476797 A7 B7 五、發明説明（1 ) 發明所屬的頜域 * (請先閱讀背面之注意事項再填寫本頁) 本發明係有關鋁或鋁合金所成濺潑靶材料（以下稱作 A 1或A 1合金濺潑靶材料）及其製造方法。尤指有關半 導體用電極膜形成用之A 1或A 1合金濺潑靶材料及其製 造方法，其中亦係有關用作液晶顯示器之電極（薄膜狀的 配線及電極本身）適當的半導體用電極膜之形成用的A 1 或A 1合金濺潑靶材料及其製造方法。 先前技術 經濟部智慧財產局員工消費合作社印製 液晶顯示器（Liquid Crystal Display，以下簡稱L C D )’與習用的影像管相比、可謀薄型化、輕量化、低消耗 電功化，而且可得高解析度之影像，故近年來其用途正擴 大中。至於相關的L C D，在最近爲更提高影像品賓，於 L C D內部以組合用作開關元件之半導體裝置之薄膜電晶 體（Thin Film Transistor以下簡稱T F T )的構造之 L CD被提出，且正被廣泛的使用著。在此，TFT係指 於已予形成玻璃等的絕緣基片上的半導體薄膜上連接由薄 膜狀金屬而成的半導體用電極而成的主動元件。而半導體 用電極，係被使用作T F T之一部分的電極，定義成含有 薄膜狀的配線及電極本身者（以下亦同）。且，於成爲 T F T之狀態配線及電極本身係經予電氣連接的。 於上述L C D所使用的半導體用電極所被要求的特性 雖有各種，惟尤其隨著近年的L C D之大型化或高精細化 之動向，爲防止信號之遲緩、低比電阻化乃正成爲最重要 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐）-4 - 476797 A7 B7 五、發明説明（2 ) 的要求特性。 (請先閱讀背面之注意事項再填寫本頁) 上述L C D用的半導體用電極之形成係藉由濺潑法而 進行，於進行此濺潑之際，可採用濺潑靶材料。此濺潑靶 #料，係利用濺潑方式於基片上形成半導體用電極而用的 _潑源者，通常爲圓盤狀或平板狀的板材。於濺潑之際， _予加速的粒子衝撞濺潑靶材料表面時，藉由運動量之交 $構成濺潑靶材料之原子會被釋放入空間而堆積於對向的 基片上。 經濟部智慧財產局員工消費合作社印製 至於供形成相關的L C D用半導體用電極而用的濺潑 靶材料，向來係以Ta、Mo、Cr、Ti、W、Zr、 Mb等高熔點金屬被使用者。然而，隨著日昨的的LS I 高積體化，電路之配線寬度正予微細化至成1 # m以下， Ta、Mo、Cr、Ti、W、Zr、Nb 等的高熔點金 屬係薄膜形狀之比電阻値較大之故，適用上乃形成困難。 亦即，如上述般採用由高熔點金屬而成的濺潑靶材料所形 成的半導體用電極材料係比電阻値大，因此較難獲得對應 於上述配線寬度之微細化。於是，取代上述高熔點金屬之 低比電阻的半導體用電極材料之開發乃爲人所期待的。 至於相關的低比電阻之半導體用電極材料，可舉出 Au、 Cu及A1 。然而，Au爲板片狀電極，亦即在電 極膜（配線膜等片成膜後作成指定圖形形狀時所需的蝕刻 特性低劣，且價昂，又C u則於膜之附著性及耐蝕性方面 有問題存在。另一方面，A 1因耐熱性並不足夠’故於 丁 F T製程上不可避免的電極膜形成後之加熱步驟（ 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐1 476797 經濟部智慧財產局員工消費合作社印製 A7 _B7_五、發明説明（3 ) 2 5 0〜4 0 0 °C左右）則有所謂小丘（hillock )之微小 的凸凹係於表面生成之問題點存在。通常在T F T -L CD，電極層係成爲最下層之故，若發生相關的小丘時 ，則於其上未能層合膜，故有進展上惡劣的問題。 至於此種電極膜上的發生小丘問題之迴避對策，例如 已予提出有由日本特開平7 — 4 5 5 5 5號公報（申請國 ••日本、申請曰：1993年7月27曰、公開日·· 1 9 9 5年2月14日）所記載的合金成分之A 1合金而 成的電極膜，及相關的A 1合金電極膜之形成用的A 1合 金濺潑靶材料。然而採用由上述A 1或A 1合金而成的濺 潑靶材料，藉由濺潑方式於基片上形成半導體用電極之際 ，會發生粒子，又發生噴濺之問題。亦即，由靶材料飛濺 ____________________…---------------------------------- 的粒子會集束（cluster)化並直接附著於基片上的薄膜上 ，又或附著，堆積於周圍壁或組件上後予以剝離，而附著 於基片上之薄膜上的情形（亦即所謂的粒子）會引起，又 ，靶材料之液滴會飛濺而附著於基片上之薄膜的情形（亦 即所謂噴濺）會引起的問題點。 針對此種發生粒子及噴濺之問題點，藉由極.力.降J氏夾 w —一............... 雜於濺潑靶材料內的夾雜物之量，呈1前爲止雖極力圖謀 對應，惟例如於日本特開平9 一 2 5 5 ^4")號公報（申請 -.---....————一― __________一 國：日本、申請日：1995年7月6日、公開曰： 1 9 9 7年1月2 8日）爲減少粒子，需極力減少靶材料 中的夾雜物之數量的必要，具體而言，揭示有將平均直_徑 1 0 // m以上的夾雜物之存在量設'成未滿4 0個/ c m 2， 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） 7〇7 (請先閱讀背面I注意事項再填寫本頁) 訂 476797 A7 B7 經濟部智慧財產局員工消費合作社印製 五、發明説明（4 ) 惟在粒子及噴濺之發生的抑制方面仍有不足的問題存在。 於上述所謂的粒子及噴濺之發生的問題點之中，噴濺 之發生因對基片上之薄膜及其上所形成的半導體用電極之 性能會帶來重大的妨礙，故成爲較大的問題點。尤其，爲 防止在A 1電極膜上之小丘發生，於使用A 1合金濺潑靶 材料之情形，有較易發生噴濺的傾向，其消除乃爲人所期 待的。 相關的噴濺之發生，不僅如上述般L CD用的半導體 用電極之形成之情形，亦與採用A 1或A 1合金濺潑靶材 料利用濺潑方式形成半導體之積體電路配線、磁氣記錄、 光磁氣記錄媒體之反射層等的情形同樣的引起問題。‘ 發明之摘述 本發明之目的，係提供在濺潑之際較難引起噴濺之發 生的A 1或A 1合金濺潑靶材料，及其製造方法。 與本發明之合適實施例有關的濺潑材料，係內存的夾 雜物之最大長度全部在2 0 //m以下的A 1或A 1合金濺 一—_ -...... ..... 潑革G材„.料j | --------- 此時’在濺潑之際，可抑制噴濺之發生。在此內存的 夾雜物之最大長度全部在2 0 //m以下一事，係若有最大 長度超過2 〇 m之夾雜物時，則起因於此夾雜物容易引 起噴_之發生，抑制噴濺發生不足夠所致。 又’以濺潑靶材料之前述夾雜物之最大長度全部在 ΙΟί/m以下爲較合適。 (請先閱讀背面之注意事項再填寫本頁) 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐）· 7 - 476797 經濟部智慧財產局員工消費合作社印製 A 7 ___B7__五、發明説明（5 ) 此時，噴濺之發生極難引起，可較確實的抑制噴濺發 生。 又，與本發明之合適實施例有關的濺潑靶材料之製造 方法，係利用噴布形成法之A 1或A 1合金濺潑靶材料之 製造方法，於在前述噴布形成法之氣體霧化步驟的氣體流 出量（Nm3) /熔液流出量（kg)之値設爲5Nm3/ k g以上的製造方法。 此時，於在噴布形成法之氣體霧化步驟，A 1或A 1 合金之溶液係經予氣體霧化且成爲熔融狀或半熔融化之小 粒、同時夾雜物亦與破碎而變小。因此，此小粒狀的A 1 或A 1合金係半熔融狀，且於依序被噴布於底板上或模型 內等而堆積著，接著形成A 1或A 1合金濺潑靶材料。此 時，於在噴布形成法之氣體霧化步驟的氣體流出量（N m )/溶液流出量（k g )之値若設爲5 N m 3 / k g以上時 ，則經予破碎後的夾雜物之大小（最大長度）全部成爲 2 0 //m以下，因此可得內存的夾雜物之大小全部爲2 0 V m以下的A 1或A 1合金濺潑靶材料。 