200912021 九、發明說明： 【發明所屬之技術領域】 本發明係關於使用於濺鍍裝置之鋁_鋰合金（aluminum -lithium alloy ingot)靶材（target)之製造方法及使用該 方法所製造之銘-鐘合金乾材。 【先前技術】 對於有機電致發光（electro iumjnescence)(有機el) 凡件，係要求能夠實現高發光效率化及高亮度化，且為環 境安定性較高之材料。以滿足此種要求之材料而言，已知 有A1-Li(鋁-鋰）系合金。在下述專利文獻j中，係記載有 以Al-Li系合金之之濺鍍膜來構成有機乩元件之電子注入 電極（陰極）。 然而，對於濺鍍用之靶材，係強烈要求具備均一性。 具體而言，係要求合金元素要均一地分散、雜質要少、夾 雜物要少、結晶組織要均一、電阻值分布要良好等。如200912021 IX. Description of the Invention: [Technical Field] The present invention relates to a method for producing an aluminum-lithium alloy ingot target used in a sputtering apparatus and a manufacturing method using the same - Bell alloy dry material. [Prior Art] For organic electroluminescence (organic el), it is required to achieve high luminous efficiency and high luminance, and it is a material with high environmental stability. An A1-Li (aluminum-lithium)-based alloy is known as a material that satisfies such requirements. In the following Patent Document j, an electron injecting electrode (cathode) in which an organic tantalum element is formed by a sputtering film of an Al-Li alloy is described. However, for targets for sputtering, uniformity is strongly required. Specifically, the alloying elements are required to be uniformly dispersed, the impurities are less, the inclusions are less, the crystal structure is uniform, and the resistance value distribution is good. Such as
Al-Li系合金等在添加元素中使用容易與氧、氮、水分反 應之材料（鋰）之合金系中，需於其合金化之際，必須謀求 抑制熔渣(slag)產生、抑制水分、及抑制與使用於熔解爐 或工具之耐火物產生反應。 以習知之AHi合金之製造方法而言，已知有在大桌 炫解之AHi合金之製造方法（參照專利文獻2)、及在^ ，溶解之Al-Li合金之製造方法（參照專利文獻3)。此外 旦ίϋ文獻4、5中係揭示有—種藉由進行添加元素之添办 里五、办液之鑄造控制或凝固控制而謀求濃度分布之均一价 320103 5 200912021 之鋁系合金之單結晶靶材之製造方法。 專利文獻1:日本特開平u_329746號公報 專利文獻2:日本特公平6-47697號公報 專利文獻3:日本特開平6_33〇2〇3號公報 專利文獻4:日本特開平7_3〇〇667號公報 專利文獻5:日本特開平1 1-12727號公報 【發明内容】 [發明欲解決之問題] 〜以往A1_Li合金之開發主要係以作為航空器用途來史 仃’而-直在對於環境氣體控制、耐火物之選定、〕 檢討、^添加方法造技術方面進ί 開發H尚未製作出—種供製㈣朗需之 十 夹雜物含量少之減鍍用乾材用鑄錠ungot)。⑴又』 右要製作供薄膜製作用濺鍍靶材所需之具有較 度之鑄錠，當然要抑制與轉材料中之 物 惟必須抑制鐘與大氣中之氧、氮、水分之反 係極低到峨，且其比重為金屬中最輕量之元1 此外，鐘係易於與氧或氮反應，且因水分: :解極二:”氧化物。因此，與鐘之合金化所需之 i合金化之材金化之溶解時，係採取以提高链 後、隹1:觸效率之方式分散材料再放入㈣之 m熔解之方法、或是分散材料並 之方法。然而’在比重為—分之1，且對氧、t; 320103 6 200912021 .極具活性之金屬鋰與鋁之合金化之熔解方面，會產生鋰之 • 氧化而阻礙合金化，故不理想。 • P方面’在冷卻固化之過程巾m無法固溶於紹 .，結晶相内，則鐘就會在銘結晶相外之晶粒界形成結晶或析 .出成為AlLi(々相）。此時，鑄旋之塑性加工性會顯著降 低，或在鍛造加工為板狀、及輥軋加工時產生破裂或邊緣 破裂（邊緣附近之龜裂）等，而難以進行_加工以势进滅 .鍍乾材。此外，在從洗鑄溶融A卜u合金之缚旋所獲得之 革巴材中，係於ΑΠ^相）結晶或析出於銘結晶相外時，合 =電阻不同之二相混合區域，而在減鍍成膜時成為； =電之原因。因此，必須規文饥心相）之結晶或析出 極^之Al-Li合金之鋰含量之上限值。 本發明係有鑑於上述問題而研創者，其目 ==雜物含量少、且組成分布均質之—材 之製&方法及鋁-鋰合金靶材。 ^ [解決問題之方案] 為解決以上問題’本發㈣—合絲材 其二單一相所構成者: 〜“ 驟.弟1步驟，在設置於維持在直* s 體:=之咖 拌；第3步驟在前述掛禍内之㈣液中並加以授 於禱模；及第4二=^呂1合金之稼液進行濟禱 制。 騾進仃别述鋁-鋰合金之鑄錠之組織控 320J〇3 7 200912021 - 在第1步财，於雉持在真空環境錢性氣體環境之 .熔解爐内之掛瑪將链熔解。接著，在第2步驟中，將鐘塊 ，強制浸潰於銘熔液中並進行授摔。藉由在上述溶解爐内進 .行鋰之熔解，而抑制合金化時之鋰之氧化等，而防止含鋰 ，化合物溶渔之產生。此外，藉由將㈣制浸潰在銘溶液中， 且進行擾拌，即可防止因為銘與鐘之比重差所引起之濃度 不均之產生，而使鋰在鋁熔液中均勻地分散。 , 帛2步驟係具有··將固定有鐘塊之石墨製插塞之前端 <部浸潰於掛禍内之步，驟；及使插塞旋轉而擾摔㈣之步 驟。鋰塊係收容於鋁製之箱體内。該箱體係於鋁熔液内盥 經塊-同熔解。插塞係在掛禍之正上方待機，於銘之溶解 中，在坩堝與插塞之間設置熱遮蔽板，藉此而防止在第1 步驟中由於輻射熱而導致鐘之炫解。炫液之授摔係藉由插 塞繞著軸旋轉動作而進行。 為了獲得由鋁單一相所構成之濺鍍用M_Li合金靶 =鐘之添加置係為3重量％以下為較佳。在此，所謂由鋁 單相所構成之A1-Li合金係指A1元素與Li元素之固熔 體（solid s〇luti〇n)。依據A卜u系平衡狀態圖，金屬u 相對於金屬A1之最大固熔限度在約6〇〇它為4重量％。然 而金屬Li之最大固熔限度係隨著溫度降低而沿著熔解度 曲線減少。因此，在最大固熔限度以上之Li添加量時，將 無法阻止凝固時AlLi(冷相）在鋁相中結晶、及從過飽和固 溶胆析出。若發生此等結晶或析出，則塑性加工性就會劣 化而使加工精度降低。此外，從減鍍用革巴材之觀點而言， 320103 8 200912021 由於比电阻不同之二相混合組成之存在，而誘發異常放電 而使成膜率受仔不安定，故膜厚分布亦劣化。因以上理由， 故將鋰添加量設為3重量％以下。 弟3步驟中，係使掛堝在熔解爐内傾動，且將銘一 裡合金之溶液洗鑄於鄰接該掛禍而設置 ^空環境或惰性氣體環境之熔職之t，藉由 解鋰之添加/炼解、潦鑄進行一貫作業，即可獲得鐘氧 化物、氮化物或氫氧化物等異物極少之M—u合金禱疑。 此外」為了抑制夾雜物析出於銘相中，以適度之冷卻速度 使其凝固為較佳。例如，在鑄模使用銅等導熱率較高材料， 應屬當然，而以-面強制冷卻鑄模一面進行炼液堯轉之方 法為較佳。 在第4步驟中，係進行所製得之銘-鐘合金之鑄旋之組 織控制。在鑄錠之.組織控制中係包括有：锻造步驟，包含 用以加工成所希望之靶材形狀之輥軋加工或抽拉加工等； 及熱處理步驟，用以去除内部應力及調整結晶組織 製程溫度之目的在於防止鐘夹雜物析出於銘相中，以較共 晶溫度更低之溫度進行為較佳，具體而言，係以咖。d 下之溫度條件進行。 ^以上方式所製造之铭-鐘合絲材可獲得異物及夹 ，物U少，且組成分布在挪以内之均質之紹單一相电 織。、因此’在減鐘成膜時可抑制異常放電之產生，並可_ 求成膜率之安定化與膜厚分布之均—化。 、 (發明之效果） 320103 200912021 如以上所述，依據本發明，即可獲得異物及夾雜物含 量少’且組成分布均勻之鋁—鋰合金靶材。 【實施方式】 以下參照圖式說明本發明之實施形態。 第1圖係顯示適用於本發明實施形態之鋁-鋰（A1_Li) 合金靶材之製造方法之熔解爐1〇之構成概略剖面圖。此熔 解爐10係具備：真空槽u，具備連接於未圖示之真空泵 之排氣口 11c ;掛堝12，設置於該真空槽n之内部（熔解 至）；及插塞13，位於該坩堝12之正上方。 在坩堝12中裝入有鋁塊21，而於插塞13之前端部係 保持有鐘塊22。真空槽丨丨之内部係調整為預定之真空環 兄或置換為惰性氣體之環境。如後所述，熔解爐1〇係於在 =堝12内將鋁塊21熔解之後，將插塞13之前端部浸潰在 其鋁熔液内而將鋰塊22熔解。 、 坩堝12係為石墨製之有底圓筒體，收容於可動容著 右2部。在可動容器14之内部係固定有在外周部捲言; 有線圈15之耐火性伴捭禮杜 持槿杜人㈣持構件…而㈣12係收容於該命 符構件16之内部。伴牲雄 玄哭- 保持構件16係例如由碳所形成。可鸯 =自it藉由轉動轴18而設置成可相對於⑽ 線圈15、i f坩堝12、保持構件16及鋁塊21係藉由對於 冰囿15通電而加埶。 v <、、、 轉動輛18係連4士於今番―古 旋轉機構， a °在真二槽11外部之未圖i 自如地轉可動容器14相對於基座構件1: 3 ’、可没為推動操作可動容器而使該可重 320103 10 200912021 器14繞著轉動軸18轉動之構成β 在㈣12之開口周緣部之最小轉動半徑位i中，係形 成有作為澆注口之唇部12A。於坩堝12之開口周緣部之盆 他區域係安裝有複數支具有與唇部12AA致相同突出高^ 之支撐棒12B。支撐棒12B係由石墨或不鏽鋼等較可承： 熱衝擊之材料所形成。 & 再者，在此等唇部12A與支撐棒12β之前端之上，係 載設有熱遮蔽板19。熱遮蔽板19係用以防止鋰塊22因為 銘塊21轉時之輻射熱㈣解者。熱遮蔽板19係由例: 石墨所形成’且以可選擇性地採取將坩堝12之開口部遮蔽 之圖示位置、與將掛㉟12之開口部開放之位置之方式構 成。具體而言’係使用例如未圖示之操縱器（manipulator) 來進行熱遮蔽板19之移動控制。 插塞13係由壓縮石墨材料所形成。插塞13係連結於 設置在真空槽11外部之未圖示驅動機構，且構成為可沿著 驅動機構之軸方向上下運動、及沿著軸周圍旋轉運動。 在插塞13之前端部13A係保持有用以收容鐘塊22之 紹製箱體23。箱體23係將例如箱狀或片狀紹材變形為適 當之形狀所形成。㈣22係以真空封人於箱體23之内部 為較佳。在本實施形態中，箱體23係使⑽製線材⑷呆 持於插塞13之前端部13A。另外，箱體23及線材24係由 與銘塊21同等之純度所形成。 在真空槽11之内部係設置有鑄模25。此禱模25係與 可動容器14相鄰接設置，且於以朝轉動軸18周圍之轉動 320103 11 200912021 動作接受從坩堝12經由唇部12A所流出之八卜以合金熔液 同時冷卻固化’㈣成預定形狀之AI-U合金之鑄靛。鑄 模25係具備··冷卻板26,在内部設有冷卻水之循環機構； 模框27,設置在冷卻板26之上方；及厚度較薄之碳片28, 其係設置在冷卻板26與模框27之間。模框27之形狀及高 度並未特別限定’可依據要形成之鑄錠形狀而適當選擇為 圓形或四角开/專。石反片2 8係以防止在洗注後之禱旋脫模性 降低為目的所設置。 接著說明使用以上述方式所構成之溶解爐1〇之本實 2形態之A卜Li合金靶材之製造方法。第2圖A至c係為 說明本實施形態之AKi合金靶材之製造方法之主要步驟 模式圖。 (第1步驟） 首先，將鋁塊21農入坩堝12之中。鋁塊21之純度愈 高愈佳，可使用例如99.99%(4nine)以上純度者。只要^ 可獲得所需量之熔液限度内，塊21之形狀或塊數並無特 別限制。 另一方面，將鋰塊22收容於内部之箱體23保持在插 塞13之前端部13A。鋰塊22之純度愈高愈佳，可使用例 =99·9%(3 nine)以上純度者。箱體23對插塞13之前端 部13A之固定雖係使用鋁製之線材24，惟當然不予限定， 亦可藉由與前端部13A之繫合作用來固定箱體23。 接，，將真空槽11之内部（熔解室）進行真空排氣而維 持於預疋之真空度。溶解室之壓力並無特別限定，惟從防 320103 12 200912021 =及=解時之氧化反應等觀點，係以真 回為Μ。例如設定為以㈣們町）以下之塵力。 • Αώ。“方面，溶解至之環境並不限定於真空環境，亦可 為氬（Ar)等惰性氣體所置換之氣體# ρ -^ ^ I夏拱疋風體％ i兄。此時，一旦將 Ί曰 内部進行真空排氣到預定壓之後，將氬氣導入 至真空槽11之内部。此時 八 壓為低之麗力。 才之料至之壓力係設定為較大氣 在真空槽11之調壓完成之後’在坩堝 設 熱遮蔽板19，且i隹一牛、上万叹置 ^進仃線圈15之通電控制而執行坩 點“ii fij。’、、理。掛堝12之加熱溫度係設定為較銘之熔 脑、n為高的溫度。藉此，銘塊21係在掛堝12内 21之^^形態中’係在與大氣祕之環境下進行銘塊 物等Π 可抑仙在轉時之反應，而可獲得氧化 物等雜質較少之鋁熔液。 此外，由於鐘塊22之溶點⑽。c)係較銘還低，因此 紹，21溶解時會有鋰塊22因為叙之輜射熱而炫解之 二= 在本實，中，由於在紹塊21之熔解時將掛 J 、相熱遮敝板19覆蓋’因此來自坩堝12輻射熱 曰到達相體23，因此可避免鋰塊22之熔融。 … (第2步驟） 接下來進行銘與鐘之合金化所需之熔解（第2圖 ::步驟中，首先將覆蓋掛禍12上部之熱遮蔽㈣去除。 …、、後’使插塞13下降預定量，且將其前端部ΐ3Α浸漬於紹 320103 13 200912021 熔液内，而將鋰塊Μ熔解。另外，此時鋁製之箱體“及 線材24亦一同溶解。 接下來使插塞13繞著其軸旋轉並攪拌坩堝12内之熔 液20(第2圖Β)。攪拌作用主要可藉由婦塞前端部UA之 形狀效應而獲得。在本實施形態中，係將插塞前端部 形成為使突起部（葉片）突出在前端部13A外周^之複數個 位置之形狀，藉此僅以插塞13之自轉即可獲得較大之攪 作用。 ， / 在本實施形態中，係在經環境調整之真空槽2丨之内部 進行鋰塊22添加至鋁熔液之操作，因此可抑制合金化時之 鐘之氧化等，且可防止含鐘化合物㈣之產生。此外，由 於藉由上述之方法使鐘塊22強制浸潰於鋁熔液中且進行 攪拌，因此可防止因為鋁與鋰之比重差所引起之濃度不 均，而可使鋰均勻地分散於鋁熔液中。再者，由於坩^ 12 為石墨製，因此可防止含有鋰之鋁熔液面對於坩堝12之衝 擊，而可抑制含鋰化合物之生成。 在此，作為濺鍍用靶材所使用之A1—Li合金，從塑性 加工及使用時之成膜特性之觀點而言，係以紹單一相為較 佳。一所謂由紹單一相所構成之AKi合金係指A1元素與 L、i兀素之固溶體。合金組織若變成多相，添加元素之組成 刀布（/辰度刀布）就變大，而塑性加工性就降低。此外，由 於比電阻不同之二相之混合組成之存在’導致在革巴材表面 產生電阻分布而引起異常放電，而無法謀求成膜率之安定 化與膜厚分布之均一化。 320103 14 200912021 為了獲得由I呂單一相所構成之錢鍍用A1 -L i合金革巴 材，鋰之添加量，以合金總成分基準，以3重量％以下為較 佳。在本實施形態中，鋰塊22之添加量係為鋁塊21、箱 體23、線材24及該鐘塊22之總重量之3%以下。 第3圖係模式性顯示a 1 -L i系平衡狀態圖（取材自： BINARY ALLOY PHASE DIAGRAMS」 Second Edition T B Massalski， ASM INTERNATIONAL ISBN: Q-8717〇-4〇4-8)。 鋰相對於鋁之最大固熔限度係為596〇c、4重量％。然而， 鋰之最大固熔限度係隨著溫度降低而沿著熔解度曲線％ 減少。因此，最大固熔限度以上之鋰添加量，將無法阻止 在凝固時AlLi( 3相）會析出至鋁相中。在本實施形態中， 係將鋰之添加量抑制在3重量％以下，並且如後所述地以一 定以上之冷卻速度進行料之料，藉此製作㈣單—相 所構成之Al-Li合金歡材。 (第3步驟） 接著進行將掛禍12内之A1-U合金之溶液2〇洗鑄 鑄模25之步驟（第2圖〇。在此步驟中，係使可動容写' 】 如圖中繞著轉動軸18以逆時針方向轉動，藉此而例 坩堝12，將熔液2〇澆鑄至鑄模25。使冷太 媸 =模25之冷卻板26之内部。因此，從掛❹流出:w S金熔液20、係在鑄模25中以一定之冷卻速度固化。藉此 P ^方止因為鐘之過餘和引起饥心相）結晶析出曰至雀 相中，在固化後亦可維持鋁單一相。 在本實施形態巾’“餘轉於真”境之溶解龙 320103 15 200912021 中k仃鋁之熔解、鋰之添加、熔解、洗鑄等一貫作業， α此可獲知鋰氧化物、氮化物或氫氧化物等異物極 Al-Li合金鱗錢。 (第4步驟） 接下來進行所獲得之A1_u合金鑄錠之組織控制。 錠之組織控制中係包括有：鍛造步驟，包含用以加工為 所希望之乾材形狀之輕乾加工或抽拉加 驟，用以去除内部應力及調整結晶組織。 ^理步 在此之製程溫度係設為55代以下。此係、由於即 限度以下，合金組織為單-相之情形，亦 ^ 、衣/皿度之不同，而使冷相因為後續之塑性加工、 二：：有析出之虞的緣故。例如’即使是在共晶點以下 又亦會因為加熱爐之均一性或加工部之過熱等 2 ’而有局部性超過共晶線（共晶溫度）之情形。若万相In an alloy system in which a material (lithium) which is easily reacted with oxygen, nitrogen, or water is used as an additive element in an Al-Li-based alloy, it is necessary to suppress the generation of slag and suppress moisture during alloying. And inhibiting the reaction with the refractory used in the melting furnace or tool. A method for producing an AHi alloy which is smeared on a large table (see Patent Document 2) and a method for producing a dissolved Al-Li alloy (see Patent Document 3) ). In addition, in the literatures 4 and 5, it is disclosed that there is a single crystal target of an aluminum alloy which has a uniform concentration of 320103 5 200912021 by performing the casting control or solidification control of the additive element. Manufacturing method of materials. Patent Document 1: Japanese Patent Publication No. Hei. No. Hei. No. Hei. No. 6-47697. Patent Document 3: Japanese Patent Publication No. Hei 6-33〇2〇3 Patent Publication No. 4: Japanese Patent Application Laid-Open No. Hei. Document 5: Japanese Laid-Open Patent Publication No. Hei No. 1-12-12 [Consultation] [Problems to be Solved by the Invention] ~In the past, the development of the A1_Li alloy was mainly used for the purpose of aircraft use, and the direct control of the environmental gas, refractory The selection, the review, the addition method, the technical aspects of the development, the development of the H has not yet been produced - a kind of supply (four) the need for less than ten inclusions of the dry material for castings used for castings ungot ungot). (1) In addition, it is necessary to make a relatively ingot for the sputtering target for film production. Of course, it is necessary to suppress the contents of the material and to suppress the oxygen, nitrogen and water in the clock and the atmosphere. It is as low as 峨, and its specific gravity is the lightest of the metals. In addition, the bell is easy to react with oxygen or nitrogen, and because of moisture: : solution of the second: "oxide. Therefore, it is necessary to alloy with the bell. When the alloying of the alloyed metal is dissolved, the method of dispersing the material in the manner of increasing the chain after the chain, the efficiency of the enthalpy, and then inserting the (m) melting method or the method of dispersing the material is adopted. -1, and oxygen, t; 320103 6 200912021. In the melting of the alloy of highly active metal lithium and aluminum, it will produce oxidation of lithium and hinder alloying, so it is not ideal. The cooling and solidification process towel m can not be dissolved in the crystal phase, and the crystal will form crystals or precipitate out in the grain boundary outside the crystal phase to form AlLi (々 phase). At this time, the plasticity of the casting spin The processability is significantly reduced, or it is broken when the forging process is a plate shape and the roll processing is performed. Or the edge is cracked (cracks near the edge), etc., and it is difficult to carry out the process to extinction. The dry material is plated. In addition, in the leather material obtained by the spinning and spinning of the A-u alloy, it is When the crystal is crystallized or precipitated out of the crystal phase, the two-phase mixed region with different resistances is formed when the film is formed by de-plating; = the reason for electricity. Therefore, it must be crystallized or The upper limit of the lithium content of the Al-Li alloy in which the electrode is deposited. The present invention has been developed in view of the above problems, and the object is a method for producing a material having a small amount of impurities and having a uniform composition distribution and a method and aluminum. - Lithium alloy target. ^ [Solution to solve the problem] In order to solve the above problem, 'the hair of the hair (four) - the wire is composed of two single phases: ~" Step. Step 1 is set to maintain in the straight * s body : = 咖 咖 ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ;骡 仃 组织 铝 铝 铝 铝 铝 铝 铝 铝 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 320 Next, in the second step, the clock block is forcibly immersed in the melt and transferred. By performing lithium melting in the above-mentioned dissolution furnace, oxidation of lithium during alloying or the like is suppressed, and lithium-containing compound is prevented from being produced. In addition, by impregnating the (4) system