Sn02組成者 爲實施例6、7，以外者爲比較例7、8。濺鎪之成膜條件爲 基板溫度200°C、300°C、輸入濺鍍功率密度鳥2.3 W/cm2 ，其他係以相同於上述濺鍍條件來實施。 (請先閱讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 表5 基板溫度 (°〇 Sn02組成」 (窜暈％ ) 電阻係數（X 10'4Qcm ) 透過率 at550nm (% ) 實施例6 200 8.87 3.2 96.1 實施例7 300 8.87 1.8 ; 96.9 比較例7 200 9.84 3.4 95.0 比較例8 300 9.84 1.9 95.5 17 本紙張尺度適用中國國家標準（CNS)A4規格（210 x 297公釐i 1229141 B7 五、發明說明（，） (請先閱讀背面之注意事項再填寫本頁) 由上述實施例6、7與比較例7、8之對比可知，在基 板溫度200°C及300°C之任一個情況下，相較於比較例7、 8，實施例6、7具有同等以上之低電阻係數、高透過率特 性，作爲透明導電體毫不遜色。 還有，在實施例及比較例中，雖對於濺鍍靶之密度、 中心線平均粗糙度Ra及平均粒徑超出本發明之範圍者未 特別指出，但是發現該等有助長濺鏟時所產生之微電弧或 瘤塊的傾向。 而且，已確認本發明之濺鍍靶密度、中心線平均粗糙 度Ra及平均結晶粒徑之調整，可進一步地抑制濺鍰時所 產生之微電弧及粒狀物，並可抑制輸入濺鍍功率密度之變 化。 (發明之效果） 經濟部智慧財產局員工消費合作社印製 本發明係於ITO靶中含有適當量之Sn02 :因而得到適 於ITO透明導電膜等之形成的濺鎪靶，不但可抑制於濺鍍 時所產生之微電弧，耳可降低於靶表面所產生之瘤塊，以 整個靶壽命期間以安定、一定條件來進行濺鍍之操作，此 爲所具有之優異之效果。 18 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐）Sn02 composition density surface roughness Ra average crystal grain size (% of lightning) (g / cm2) (// m) (// m) Comparative Example 1 10.83 7.11 0.39 3.53 Comparative Example 2 10.46 7.12 0.30 3.27 Comparative Example 3 9.97 7.10 0.32 3.74 Example 1 9.30 7.11 0.36 3.41 Example 2 9.19 7.12 0.35 3.15 Example 3 9.09 7.10 0.36 3.24 Example 4 9.02 7.09 0.33 3.68 Example 5 8.95 7.08 0.37 3.25 11 This paper size applies the Chinese National Standard (CNS) A4 specification (210 X 297 mm) (Please read the notes on the back before filling out this page) ----- Order --------- Line · Printed by the Intellectual Property Bureau Employee Consumer Cooperative of the Ministry of Economic Affairs 1229141 A7 B7 V. Description of the invention) Table 2 Number of micro-arc generations (times) printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs, and the cumulative amount of electricity generated by Sn02 (WHr / cm2) (% by weight) 40 80 120 160 Comparative Example 2 10.46 13 60 404 1761 Comparative Example 3 9.97 2 24 163 804 Example 1 9.30 0 17 69 647 Example 2 9.19 2 17 32 144 Example 3 9.09 0 13 27, 121 Example 4 9.02 1 20 33 169 Implementation Example 5 8.95 1 22 52 473 12 (Please first Read the notes on the reverse side and fill in this page) --------- Order --------- Line. This paper size is applicable to China National Standard (CNS) A4 (210 X 297 mm) 1229141 A7 B7 V. Description of the invention (\\) Table 3 Coverage rate of printed tumor mass (%) by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs Sn02 Composition Cumulative Electricity (WHr / cm2) (Min.%) 40 80 120 160 Comparative Example 1 10.83 0.33% 3.42 23.71 78.37 Comparative Example 2 10.46 0.24 2.71 20.08 40.29 Comparative Example 3 9.97 0.06 1.21 4.58 18.77 Comparative Example 4 9.60 0.13 0.44 1.93 5.80 Comparative Example 5 9.55 0.07 0.16 1.05 3.02 Comparative Example 6 7.89 0.00 0.06 0.16 0.35 Example 1 9.30 0.05 0.64 2.49 9.31 Example 2 9.19 0.02 0.03 0.03 0.04 Example 3 9.09 0.02 0.02 0.02; 0.03 Example 4 9.02 0.02 0.03 0.04 0.05 Example 5 8.95 0.04 0.68 2.65 9.89 13 (Please read the precautions on the back first (Fill in this page) # Order --------- Line-This paper size is applicable to China National Standard (CNS) A4 (210 X 297 mm) 1229141 Printed by A7 B7 of the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs Description of the invention (/) Table 4 Input splash Power density (W / cm2) Sn02 composition cumulative power (WHr / cm2) (% by weight) 40 80 120; 160 Comparative Example 1 10.83 0.50 0.54 0.57 0.64 Comparative Example 2 10.46 0.50 0.52 0.55 0.58 Comparative Example 3 9.97 0.50 0.52 0.54 0.56 Implementation Example 1 9.30 0.50 0.52 0.53 0.53 Example 2 9.19 0.50 0.50 0.50 0.53 Example 3 9.09 0.50 0.50 .0.50 0.52 Example 4 9.02 0.50 0.50 0.52 0.53 Example 5 8.95 0.50 0.52 0.54 0.55 (Please read the notes on the back before filling in (This page) Fee-booking ------- line. This paper size is applicable to China National Standard (CNS) A4 (210 X 297 mm) 1229141 A7 B7 Printed by the Consumer Cooperative of Intellectual Property Bureau of the Ministry of Economic Affairs Description of the