又，若將前述氣體流出量（N m 3 ) /熔液流出量（ k g )之値設爲1 〇 N m 3 / k g以上時，則可得內存的夾 雜物之大小（最大長度）全部爲1 〇 y m以下的A 1或 A 1合金濺潑靶材料。 再者，若採用氮氣作爲在前述氣體霧化步驟之霧化用 氣體時，同時將前述氣體流出量（N m 3 )/熔液流出量（ k g )之値設爲1 〇Nm3/k g以上時即較合適。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐）· 8 - (請先閱讀背面之注意事項再填寫本頁) 476797 A7 B7 五、發明説明（6 ) (請先閱讀背面之注意事項再填寫本頁) 此時’若內存的夾雜物之大小（最大長度）全部在 1 〇 A m以下時，同時可得氮氣濃度〇 · 1 m a s s % ( 質量％)之之A丨或六1合金濺潑材料。由而，於進行濺 潑之際’較難發生濺潑現象，又，可形成比電阻値較小的 A 1或a 1合金薄膜。 藍施例之說明 以下說明本發明之較佳實施形態之A 1或A 1合金濺 潑祀材料及其製法之實施形態。 本發明係爲開發出較難發生噴濺之A 1或A 1合金濺 潑革E材料而經精心硏究的結果，以所得的見解爲準而完成 者。 本發明人等，係製作出具有各種大小的夾雜物之A 1 縣潑靶材料及A 1合金濺潑靶材料，採用此等作爲濺潑靶 材料進行濺潑，詳細調查此等濺潑靶材料之濺潑時的狀況 〇 經濟部智慧財產局員工消費合作社印製 結果，噴濺係因於濺潑靶材料中內存的夾雜物之周圍 ’尤其於夾雜物之正上方、靶材料之冷却受部分阻礙而生 成的。亦即，於濺潑時各該位置係利用電漿的加熱予以熔 融’乃發現此熔融層受電磁力影響而飛散成液滴，又於噴 濺方面’夾雜物之尺度亦較上述日本特開平 9 - 2 5 5 6 4號公報記載的夾雜物之量需具有較大的相 關關係，再者，對夾雜物之大小（最大長度，亦即最大長 度部分之長度）在2 Ο μ m以下的情形，需可抑制噴濺之 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） 9 - 476797 A7 B7 五、發明説明（7 ) 發生，尤其在夾雜物之大小在1 〇 以下的情形，噴濺 幾乎並未生成。 (讀先閱讀背面之注意事項再填寫本頁) 亦即，內存的夾雜物之大小（最大長度）全部在2 0 以下之A 1濺潑靶材料及A 1合金濺潑靶材料，係於 進行濺潑之際由於夾雜物引起的冷却阻礙部分變小，熔融 層變成較難生成之故，熔融層之液滴的飛濺，亦即噴濺之 發生劇減，變成較難引起，可知噴濺發生之抑制需變成足 夠，尤其上述夾雜物之大小全部在1 〇 /i m以下的情形， 變成幾乎不發生噴濺現象。 其次，雖爲與本實施形態有關的A 1或A 1合金濺潑 靶材料之製造方法，惟採用A 1或A 1合金之熔液利用噴 布形成法製作鑄塊。亦即，將A 1或A 1合金之熔液予以 :氣體霧化並使堆積而得鑄塊。此時，於在噴布形成法之氣 〜·—. ______________— .·...〜一..一+ 體霧化步驟之氣體流出量（N m 3 ) /熔液流出量（k g ) —————^ -,w+-〜 …〜一 .·— -·*'·" J，.------------- .... 之値設爲5 N m 3 / k g以上。如此，則本實施形態之A 1 或A 1合金濺潑靶材料，亦即可得內存的夾雜物之最大長 、气今麗在2 0 // m以下的A I或A 1合金而成的濺潑靶材 經濟部智慧財產局員工消費合作社印製 料材料。於在噴布成形法的氣體霧化步驟之氣體流出量（ N m 3 ) /熔液流出量（k g )之値設爲5 N m 3 / k g以 上一事，係若未滿5 N m 3 / k g時，則所得的A 1或A 1 合金濺潑靶材料變成夾雜物存在有相當數最大長度超過 2 0 // m ’而相關的濺潑靶材料在進行濺潑之際有成爲噴 灘之發生起點的問題存在所致。 如上述，由噴布形成法而得的A 1或A 1合金濺潑靶 本紙張尺度適用中國國家標準（CNS ) A4規格（210 X 297公楚：）-10 - 476797 A7 B7_ 五、發明説明（8 ) (請先閱讀背面之注意事項再填寫本頁) 材料，與由真空熔解法等而得的A 1或A 1合金濺潑靶材 料相比，材料中的氧氣濃度較高。此爲前者與後者相比， 顯示出材料中的夾雜物大量存在的事實。儘管如此，在進 行濺潑之際前者與後者相比較難引起噴濺之發生。此爲前 者與後者相比，材料中的夾雜物之大小較小所致。亦即， 如同前者之情形，在夾雜物之大小較小的情形，即使夾雜 物之個數較多，其影響亦小，噴濺之發生較難引起所致， 後者之真空熔解法或大氣熔解法，終於會大量形成大小超 過2 0 之夾雜物，故乃成爲噴濺發生之起點。 經濟部智慧財產局員工消費合作社印製 但是，利用噴布形成法製造A 1或A 1合金濺潑靶材 料之際，於採用氮氣作爲噴布形成法之氣體霧化步驟的霧 化用氣體之情形，所得的A 1或A 1合金濺潑靶材料變成 氮氣濃度較高。採用相關的氮氣濃度較高的濺潑靶材料， 利用濺潑方式所形成的A 1電極膜等之A 1或A 1合金薄 膜，係氮氣濃度高，由於此氮氣之影響使比電阻値變大。 例如採用由A 1 — T i合金（含有T i之A 1合金）而成 的濺潑靶材料形成A 1合金薄膜之情形，如第7圖所示， 濺潑靶材料之N量愈高，則所形成的A 1合金薄膜之電阻 係數會變愈高。因此，若由期間的A 1或A 1合金薄膜之 比電阻値之點觀察，形成此薄膜所用的A 1或A 1合金濺 潑材料之氮氣濃度以較低者爲宜以〇 · 1 m a s s (質量 )%以下爲令人期待的。 作成0 · lma s s%以下一事，係有抑制由於氮氣 濃度之增加而引起的電阻係數之上升的意義，以與氮氣濃 本紙張尺度適用中國國家標準（CNS ) A4規格（210X29*7公釐1 . 11 ." 476797 A7 ______ B7_ 五、發明説明（9 ) 度0%之電阻係數相同者爲大受期盼的，爲滿足此點，乃 規定出上述界限値。 因此’於採甲多氣作爲在噴布形成法的氣體霧化步;驟 ^霧化i g體之彳青形應開發出可減少所得的A 1或A j _ 合 金濺潑靶材料之氮氣濃度的技術，尤指可減低至〇 . ]_ ____ ·... .... ·' — = / - " - ---- ···· - ·- m a s s %之技術，並進行精心硏究。其結果，於在噴布 形成法的氣體霧化步驟之氣體流出量（N m 3 )/熔液流出 量（k g )之値，亦即若將氮氣流出量（N m 3 ) /熔液流 出量（k g )之値設成1 〇 N m 3 / k g以上時，則可知可 得氮氣濃度在0 · 1 m a s s %以下之A 1或A 1合金濺 潑靶材料。 如此而得的A 1或A 1合金濺潑靶材料，因係以與前 述本實施形態之製造方法基本上同樣的構成之製造方法而 得者，故內存的夾雜物之大小（最大長度）全部在1 0 V m以下，因此於進行濺潑之際較難引起噴濺之發生。 經濟部智慧財產笱員工消費合作社印製 因此，利用噴布形成法製造A 1或A 1合金濺潑靶材 料之際於採用氮氣作爲在噴布成形法的氣體霧化步驟之霧 化用氣體之情形，若於此氣體霧化步驟之氣體流出量（N m 3 ) /熔液流出量（k g )之値設爲1 0 N m 3 / k g以 i:時，內存的夾雜物之大小（最大長度）全部在1 〇 /zm 以下時，同時可得氮濃度在〇 . Ima s s%以下在A 1 或A 1合金濺潑靶材料。若依相關的A 1或A 1合金濺潑 材料時，在進行濺潑之際較難引起噴濺之發生，又可形成 比電阻値較小的A 1或A 1合金薄膜。