in the solution and performing the scramble, it is possible to prevent the lithium from being uniformly dispersed in the aluminum melt due to the uneven concentration caused by the difference in specific gravity between the mark and the bell. The step 2 is a step of immersing the front end of the graphite plug to which the block is fixed, in the step of smashing, and rotating the plug to disturb (4). The lithium block is housed in an aluminum case. The tank system is melted in the aluminum melt by block-same melting. The plug is placed in the upper side of the hazard. In the dissolution of Yu, a heat shield is placed between the cymbal and the plug, thereby preventing the glare from being caused by the radiant heat in the first step. The sinking of the liquid is carried out by the rotation of the plug around the shaft. In order to obtain an M_Li alloy target for sputtering composed of a single aluminum phase, it is preferable to add 3% or less of the addition of the clock. Here, the A1-Li alloy composed of a single phase of aluminum means a solid sol of the A1 element and the Li element. According to the A-u system equilibrium state diagram, the maximum solid-solution limit of the metal u with respect to the metal A1 is about 6 〇〇, which is 4% by weight. However, the maximum solid solubility limit of the metal Li decreases along the melting curve as the temperature decreases. Therefore, when Li is added at a maximum solidification limit or more, it is impossible to prevent AlLi (cold phase) from crystallizing in the aluminum phase and precipitation from the supersaturated solid solution during solidification. When such crystallization or precipitation occurs, the plastic workability is deteriorated and the processing accuracy is lowered. Further, from the viewpoint of the leather material for the plating reduction, 320103 8 200912021, due to the existence of a two-phase mixed composition having a different specific resistance, an abnormal discharge is induced and the film formation rate is unstable, so that the film thickness distribution is also deteriorated. For the above reasons, the amount of lithium added is 3% by weight or less. In the third step of the younger brother, the hanging raft is tilted in the melting furnace, and the solution of the alloy of Mingyili is washed and cast in the vicinity of the smashing environment to set the environment of the empty environment or the inert gas environment, by solving the lithium Adding / refining, casting, and consistent operation, you can get the M-u alloy prayer with very few foreign substances such as oxides, nitrides or hydroxides. In addition, in order to suppress the inclusion of inclusions in the phase, it is preferred to solidify at a moderate cooling rate. For example, it is preferable to use a material having a high thermal conductivity such as copper in the mold, and it is preferable to carry out the method of refining the liquid while forcibly cooling the mold. In the fourth step, the structure control of the cast ring of the produced Ming-Zhong alloy is carried out. In the ingot control, the tissue control includes: a forging step, including a rolling process or a drawing process for processing into a desired target shape; and a heat treatment step for removing internal stress and adjusting the crystal structure process The purpose of the temperature is to prevent the inclusion of the bell inclusions from being in the same phase, preferably at a temperature lower than the eutectic temperature, and in particular, it is a coffee. The temperature conditions under d are carried out. ^The Ming-Zhonghe wire material manufactured by the above method can obtain foreign matter and clips, and the material U is small, and the composition is distributed in the uniformity of the single phase of the wire. Therefore, the occurrence of abnormal discharge can be suppressed when the film is formed by the reduction of the clock, and the film formation rate can be stabilized and the film thickness distribution can be uniformized. (Effect of the Invention) 320103 200912021 As described above, according to the present invention, an aluminum-lithium alloy target having a small content of foreign matter and inclusions and having a uniform composition distribution can be obtained. [Embodiment] Hereinafter, embodiments of the present invention will be described with reference to the drawings. Fig. 1 is a schematic cross-sectional view showing a configuration of a melting furnace 1〇 which is applied to a method for producing an aluminum-lithium (A1_Li) alloy target according to an embodiment of the present invention. The melting furnace 10 includes a vacuum chamber u, and includes an exhaust port 11c connected to a vacuum pump (not shown), a hook 12 disposed inside the vacuum tank n (melted), and a plug 13 located at the crucible Just above the 12th. The aluminum block 21 is housed in the crucible 12, and the clock block 22 is held at the end before the plug 13. The interior of the vacuum chamber is adjusted to a predetermined vacuum ring or an inert gas atmosphere. As will be described later, the melting furnace 1 is melted after the aluminum block 21 is melted in the = 12, and the end portion of the plug 13 is immersed in the aluminum melt to melt the lithium block 22. The 坩埚12 series is a bottomed cylindrical body made of graphite, and is housed in the right and movable parts. The outer periphery of the movable container 14 is fixed to the outer peripheral portion; the fire resistance of the coil 15 is accompanied by the 捭 捭 槿 人 人 人 四 四 四 四 四 四 四 四 四 四 四 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 With the male sacred crying - the holding member 16 is formed, for example, of carbon. The 鸯 = self-it is set by the rotation shaft 18 so as to be twistable with respect to the (10) coil 15, the i f 坩埚 12, the holding member 16 and the aluminum block 21 by energizing the hail 15. v <,,, Rotating 18 series of 4 in the current "Ancient Rotating Mechanism", a ° outside the true two slots 11 is not shown i freely transfer the movable container 