invention (θ) 'In the above Table 2 and Figs. 1 to 4, it is shown that when the composition of Sn02 in the ITO is changed from 8.95 to 10.83 (wt%), the cumulative power of sputtering is 40, 80, 120, 160 W / The number of micro arcs in cm2. In the range of the present invention (the composition of% 02 is in the range of 8.80 to 9.40% by weight) in Sn028.95 to 9.30% by weight of Examples 1 to 5, even if the accumulated electric quantity is increased, the number of micro-arc generation will not be excessive. increase. However, in the range beyond Sn02 9.40'wt% (Comparative Examples 1 to 3) outside the scope of the present invention, it was found that the number of micro-arc generations increased rapidly. Especially in the case of the present invention, the composition of Sn02 was In the range of 8.90 to 9.30% by weight, and in the range of Sn02 having a composition of 9.00 to 9.20% by weight (Examples 2 to 4), it was found that the increase in the number of micro-arc generation was significantly suppressed. As shown in Examples 1 to 5, the presence of the Sn02 composition within the scope of the present invention in the ITO target is extremely effective in suppressing the micro-arc. < In the above Table 3 and FIG. 5 to FIG. 8, when the Sn02 composition in the ITO target is changed in the range of 8.95 to 9.30 (% by weight), the cumulative amount of spattered ore is 40, 80, 120, Coverage of tumor mass at 160W / cm2. In the range of the present invention (the composition of Sn02 is in the range of 8.80 to 9.40% by weight), in Sn028.95 to 9.30% by weight of Examples 1 to 5, even if the cumulative electric quantity is increased, the nodules coverage will not be excessive. Increase. However, in the range outside the scope of the present invention exceeding 9.40% by weight of Sn02 (Comparative Examples 1 to 6), although there are more or less changes, the lump 15 is a paper size that applies the Chinese National Standard (CNS) A4 specification ( 210 X 297 mm) -------------------- 丨 Order --------- line (Please read the precautions on the back before filling this page ) 1229141 A7 B7 V. Description of the Invention (A) The coverage rate has increased rapidly. (Please read the precautions on the back before filling this page.) In the case of the present invention, in particular, the composition of Sn02 is in the range of 8.90 to 9.30% by weight, and the composition of Sn022 is in the range of 9.0 to 9.20% by weight. In Examples 2 to 4), the coverage of the tumor mass hardly increased and was significantly suppressed. As shown in Examples 1 to 5, the presence of the Sn02 composition within the scope of the present invention in the ITO target is extremely effective for suppressing tumor masses. In the above Table 4 and FIG. 9, when the Sn02 composition in the ITO target is changed in the range of 8.95 to 10.83 (% by weight), the input sputtering power density (W, cm, 80, 120, 160 W / cm2) of the cumulative sputtering power (W / cm2) (Also, it is omitted because there is no difference in the cumulative power consumption of 40 W / cm2 in the splatter ore.) 〇 Examples 1 to 5 within the scope of the present invention (the composition of Sn022 is 8.80 to 9.40% by weight) From Sn028.95 to 9.30% by weight, even if the accumulated power is increased, the input power density does not change excessively. However, in the range outside the range of the present invention of 9.40% by weight of Sn02 (Comparative Examples 1 to 3), it has been found that in order to make the film formation rate constant, it is necessary to change (increase) the input sputtering power density. Printed by a member of the Intellectual Property Bureau of the Ministry of Economic Affairs and a consumer cooperative, especially in the case of the present invention, the composition of Sn02 is in the range of 8.90 to 9.30% by weight, and the composition of Sn02 is in the range of 9.00 to 9.20% by weight (Example 2 to 4), there is almost no need to change the input sputtering power density. As shown in Examples 1 to 5, the existence of the Sn02 composition in the scope of the present invention in the ITO target is extremely effective in suppressing the change in the input sputtering power density. 