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） •12- 476797 A7 B7 五、發明説明（10 ) 如上述般於採用氮氣作爲在噴布形成法的氣體霧 驟之霧化用氣體的情形，、於氣體霧化步驟之氣體流出量（476797 A7 B7 V. Description of the invention (1) The jaw area to which the invention belongs * (Please read the notes on the back before filling out this page) This invention relates to splash target materials made of aluminum or aluminum alloy (hereinafter referred to as A 1 or A 1 alloy splash target material) and its manufacturing method. In particular, it relates to A 1 or A 1 alloy sputtering target materials for forming electrode films for semiconductors, and a method for manufacturing the same. It also relates to appropriate electrode films for semiconductors used as electrodes (thin-film wiring and electrodes themselves) of liquid crystal displays. A 1 or A 1 alloy sputtering target material for forming and its manufacturing method. In the past, the Intellectual Property Bureau staff of the Ministry of Technology and Economy printed liquid crystal displays (hereinafter referred to as LCDs) in consumer cooperatives. Compared with conventional video tubes, they can be made thinner, lighter, and have lower power consumption. Resolution image, so its use is expanding in recent years. As for the related LCD, recently, in order to improve the image quality, L CD with the structure of thin film transistor (hereinafter referred to as TFT) which is a semiconductor device used as a switching element in the LCD has been proposed, and is being widely used. Use it. Here, the TFT refers to an active device in which a semiconductor film made of a thin-film metal is connected to a semiconductor thin film formed on an insulating substrate such as glass. The semiconductor electrode is an electrode used as a part of T F T and is defined as a thin film-like wiring and the electrode itself (the same applies hereinafter). In addition, the wiring and the electrodes themselves are electrically connected in a state of T F T. Although there are various required characteristics of the electrodes for semiconductors used in the above LCDs, especially in recent years, with the trend of large-scale or high-definition LCDs, it is becoming most important to prevent signal delay and low specific resistance. This paper size applies to the Chinese National Standard (CNS) A4 specification (210X297 mm)-4-476797 A7 B7 5. The required characteristics of the invention description (2). (Please read the precautions on the back before filling in this page.) The formation of the above-mentioned semiconductor electrodes for L C D is performed by the sputtering method, and sputtering targets can be used for this sputtering. The sputtering target material is a sputtering source used to form a semiconductor electrode on a substrate by a sputtering method, and is usually a disc-shaped or plate-shaped plate. At the time of splashing, when the pre-accelerated particles collide with the surface of the splashing target material, the atoms constituting the splashing target material will be released into space and accumulated on the opposing substrate by the intersection of the amount of motion. For the sputtering target materials used to form relevant LCD semiconductor electrodes, the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs has always used high melting metals such as Ta, Mo, Cr, Ti, W, Zr, and Mb. By. However, with the increase of LS I, the wiring width of the circuit is being reduced to less than 1 # m. High melting point metal films such as Ta, Mo, Cr, Ti, W, Zr, Nb, etc. The shape has a large specific resistance 値, which makes it difficult to apply. That is, as described above, the electrode material for a semiconductor formed by using a sputtering target material