14 relative to the base member 1: 3 ', can not In order to facilitate the operation of the movable container, the weight of the retractable 320103 10 200912021 is rotated about the rotating shaft 18, and in the minimum rotational radius i of the peripheral edge portion of the opening of the (four) 12, a lip portion 12A as a spout is formed. The basin in the peripheral portion of the opening of the cymbal 12 is provided with a plurality of support rods 12B having the same protrusion height as the lip portion 12AA. The support rod 12B is formed of a material such as graphite or stainless steel which is more resistant to thermal shock. & Further, a heat shielding plate 19 is attached to the front end of the lip portion 12A and the support rod 12β. The heat shield plate 19 is used to prevent the lithium block 22 from being dissipated by the radiant heat (4) when the block 21 is rotated. The heat shielding plate 19 is formed of, for example, graphite, and is configured to selectively take a position where the opening of the crucible 12 is shielded and a position where the opening of the hanging 3512 is opened. Specifically, the movement control of the heat shield plate 19 is performed using, for example, a manipulator (not shown). The plug 13 is formed of a compressed graphite material. The plug 13 is coupled to a drive mechanism (not shown) provided outside the vacuum chamber 11, and is configured to be movable up and down along the axial direction of the drive mechanism and to rotate around the periphery of the shaft. The end portion 13A retains the casing 23 for accommodating the block 22 before the plug 13. The casing 23 is formed by, for example, deforming a box-shaped or sheet-like material into an appropriate shape. (4) It is preferable that the 22 series is vacuum-sealed inside the casing 23. In the present embodiment, the casing 23 holds the wire (4) made of (10) in the end portion 13A before the plug 13. Further, the casing 23 and the wire 24 are formed of the same purity as the ingot 21. A mold 25 is provided inside the vacuum chamber 11. The prayer mold 25 is disposed adjacent to the movable container 14 and is configured to receive the rotation of the alloy melt from the crucible 12 via the lip portion 12A while being cooled toward the rotation axis 18 by 320103 11 200912021. Casting of AI-U alloy in a predetermined shape. The mold 25 is provided with a cooling plate 26, and a circulation mechanism for cooling water is provided therein; a mold frame 27 is disposed above the cooling plate 26; and a thin carbon sheet 28 is provided on the cooling plate 26 and the mold. Between boxes 27. The shape and height of the mold frame 27 are not particularly limited. Depending on the shape of the ingot to be formed, it is appropriately selected to be circular or four-corner open/special. The stone reverse film 8 8 is provided for the purpose of preventing the mold release property from being lowered after the washing. Next, a method of producing the A-Li alloy target using the present embodiment of the dissolution furnace 1 constructed as described above will be described. Figs. 2A to 2C are schematic diagrams showing main steps of a method of manufacturing an AKi alloy target according to the present embodiment. (First Step) First, the aluminum block 21 is introduced into the crucible 12. The purity of the aluminum block 21 is preferably as high as possible, and for example, a purity of 99.99% (4 nine) or more can be used. The shape or the number of blocks of the block 21 is not particularly limited as long as the desired amount of melt is obtained. On the other hand, the casing 23 in which the lithium block 22 is housed is held at the end portion 13A before the plug 13. The higher the purity of the lithium block 22, the better, and the purity of the sample = 99.9% (3 nine) or more can be used. The fixing of the end portion 13A of the plug 23 to the plug 13 is performed by using the aluminum wire 24, but it is of course not limited, and the case 23 can be fixed by cooperation with the front end portion 13A. Then, the inside of the vacuum chamber 11 (melting chamber) is evacuated to maintain the vacuum degree of the pre-twisting. The pressure in the dissolution chamber is not particularly limited, but from the viewpoints of prevention of 320103 12 200912021 = and = oxidation reaction at the time of solution, it is true. For example, it is set to the dust power below (4). • Hey. "In terms of the environment, the environment to be dissolved is not limited to a vacuum environment, and it may be a gas replaced by an inert gas such as argon (Ar). #ρ -^ ^ I Summer arch 疋 风 body% i brother. At this time, once Ί曰After the inside of the vacuum is evacuated to a predetermined pressure, argon gas is introduced into the inside of the vacuum chamber 11. At this time, the eight pressures are low, and the pressure is set to a larger gas in the vacuum tank 11 Then, 'the heat shielding plate 19 is set, and the power supply control of the enthalpy coil 15 is performed, and the “ point "ii fij is performed. ‘,、理理. The heating temperature of the hanging raft 12 is set to a temperature higher than that of the melting brain and n is high. In this way, the inscription block 21 is in the form of the ^^^ in the hanging raft 12, and is in the environment of the secret atmosphere to perform the reaction of the lumps, etc. Less aluminum melt. In addition, due to the melting point of the block 22 (10). c) The system is still lower than the Ming, so Shao, there will be lithium block 22 dissolved in the dissolution of the 21 due to the heat of the sputum = in the real, in the melting of the block 21 will hang J, phase The heat concealing plate 19 covers 'and thus the radiant heat from the crucible 12 reaches the phase body 23, so that the melting of the lithium block 22 can be avoided. ... (Step 2) Next, perform the melting required for the alloying of Ming and Zhong (Fig. 2:: In the step, first remove the heat shield (4) from the upper part of the cover 12. ..., and then make the plug 13 The predetermined amount is