16 This paper size applies the Chinese National Standard (CNS) A4 specification (210 X 297 mm) A7 1229141 ____B7__ 5. Description of the invention (A). In the examples, although the results of measuring the micro-arc, the generation of nodules, and the input sputtering power density in the range of 8.90 to 9.30% by weight of the Sn02 composition are shown, in the present invention, that is, the Sn02 composition is 8.80. In the range of ~ 9.40% by weight, similarly good effects are obtained. In addition, as shown in Table 1, the density of the ITO sputtering target is 100 g / cm3 or more, the centerline average roughness Ra of the target is 0.5 // m or less, and the average crystal grain size of the target is less than 4 // m. Good results can be obtained under these conditions. (Examples 6, 7 and Comparative Examples 7, 8) Next, films were formed using targets with different Sn02 compositions, and the resistivity and transmittance in the visible range of the obtained ITO films were measured for comparison. The results are shown in Table 5. The constituents of Sn02 included in the scope of the present invention are Examples 6 and 7, and the others are Comparative Examples 7 and 8. Film formation conditions for sputtering were substrate temperature 200 ° C, 300 ° C, input sputtering power density 2.3 W / cm2, and other conditions were implemented under the same sputtering conditions as described above. (Please read the precautions on the back before filling out this page) Printed by the Intellectual Property Bureau of the Ministry of Economic Affairs, Employee Consumer Cooperatives, Table 5 Substrate temperature (° OSn02 composition) (% halo) Resistivity (X 10'4Qcm) Transmission at550nm ( %) Example 6 200 8.87 3.2 96.1 Example 7 300 8.87 1.8; 96.9 Comparative Example 7 200 9.84 3.4 95.0 Comparative Example 8 300 9.84 1.9 95.5 17 This paper size applies the Chinese National Standard (CNS) A4 specification (210 x 297 mm) i 1229141 B7 V. Description of the Invention (,) (Please read the precautions on the back before filling this page) From the comparison between the above Examples 6, 7 and Comparative Examples 7, 8, it can be seen that the substrate temperature is 200 ° C and 300 ° C In either case, compared to Comparative Examples 7, 8, Examples 6 and 7 have equivalent low resistivity and high transmittance characteristics, and are not inferior as transparent conductors. In addition, in Examples and Comparative Examples Although the density, the centerline average roughness Ra, and the average particle diameter of the sputtering target are not specifically mentioned outside the scope of the present invention, they have been found to contribute to the tendency of micro-arc or nodules generated during sputtering. And, already It is recognized that the adjustment of the sputtering target density, the centerline average roughness Ra, and the average crystal grain size of the present invention can further suppress the micro-arc and particles generated during sputtering, and can suppress the change in the input sputtering power density. (Effects of the invention) Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs This invention contains an appropriate amount of Sn02 in the ITO target: Therefore, a sputtering target suitable for the formation of ITO transparent conductive film and the like can be obtained, which can not only suppress the sputtering The micro-arc generated during plating can reduce the nodules generated on the surface of the target, and the sputtering operation is performed under stable and certain conditions throughout the life of the target, which is an excellent effect. 18 Paper Size Applicable to China National Standard (CNS) A4 (210 X 297 mm)