made of a high-melting-point metal has a larger specific resistance than that of the resistor, and therefore it is difficult to obtain a miniaturization corresponding to the wiring width. Therefore, development of an electrode material for a semiconductor having a low specific resistance instead of the above-mentioned high melting point metal is expected. Examples of the relevant low-resistance electrode materials for semiconductors include Au, Cu, and A1. However, Au is a plate-like electrode, that is, the required etching characteristics when forming a specified pattern shape after forming a film such as an electrode film (wiring film) are inferior and expensive, and Cu has adhesion and corrosion resistance to the film. On the other hand, there is a problem. On the other hand, A 1 is not sufficiently heat resistant, so the heating step after the formation of the electrode film is inevitable in the DFT process (this paper size applies the Chinese National Standard (CNS) A4 specification (210X297) 1 476797 Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs A7 _B7_ V. Description of the invention (3) 2 50 ~ 4 0 0 ° C) There are so-called hillocks (micro-concave) formed on the surface There are problems. Usually in the case of TFT-L CD, the electrode layer becomes the lowest layer. If related hillocks occur, the film cannot be laminated thereon, so there is a problem of poor progress. The countermeasures against the occurrence of hillock problems on the electrode film have been proposed, for example, in Japanese Unexamined Patent Publication No. 7-4 5 5 5 5 (applicant country • Japan, application date: July 27, 1993, open date · · Recorded on February 14, 1959 Electrode film made of gold alloy A 1 alloy and related A 1 alloy sputtering target material for forming A 1 alloy electrode film. However, the sputtering target material made of the above A 1 or A 1 alloy is used, When a semiconductor electrode is formed on a substrate by a sputtering method, particles may be generated and a problem of sputtering may occur. That is, the target material is splashed ____________________...-------------- -------------------- The particles will be clustered and directly attached to the film on the substrate, or attached to the surrounding wall or component It will be peeled off, and it will be caused by the situation that it is attached to the film on the substrate (so-called particles), and that the droplet of the target material will be splashed and it will be caused by the situation that it is attached to the film on the substrate (so-called splashing). Aiming at the problems of such particles and splashing, the force of the J-clamp w is reduced by a force of one ............. It is mixed with the target material. Although the amount of inclusions in the contents is as high as 1 until the end of the attempt to cope, but for example, in Japanese Patent Application Laid-Open No. 9 1 2 5 5 ^ 4 ") (application -.---....