lowered, and the front end portion ΐ3Α is immersed in the melt of the 320103 13 200912021, and the lithium crucible is melted. In addition, the aluminum box “and the wire 24 are also dissolved together at this time. Next, the plug 13 is made. Rotating and stirring the molten metal 20 in the crucible 12 around its axis (Fig. 2). The stirring action can be mainly obtained by the shape effect of the front end portion UA of the female plug. In the present embodiment, the front end portion of the plug is inserted. The projections (blades) are formed so as to protrude from the plurality of positions on the outer circumference of the distal end portion 13A, whereby a large agitating action can be obtained only by the rotation of the plug 13. In the present embodiment, The operation of adding the lithium block 22 to the aluminum melt in the inside of the environmentally-adjusted vacuum chamber 2丨 suppresses the oxidation of the clock during the alloying, and prevents the occurrence of the compound (4). Further, The method of forcibly immersing the block 22 in the aluminum melt and proceeding Stirring, so that the concentration unevenness caused by the difference in specific gravity between aluminum and lithium can be prevented, and lithium can be uniformly dispersed in the aluminum melt. Further, since 坩^ 12 is made of graphite, aluminum containing lithium can be prevented. The impact of the molten metal on the ruthenium 12 can suppress the formation of a lithium-containing compound. Here, the A1-Li alloy used as a target for sputtering is obtained from the viewpoints of plastic working and film formation properties at the time of use. It is preferred to use a single phase. The so-called AKi alloy consisting of a single phase refers to the solid solution of the A1 element and the L and i bismuth. If the alloy structure becomes multi-phase, the composition of the added element is knives (/ The knives of the knives are larger, and the plastic workability is lowered. In addition, the presence of a mixture of two phases having different specific resistances results in an abnormal discharge due to a resistance distribution on the surface of the leather material, and film formation cannot be achieved. The stability of the rate and the uniformity of the film thickness distribution. 320103 14 200912021 In order to obtain the A1 -L i alloy leather material for the money plating composed of the single phase of I Lu, the amount of lithium added is based on the total composition of the alloy, to 3 Below weight% is preferred In the present embodiment, the amount of lithium block 22 added is 3% or less of the total weight of the aluminum block 21, the case 23, the wire 24, and the block 22. The third figure shows the pattern a 1 -L i Balance state diagram (from BINARY ALLOY PHASE DIAGRAMS) Second Edition TB Massalski, ASM INTERNATIONAL ISBN: Q-8717〇-4〇4-8) The maximum solidification limit of lithium relative to aluminum is 596〇c, 4 % by weight. However, the maximum solid solution limit of lithium decreases along the melting curve as the temperature decreases. Therefore, the amount of lithium added above the maximum solid limit cannot prevent AlLi (3 phase) from precipitating during solidification. To the aluminum phase. In the present embodiment, the amount of lithium added is reduced to 3% by weight or less, and the material is fed at a cooling rate of a certain temperature or more as described later, thereby producing a (four) single-phase Al-Li alloy. Happy. (Step 3) Next, the step of washing the casting mold 25 of the A1-U alloy in the catastrophe 12 is carried out (Fig. 2, in this step, the movable volume is written] ” The rotating shaft 18 is rotated in a counterclockwise direction, whereby the melt 2 is cast into the mold 25 by way of example 12. The cold is too cold = the inside of the cooling plate 26 of the mold 25. Therefore, flowing out from the hanging: w S gold The melt 20 is solidified in the mold 25 at a certain cooling rate, whereby the P ^ square stops the crystallization of the ruthenium due to the excess of the clock and the hunger phase, and the aluminum single phase can be maintained after curing. . In the embodiment of the present invention, the "return to the true" environment dissolves the dragon 320103 15 200912021 in the k 仃 aluminum melting, lithium addition, melting, washing and other consistent operations, α can know lithium oxide, nitride or hydrogen Foreign matter such as oxides is extremely Al-Li alloy. (Step 4) Next, the structure control of the obtained A1_u alloy ingot was performed. The ingot tissue control system includes a forging step including a light-drying process or a drawing process for processing into a desired dry material shape to remove internal stress and adjust the crystal structure. ^Steps The process temperature here is set to 55 generations or less. This system, because it is below the limit, the alloy structure is a single-phase, and also the difference between the clothing and the degree of the clothing, so that the cold phase is due to the subsequent plastic processing, and the second:: there is a precipitation. For example, even below the eutectic point, there is a case where the eutectic line (eutectic temperature) is locally exceeded due to the uniformity of the heating furnace or the overheating of the processed portion. If Wanxiang
Urx/ =作為靶材使用時會構成電壓上升、產生發弧 因§)#異常放電之原因，而導致成膜率之參差不齊。 产織化=^形％中，係考慮到步驟進行時之數十度溫 二：入* 乂程溫度之上限設定為55〇。。以下，以避免靶 材之合金組織之多相化。 藉由以上方式，製造本發明之以七合金 本實施形態之A卜u合金乾材，㈣m 據 Q孟靶材即可獲得異物及夾雜物含 /，、、且成分布均—（例如土5¾以内）之鋁單一相組織。因 可抑制在騎成膜時異常放電之產生， 之安定化與膜厚分布之均—化。 X成膜羊 320103 16 200912021 [實施例] (實施例1) 使用參照第1圖所說明之熔解爐1〇製作ApLi合金鑄 疑。銘塊21係使mQmm平方之桿狀高純度^純度 99. 99%)。作為收容經塊22之箱體23，則準備將上述高純 度L行幸昆軋力u工作成厚U2mm之銘箱。鐘塊22係使用 直徑10mm Φ之桿狀鋰（本城金屬公司製，純度99⑽）。 坩禍12係使用壓縮石墨製坩堝。坩堝&之形^係為 有底圓筒形，如第4圖所示’係使用内徑175mm卜深产 3〇〇·者。將高純度銘7, 750g安置於此坩堝，在將熔解= 内之麗力減職之後，藉由感應加熱（麵） 將掛禍加熱到7 5 0 °C而將高純度銘溶解。 在此，熔融鋁之溫度監控係如第4圖所示，使用裝入 於設置在坩堝12中之高純度石墨製之熱電偶保護管如之 CA鞘套型（sheath)熱電偶。保護管3〇係使用外形為長 15mm、寬15_、高310mm，内徑為4ππηφ，而深度為3〇〇mm 者。 以厚度0· 2mm之向純度銘箔將3重量％之鐘包覆2層， 且用高純度鋁線（99· 99«綁緊固定在位於坩堝上部之插塞 13之前端部13 A。在坩堝之開口部係設置石墨製之熱遮蔽 板19，且在添加鋰之前係將坩堝開口部打開。 在銘熔液溫度為750T：之情況下，亦將爐内壓力維持 於1.33xl(T2pa。接著，在此溫度下將熱遮蔽板去除並將坩 堝開口部打開之後，迅速移動插塞並強制使保持在插塞前 320103 17 200912021 端部之鋰塊浸潰於鋁熔液，進行丨分鐘攪拌。之後，停止 坩堝之感應加熱，且於大約.70(TC下，將合金熔液從坩堝 朝鑄模（内徑260ππηφ、高度60mm)進行澆鑄，而獲得圓板 狀之銘-鐘合金溶液。 如第5圖所示，分別從所獲得之鑄錠之頂部與底部之 中心起距離20mm内側之部位（a點、]3點）、及從該鑄錠之 側面之高度方向中央部起距離5mm内側之部位（c點）採集 樣本，且藉由ICP-AES(高頻電漿發光分光分析）法進行鋰 之組成分析。分析結果為：在a點為3. 08重量％、b點為 2. 90重量％、c點為3. 02重量％，均在3 〇重量％±5%以内。 取樣後之鑄錠經進行衝壓鍛造與輥軋加工，獲得可加 工到厚度15mm而不會破裂、厚度i2mm、直徑2〇〇_公之濺 鍍靶材。衝壓鍛造之製程溫度係設為55(rc，於熱處理後 進行輥軋，且在45(TC下進行最終熱處理。藉由銦系焊材 將其接合於銅製冷卻板（背板（backing plate))，且將其安 置於濺鍍裝置，在減壓氬氣體環境〇. 9Pa、lkW2 Dc濺鍍 條件下進行1小時濺鍍處理。濺鍍時，異常放電現象未出 現，過程很穩定。 之後，將靶材從裝置中卸下，且進行該靶材之表面觀 察、將該靶材作十字切割之剖面觀察及該剖面之組成分 析。表面觀察及剖面觀察係使用倍率5〇倍之ccd放大鏡。 濺鍍後之靶材表面，整個表面皆未觀察到凹陷、突出、膨 脹等，相當平滑。作十字切割之整個剖面區域亦未觀察到 空隙（vend)等。在十字剖面之厚度中央部中，係藉由以下 320103 18 200912021 方式從：當於編周冑、中間部、中心部之部分 本’且藉由抓AES料行^組成分析。樣 (測定之結果） 外周。IM個位置：3. Q8重量％、2. 98重 量％、2.86重量％ .抑重 中間部4個位置 量％、2. 86重量％ 3.02 重量 ％、2.96 重量 ％、3.〇〇 重 中心部1個位置：2.88重量％ 總計9個位置，在“重量紐％以内。 此外為了觀察组織，而從十字剖面之組成分析用試 料之抓术位置附近外周部2個位置、中間部2個位置、中 1個4立置進行取樣。從A卜Li合金之組織觀察結果， 可碟認到皆為鐘时於銘之狀態之料一相。 (實施例2) 除在氮氣環境下進行A卜Li合金化之熔解料，以與 實施例1同樣之方法製作Al-Li合金靶材。 、 —使炼解爐内之壓力設為133xl()-2pa將㈣内之㈣ 融鋁熔液之度在750°C中，於一耳將爐内壓力減壓至 2. 66Pa之後’將高純度銘氬氣（純度99. 、露點溫度一 C以下）導人至爐内，而作成在氬氣環境下之壓力6.66χ 104Pa之減壓狀態。接著在此温度下打開坩堝之蓋(熱遮蔽 板），使插塞下降而強制使鋰塊浸潰於鋁熔液内，進行i 分鐘擾拌。在㈣之感應加熱停止後，料於内徑26〇随 φ、尚度60mm之鑄模内，並進行冷卻固化，而獲得a卜 320103 19. 200912021 :孟轉旋°以後之步驟係以與實施例1同樣方式，而獲得 旱度12mm、直锉20〇_0之濺鍍靶材。 針對所獲得之賤鍍乾材進行與實施例1相同之賤鍍測 與組成分析。可進行濺鍍且無異常放電，而鋰之組成分 $結果料3.0重量％±5%以内。此外，從十字剖面之組成 刀析用4料之採集位置附近之外周部2個位置、中間部2 個位置、中心部1個位置進行取樣而進行組織觀察之結 果可確遂到皆為與實施例i相同之裡固溶於紹之狀態之 !呂單一相。 (實施例3) 示將鑄模之形狀设為寬度22〇mm、長度5〇〇mm、深度 25mm以外’其餘均以與上述實施例2相同之方法製作mi 合金鑄錠。之後，將表面切削，進行衝壓鍛造、輥軋加工， 製作出厚度l〇mm、長度1〇〇〇mm之鑄錠，而不會產生破裂。 此外，加工成厚度8mm、直徑2〇〇ιηιηφ之濺鍍靶材形狀，進 行與實施例1相同之錢鍍測試與組成分析。可進行濺鍍且 無異常放電，鐘之組成分析結果亦為3 〇重量％±5%以内。 此外，從十字剖面之組成分析用試料之採集位置附近之外 周部2個位置、中間部2個位置、中心部丄個位置取樣而 進行組織觀察之結果，與實施例i相同，可確認到皆為鋰 固熔於鋁之狀態之鋁單一相。 (比較例1) 在1 000 C使用加熱用大氣加熱爐（電爐），將高純度鋁 7, 〇〇〇克安置於氧化鎂製坩堝（内徑175ππηφ、深度 320103 20 200912021 随），且於大氣中藉由加熱使之溶解。以氧化紹板將表 面所產生之链之氧化物去除，且與實施例i同樣將由銘箱 所包覆之預定量之鋰迅速投入於鋁熔液内。投入物之一部 分係在溶液表面浮游成為氧化物。在㈣表面浮游之氧化 物（熔渣）係以氧化鋁板去除。 將掛禍内之A卜Li合金炫液洗鑄於内徑26〇随少 度6〇随之鑄模並進行冷卻，而獲得Ai-Li合金鱗錠。分別 ㈣軸之高度方向之頂部與底部之中心起輯2〇職内 ^之》ίΜ立（第5圖之a點、b ,點）、及從該鎊錠之側面之高 j向中央部起距離5·内側之部位（第5圖之c點）採集 、且藉由ICP-AES(尚頻電漿發光分光分析)法進行鋰 之:且2析。分析結果為：在a點為2·82重量%、b點為 56重㈣、C點為2.98重量％，最大為3·〇重量％的一15%。 將取樣後之鑄錠進行衝壓锻造與減加工，加工到厚 I151"。雖作成厚度—、直徑丽必之減鍍乾材，惟 2表面觀察時可觀察到異物、空隙。在將此蘭乾材作 ::切割並進行剖面觀察結果，也在剖面部觀察到異物、 二隙，而無法作為成膜用濺鍍靶材來使用。 (比較例2) 藉由真空感應加熱爐在氬氣環境下進行Μ '^ ^ ^厂疋1丁 Λ丄_乙1合金 溶解。將4重量％之鐘以厚度〇 2_之高純度㈣包覆 2且以在插塞之前端(參照第1圖)藉振動就會立刻脫 :方式簡單地以鋁線輕輕地固定吊掛在坩堝上部。至於 3金化之條件係與實施例2同樣進行，㈣之添加係將 320103 21 200912021 7之蓋打開，輕輕地振動插塞，而使由㈣包覆的裡塊掉 洛至魅溶液面。 ， 在緩慢旋轉之鋁熔液面可觀察到類似氧化物之浮游 物。在停止感應加熱後，洗鑄於内徑26〇_、高度6〇麵 之㈣並進行冷卻，而獲得AKi合金缚旋。分別從該鱗 錠之^度方向之頂部與底部之中心起距離2〇賴内側之部 位（第5圖之a點、b點）、及從該禱旋之側面之高度方向 中央部起輯5mm内側之部位（第5圖之〇點）採集樣本， 且藉由ICP-AES(高頻電聚發光分光分析）法進行鐘之挺成 ^斤。分析結果為：在a點為3. 〇2重量％、b點為2. Μ重 量％、c點為2.90重量％，在3.0重量％±5%以内。 以後之步雜係以與實施例i相同方式進行而獲得厚度 12咖、直徑2__之濺鍍然後，進行與實施例工 相同之濺鑛測試與組成分析。在}小時之_測試中產生 了 5次異常放電。又進行濺鏟測試後之乾材表面觀察、作 十字切割之剖面觀察、組成分析。在表面經轉認到有可部 為是異常放電時所產生之突出狀，進一步在全面確認到有 13處大们随之孔穴或凹陷。此外，在剖面觀察中亦觀察 到可認為是捲入氧化物之一部分而固化之許多個空隙等。 再者j從、组成分析用試料之採集位置附近之外周部2個位 ，、+間部2個位置、中心部j個位置進行取樣而觀察組 ，’、之結果’可確認為係屬於㈣溶於㉟之狀態之由紹相與 A1U相（石相）所構成之2相。 以上雖說明了本發明之實施形態及實施例，惟本發明 320103 22 200912021 亦可根據本發明之When used as a target, Urx/= will cause voltage rise and arcing due to §)# abnormal discharge, resulting in uneven film formation rates. In the production weaving = ^ shape %, taking into account the tens of degrees of temperature when the step is performed. The upper limit of the process temperature is set to 55 〇. . The following is to avoid the heterogeneity of the alloy structure of the target. By the above method, the A-u alloy dry material of the present embodiment of the present invention is produced, and (4) m according to the Q-Meng target material, foreign matter and inclusions can be obtained, and the distribution is uniform (for example, soil 53⁄4) Within the aluminum single phase organization. Since it is possible to suppress the occurrence of abnormal discharge during riding film formation, the stabilization and film thickness distribution are uniform. X-formed sheep 320103 16 200912021 [Examples] (Example 1) An ApLi alloy was cast by using a melting furnace 1 described with reference to Fig. 1 . The ingot block 21 is a rod-shaped high purity of mQmm squared purity 99. 99%). As the casing 23 for accommodating the block 22, it is prepared to operate the above-mentioned high-purity L-fortunate rolling force u into a U2 mm thick box. For the clock block 22, rod-shaped lithium having a diameter of 10 mm Φ (manufactured by City Metal Co., Ltd., purity 99 (10)) was used. The 12 series is made of compressed graphite. The shape of the 坩埚& is a bottomed cylindrical shape, as shown in Fig. 4, which uses an inner diameter of 175 mm and a deep production of 3 〇〇. Place the high-purity Ming 7, 750g in this 坩埚, and after the melting = the inside of Lili, reduce the high-purity by heating the heat to 750 °C by induction heating (face). Here, the temperature monitoring of the molten aluminum is as shown in Fig. 4, using a thermocouple protection tube such as a CA sheath thermocouple incorporated in high purity graphite provided in the crucible 12. The protective tube 3 is a shape having a length of 15 mm, a width of 15 mm, a height of 310 mm, an inner diameter of 4ππηφ, and a depth of 3 mm. A 3 wt% bell is coated with 2 layers of a purity of 0·2 mm, and a high-purity aluminum wire (99·99« is fastened to the front end 13 A of the plug 13 located at the upper portion of the crucible. The opening of the crucible is provided with a heat shield plate 19 made of graphite, and the opening of the crucible is opened before the addition of lithium. In the case where the temperature of the melt is 750 T:, the pressure in the furnace is also maintained at 1.33 x 1 (T2pa). Then, after the heat shielding plate is removed at this temperature and the opening of the crucible is opened, the plug is quickly moved and the lithium block held at the end of the plug 320103 17 200912021 is forced to be immersed in the aluminum melt for a minute of stirring. After that, the induction heating of the crucible is stopped, and at about .70 (TC, the alloy melt is cast from the crucible toward the mold (inner diameter 260ππηφ, height 60 mm) to obtain a disk-shaped inscription-bell alloy solution. As shown in Fig. 5, the distance from the center of the top of the obtained ingot to the center of the bottom of the ingot is 20 mm (a point, 3 points), and the distance from the center of the side surface of the ingot to the inside of the height of 5 mm. The part (point c) collects the sample and uses the IC重量重量。 