——————- _____ _____ One country: Japan, application date: July 6, 1995, published: January 28, 1997) To reduce particles, it is necessary to reduce the number of inclusions in the target material as much as possible, specifically In terms of disclosure, it is revealed that the average amount of inclusions with an average diameter of more than 10 // m is set to be less than 40 pieces / cm 2. This paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm). ) 7〇7 (Please read the precautions on the back of the page before filling in this page) Order 476797 A7 B7 Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economy There are deficiencies. Among the above-mentioned problems of so-called particles and sputtering, the occurrence of sputtering becomes a major problem because it will cause a major obstacle to the performance of the thin film on the substrate and the semiconductor electrode formed thereon. point. In particular, in order to prevent hillocks on the A 1 electrode film, in the case where an A 1 alloy is used to sputter the target material, there is a tendency that spatter is more likely to occur, and its elimination is expected. The related spatters occur not only as described above for the formation of semiconductor electrodes for L CDs, but also for the formation of semiconductor integrated circuit wiring and magnetism by sputtering methods using A 1 or A 1 alloy sputtering target materials. Recording, reflective layers of magneto-optical recording media, etc. also cause problems. ‘Summary of the Invention The object of the present invention is to provide an A 1 or A 1 alloy sputtering target material which is less likely to cause splashing during splashing, and a method for manufacturing the same. The splashing material related to a suitable embodiment of the present invention is that the maximum length of the inclusions in the memory is all A 1 or A 1 alloy splashing below 2 0 // m. .. Splash leather G material „.j | --------- At this time, 'spattering can be suppressed during splashing. The maximum length of inclusions in this memory is all 20 / The matter below / m is that if there is an inclusion with a maximum length of more than 20m, it is because the inclusion easily causes the occurrence of spraying, and it is not sufficient to suppress the occurrence of spraying. It is more appropriate that the maximum length of the inclusions is below ΙΟί / m. (Please read the precautions on the back before filling in this page) This paper size applies the Chinese National Standard (CNS) A4 size (210X297 mm) · 7-476797 Economy Printed by the Consumers ’Cooperative of the Ministry of Intellectual Property Bureau A 7 ___B7__ 5. Description of the Invention (5) At this time, the occurrence of splashes is extremely difficult to cause, and the occurrence of splashes can be suppressed more reliably. It is also related to a suitable embodiment of the present invention. The manufacturing method of the sputtering target material is the sputtering method of A 1 or A 1 alloy using the spray forming method. The manufacturing method is a manufacturing method in which the gas outflow (Nm3) / melt outflow (kg) in the gas atomizing step of the aforementioned spray forming method is set to 5Nm3 / kg or more. In the gas atomization step of the method, the solution of the A 1 or A 1 alloy is atomized by gas and becomes molten or semi-melted pellets, and the inclusions are also broken and broken to become smaller. Therefore, the small granular A 1 Or the A 1 alloy is semi-melted, and is sprayed on the base plate or the mold in order to accumulate, and then A 1 or A 1 alloy splash target material is formed. At this time, in the spray forming method If the gas outflow (N m) / solution outflow (kg) of the gas atomization step is set to 5 N m 3 / kg or more, the size (maximum length) of the inclusions after the crushing will all become 2 0 // m or less, so the size of inclusions in the memory can be all A 1 or