The P-AES (high-frequency plasma luminescence spectrometry) method for the analysis of the composition of the lithium. The analysis results are: at a point of 3. 08% by weight, b point is 2. 90% by weight, c point is 3. 02% by weight , all within 3 〇% by weight ± 5%. After sampling, the ingot is subjected to stamping forging and rolling, and can be processed to a thickness of 15mm without cracking, thickness i2mm, diameter 2〇〇_gong sputtering target The process temperature of stamping forging is set to 55 (rc, rolling after heat treatment, and final heat treatment at 45 (TC). It is bonded to a copper cooling plate (backing plate) by indium-based welding consumables. )), and placed in a sputtering device, under a reduced pressure argon atmosphere 〇. 9Pa, lkW2 Dc sputtering conditions for 1 hour sputtering treatment. During sputtering, abnormal discharge phenomenon did not occur, the process is stable. The target is removed from the device, and the surface of the target is observed, the cross-section of the target is cross-cut and the composition of the cross-section is analyzed. The surface observation and the cross-section observation are ccd magnifiers with a magnification of 5 times. The surface of the target after sputtering, no concave is observed on the entire surface , protrusion, expansion, etc., is quite smooth. No cross-sections have been observed in the entire cross-sectional area of the cross-cut. In the central part of the thickness of the cross-section, the following is the way from the following 320103 18 200912021: Part of the middle part, the center part, and the composition of the AES material line. The sample (measurement result) outer circumference. IM positions: 3. Q8 wt%, 2.98 wt%, 2.86 wt%. 4 positions in the middle of the heavy portion, 2.86 wt% 3.02 wt%, 2.96 wt%, 3. One center position of the weight center: 2.88 wt% A total of 9 positions, within the weight %. Further, in order to observe the tissue, the composition of the cross-section analysis was sampled at two positions in the outer peripheral portion near the grasping position of the sample, two positions in the middle portion, and one in the middle. Observed from the structure of the A-Li alloy, it can be recognized as a material in the state of the clock. (Example 2) An Al-Li alloy target was produced in the same manner as in Example 1 except that the molten material of Ab Li alloying was subjected to a nitrogen atmosphere. —————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————————— Purity argon gas (purity 99., dew point temperature below C) is introduced into the furnace to produce a reduced pressure of 6.66 χ 104 Pa under an argon atmosphere. Then, the lid (heat shield) was opened at this temperature, and the plug was lowered to force the lithium block to be immersed in the aluminum melt for 1 minute. After the induction heating of (4) is stopped, it is prepared in a mold with an inner diameter of 26 φ and a φ degree of 60 mm, and is cooled and solidified to obtain ab 320103 19. 200912021: the steps after the rpm are the same as the examples. 1 In the same way, a sputter target with a dryness of 12 mm and a diameter of 20 〇 _0 was obtained. The same ruthenium plating and composition analysis as in Example 1 was carried out for the obtained ruthenium plating dry material. It can be sputtered without abnormal discharge, and the composition of lithium is within 3.0% by weight ± 5% of the result. In addition, from the cross-section of the cross-section, the results of the tissue observation at two positions in the vicinity of the collection position of the four materials, the two positions in the middle portion, and one position in the center portion can be confirmed and implemented. Example i is the same in the same state as the solid state! Lu single phase. (Example 3) A mi alloy ingot was produced in the same manner as in the above Example 2 except that the shape of the mold was set to have a width of 22 mm, a length of 5 mm, and a depth of 25 mm. Thereafter, the surface was cut, and press forging and rolling were performed to produce an ingot having a thickness of 10 mm and a length of 1 mm without causing cracking. Further, the shape of the sputtering target having a thickness of 8 mm and a diameter of 2 〇〇 ηηηηφ was processed, and the same money plating test and composition analysis as in Example 1 were carried out. It can be sputtered without abnormal discharge, and the composition analysis result of the clock is also within 3 〇%%±5%. In addition, from the vicinity of the collection position of the analysis sample of the cross-section, the results of the tissue observation at two positions in the peripheral portion, the two positions in the middle portion, and the center portion are sampled, and the results are confirmed in the same manner as in the example i. A single phase of aluminum that is solidified in the state of aluminum. (Comparative Example 1) Using a heating furnace (electric furnace) for heating at 1 000 C, high-purity aluminum 7 and gram were placed in a magnesite made of magnesium oxide (inner diameter 175ππηφ, depth 320103 20 200912021), and in the atmosphere. It is dissolved by heating. The oxide of the chain generated by the surface was removed by oxidation of the plate, and a predetermined amount of lithium coated by the name box was quickly introduced into the aluminum melt in the same manner as in the example i. A portion of the input floats on the surface of the solution to form an oxide. The oxide (slag) floating on the surface of (4) is removed by an alumina plate. The A-Li alloy in the accident was washed and cast into an inner diameter of 26 〇 with a minimum of 6 〇 and then molded and cooled to obtain an Ai-Li alloy scale. (4) The center of the top and bottom of the height direction of the axis (2) The position of the ^ 内 》 ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( Lithium was collected from the inner portion (point c in Fig. 5) and was analyzed by ICP-AES (still frequency plasma spectroscopy). The analysis results were: 2·82% by weight at point a, 56 weight (four) at point b, 2.98 wt% at point C, and a maximum of 15% by weight of 3·〇. The sampled ingot is subjected to stamping forging and subtraction processing to a thickness of I151". Although it is made into a thickness--diameter-reduced dry-plated dry material, only foreign matter and voids can be observed when the surface is observed. As a result of observation of the cross section of the dried lime material, the foreign matter and the two gaps were observed in the cross section, and it was not used as a sputtering target for film formation. (Comparative Example 2) The Μ '^ ^ ^ 疋 1 Λ丄 乙 _ _ 1 alloy was dissolved in an argon atmosphere by a vacuum induction heating furnace. 4% by weight of the bell is coated with a high purity (4) of thickness 〇2_2 and is immediately removed by vibration at the front end of the plug (refer to Fig. 1): the method is simply hanged with aluminum wire In the upper part. As for the conditions of the 3 golding, the same conditions as in the second embodiment are carried out. The addition of (4) is to open the cover of 320103 21 200912021 7 and gently vibrate the plug, so that the inner block covered by the (4) is dropped to the surface of the charm solution. An oxide-like float can be observed on the slowly rotating aluminum melt. After the induction heating was stopped, the inner diameter of 26 〇 and the height of 6 〇 (4) were washed and cooled to obtain an AKa alloy. The distance from the top of the scale to the center of the bottom of the scale is 2, the inner side (the a point and the b point in Fig. 5), and the center from the height side of the side of the prayer is 5 mm. The inner part (the point of Fig. 5) collects the sample, and the ICP-AES (high-frequency electro-polymerization luminescence spectroscopic analysis) method is used to carry out the test. The analysis results were as follows: a point of 3. 〇 2% by weight, and point b was 2. Μ by weight %, c point was 2.90% by weight, and within 3.0% by weight ± 5%. Subsequent steps were carried out in the same manner as in Example i to obtain a sputtering thickness of 12 coffees and a diameter of 2 mm, and then the same sputtering test and composition analysis as in the example work were carried out. Five abnormal discharges occurred during the hourly test. The surface of the dry material after the spatter shovel test was observed, the cross-section of the cross-cut was observed, and the composition analysis was performed. When the surface was recognized to have a protrusion that was generated when the part was abnormally discharged, it was further confirmed that there were 13 places with holes or depressions. Further, in the cross-sectional observation, many voids and the like which can be considered to be entrapped in one part of the oxide are observed. In addition, j is sampled and observed in two places in the vicinity of the collection position of the analysis sample, and two positions in the middle portion and the j position in the center portion, and the result of ', can be confirmed as belonging to (4) It is dissolved in the state of 35 and consists of two phases consisting of the A1U phase (stone phase). The embodiments and examples of the present invention have been described above, but the present invention 320103 22 200912021 may also be in accordance with the present invention.
下在坩堝内進行鋁之熔解，惟不限於此，亦可 性氣體環境下進行鋁之熔解。 亞、、月 當然不限定於該等實施形態及實施例， 技術思想作各種變更。 此外，在以上實施形態中，雖係將冷卻板26與模框 27組合來構成鑄模25,惟亦可使用將冷卻板26與模框π 一體形成之鑄模。 【圖式簡單說明】 第1圖係為顯示在本發明實施形態中所使用之熔解爐 之概略構成之側剖面圖。 =弟2圖A至c係為模式性顯示在本發明實施形態中所 說明之鋰合金化步驟與澆鑄步驟之主要部分剖面圖。 第3圖係為A1 —L i系平衡狀態圖。 ，第4圖A及B係為顯示在本發明實施例中所使用之石 墨衣坩堝之構成之平面圖及側剖面圖。 第5圖係為顯示在本發明實施例之A1_Li合金鑄錠之 組成分析用樣本採集位置圖。 【主要元件符號說明】 可動容器 熔解爐 11 c 排氣埠 12 A 唇部 13 插塞 14 备令 11 真空槽 12 坩堝 12Β 支撐棒 13Α 前端部 15 線圈 23 320103 200912021 16 保持構件 17 基座構件 18 轉動軸 19 熱遮蔽板 20 A1-Li合金溶液 21 鋁塊 22 裡塊 23 箱體 24 線材 25 鑄模 26 冷卻板 27 模框 28 $炭片 30 保護管 24 320103The melting of aluminum is carried out in the crucible, but it is not limited thereto, and the melting of aluminum can also be carried out in a gas atmosphere. It is of course not limited to these embodiments and examples, and various changes are made in the technical idea. Further, in the above embodiment, the mold 25 is formed by combining the cooling plate 26 and the mold frame 27. However, a mold in which the cooling plate 26 and the mold frame π are integrally formed may be used. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a side cross-sectional view showing a schematic configuration of a melting furnace used in an embodiment of the present invention. Fig. A to c are schematic cross-sectional views showing principal parts of the lithium alloying step and the casting step described in the embodiment of the present invention. Figure 3 is a diagram of the equilibrium state of the A1 - L i system. 4 and A are plan views and side cross-sectional views showing the constitution of the graphite enamel used in the embodiment of the present invention. Fig. 5 is a view showing a sample collection position for composition analysis of an A1_Li alloy ingot according to an embodiment of the present invention. [Main component symbol description] Movable container melting furnace 11 c Exhaust 埠 12 A Lip 13 Plug 14 Preparation 11 Vacuum chamber 12 坩埚 12 Β Support rod 13 Α Front end portion 15 Coil 23 320103 200912021 16 Holding member 17 Base member 18 Rotating Shaft 19 Heat shield plate 20 A1-Li alloy solution 21 Aluminum block 22 Inner block 23 Box 24 Wire 25 Mold 26 Cooling plate 27 Mold frame 28 Charcoal sheet 30 Protection tube 24 320103