A 1 alloy splashing target material below 20 V m. In addition, if the aforementioned gas outflow (N m 3) / melt The size (maximum length) of the inclusions in the memory can be obtained when the flow rate (kg) is set to 1 〇N m 3 / kg or more. All of the A 1 or A 1 alloy splash target materials that are less than 10 μm. In addition, if nitrogen is used as the atomizing gas in the gas atomizing step, the gas outflow amount (N m 3) / Melt outflow (kg) is more appropriate when it is set to more than 10 Nm3 / kg. This paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm) · 8-(Please read the precautions on the back first Fill out this page again) 476797 A7 B7 V. Description of the invention (6) (Please read the precautions on the back before filling out this page) At this time 'If the size (maximum length) of the inclusions in the memory are all below 1 〇A m At the same time, A1 or six 1 alloy splash materials with nitrogen concentration of 0.1 mass% can be obtained. As a result, the sputtering phenomenon is less likely to occur during the sputtering, and an Al or a 1 alloy thin film having a smaller specific resistance 値 can be formed. Explanation of Blue Example The following describes the A 1 or A 1 alloy sputtering target material and the manufacturing method of the preferred embodiment of the present invention. The present invention is the result of careful research for the development of A 1 or A 1 alloy splash leather E material which is less likely to be splashed, and is based on the findings obtained. The present inventors have produced A 1 prefective sputtering target materials and A 1 alloy sputtering target materials with inclusions of various sizes, and used these as sputtering target materials for sputtering, and investigated these sputtering target materials in detail. The state of the splash. The result of printing by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs, the splash is caused by the surrounding of the inclusions in the target material, especially above the inclusions, and the cooling part of the target material. Generated by obstruction. That is, each position was melted by the heating of the plasma when it was splashed. It was found that the molten layer was scattered into droplets under the influence of electromagnetic force, and the size of the inclusions in the splashing was also larger than that of Japanese Patent Application Laid-Open No. 9 -The amount of inclusions described in JP 2 5 5 6 4 must have a large correlation. Furthermore, the size of the inclusions (the maximum length, that is, the length of the maximum length portion) is less than 20 μm. The size of this paper that can suppress the splatter is applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm) 9-476797 A7 B7 V. Description of the invention (7) Occurred, especially when the size of the inclusions is below 10 , The splatter was almost not generated. (Read the precautions on the back before you fill in this page.) That is, the size (maximum length) of inclusions in the memory are all below 20 A1 sputtering target material and A1 alloy sputtering target material. In the case of splashing, the part of the cooling hindrance caused by the inclusions becomes smaller, and the molten layer becomes more difficult to form. The splash of the droplets in the molten layer, that is, the occurrence of splashes, decreases sharply, and it is more difficult to cause the splashes. The suppression needs to be sufficient, especially when the size of the above-mentioned inclusions is all 10 / im or less, and there is almost no spatter. Next, although it is a method for manufacturing an A 1 or A 1 alloy sputtering target material related to this embodiment, an ingot is produced by a spray forming method using a melt of the A 1 or A 1 alloy. That is, the molten metal of A 1 or A 1 alloy is gas atomized and deposited to obtain an ingot. At this time, the gas in the spray forming method ~ · —. ______________— ..... ~ 一 .. 一 + gas outflow (N m 3) / melt outflow (kg) in the body atomization step — ———— ^-, w +-~… ~ 一. · —-· * '· &Quot; J ， .------------- .... The 値 is set to 5 N m 3 / kg or more. In this way, if the target material of A 1 or A 1 alloy is splashed in this embodiment, the maximum length of the inclusions in the memory and the splash of AI or A 1 alloy below 20 0 m can be obtained. Spill targets Print materials for cooperatives of employees of the Intellectual Property Bureau of the Ministry of Economic Affairs. The gas outflow (N m 3) / melt outflow (kg) in the gas atomization step of the spray forming method is set to 5 N m 3 / kg or more, if it is less than 5 N m 3 / When kg, the obtained A 1 or A 1 alloy splash target material becomes inclusions and there is a considerable amount of maximum length exceeding 20 0 // m ', and the related splash target material becomes a jet beach during splashing There is a problem with the starting point. As mentioned above, the A 1 or A 1 alloy splash target obtained by spray forming method is applicable to the Chinese National Standard (CNS) A4 specification (210 X 297 Gongchu): -10-476797 A7 B7_ V. Description of the invention (8) (Please read the precautions on the reverse side before filling out this page) The material has a higher oxygen concentration than the A 1 or A 1 alloy sputtering target material obtained by vacuum melting or the like. This is the fact that the former shows a large amount of inclusions in the material compared with the latter. However, the former is less likely to cause splashes than the latter when splashing. This is due to the smaller size of the inclusions in the material compared to the latter. That is, as in the former case, in the case where the size of the inclusions is small, even if the number of inclusions is large, the influence is small, and the occurrence of splashing is more difficult to cause. The latter vacuum melting method or atmospheric melting At last, a large number of inclusions larger than 20 are formed, so it is the starting point of splashing. Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs. However, when the A 1 or A 1 alloy sputtering target material is manufactured by the spray forming method, nitrogen gas is used as the atomizing gas in the gas atomizing step of the spray forming method. In some cases, the obtained A 1 or A 1 alloy splash target material becomes a high nitrogen concentration. The relevant sputtering target material with a relatively high nitrogen concentration is used, and the A 1 or A 1 alloy film such as the A 1 electrode film formed by the sputtering method has a high nitrogen concentration. Due to the influence of this nitrogen, the specific resistance 値 becomes larger. . For example, when a sputtering target material made of A 1-T i alloy (A 1 alloy containing T i) is used to form an A 1 alloy thin film, as shown in FIG. 7, the higher the N amount of the sputtering target material, The higher the resistivity of the formed Al alloy film. Therefore, if the specific resistance 値 of the A 1 or A 1 alloy thin film is observed during the period, the lower the nitrogen concentration of the A 1 or A 1 alloy sputtering material used to form the thin film, the better it is 0.1 mass ( Mass)% or less is expected. Making it less than 0 · lma ss% has the significance of suppressing the increase of the resistivity caused by the increase of nitrogen concentration. The paper is in accordance with the Chinese National Standard (CNS) A4 specification (210X29 * 7 mm1) in accordance with the nitrogen paper standard. 11. &Quot; 476797 A7 ______ B7_ 5. Description of the Invention (9) Those with the same 0% resistivity are highly anticipated. In order to meet this point, the above-mentioned limits are stipulated. Therefore, 'Yu Jiaduoqi As a gas atomization step in the spray formation method, the technology of reducing the nitrogen concentration of the obtained A 1 or A j _ alloy splash target material should be developed, especially to reduce the nitrogen concentration of the obtained A 1 or A j _ alloy splash target material. To 〇.] _ ____ · ... .... · '— = /-"----- ····-·-mass% technology and careful research. The results, in The amount of gas outflow (N m 3) / melt outflow (kg) in the gas atomization step of the spray forming method, that is, if the nitrogen outflow (Nm3) / melt outflow (kg) When it is set to more than 10 N m 3 / kg, it can be known that A 1 or A 1 alloy sputtering target material whose nitrogen concentration is less than 0 · 1 mass% The A 1 or A 1 alloy sputtering target material obtained in this way is obtained by a manufacturing method having a structure basically the same as that of the manufacturing method of the present embodiment, so the size (maximum length) of the inclusions in the memory is all Below 10 V m, it is difficult to cause splashing during splashing. Printed by the Intellectual Property of the Ministry of Economic Affairs and printed by the Consumer Consumer Cooperative. Therefore, A 1 or A 1 alloy sputtering target materials are manufactured by spray forming method. In the case of using nitrogen as the atomizing gas in the gas atomizing step of the spray forming method, if the gas outflow amount (N m 3) / melt outflow amount (kg) is used in this gas atomization step When it is set to 10 N m 3 / kg and i :, the size (maximum length) of the inclusions in the memory is all below 10 / zm, and the nitrogen concentration can be obtained at 0.1 Ima ss% below A 1 or A 1 alloy splash target material. If according to the relevant A 1 or A 1 alloy splash material, it is more difficult to cause splashing during splashing, and A 1 or A 1 with a smaller specific resistance 値Alloy film. This paper size is applicable to China National Standard (CNS) A4 specification (210X297 PCT) • 12- 476797 A7 B7 V. Description of the Invention (10) as aforesaid to the use of nitrogen as the atomizing gas for the quench gas mist formation method in the case of spraying the gas effluent ,, amount of atomizing gas in step (
Nm3) /熔液流出量（kg)之値若設爲1 ON m 3/ ........ ..... . . ” k g以上時，可得氮濃度在〇 · 1 m a s s %以下的A 1 "" _________ 一-，〆，’ 或A 1合金濺潑靶材料。此係由氣體霧化而得的A 1或 A 1合金之液滴（熔融狀或半熔融狀的小粒）堆積於底板 上或模型內等之後，此液滴受麗氣苤坌座金JiJt J-MMJt ，因此A 1及N間之反應較難生成，氮化物之生成_iL變少 .一 . —— …一一.....…——......... -…一，〆 所致。 ............. 針對此點，若將上述氮氣流出量（N m 3 )/熔液流出 量（k g )之値設成未滿1 〇 N m 3 / k g時，則已堆積於 底板上或模型內等的液滴之冷却成爲不足夠，尤其於該堆 積物（液滴之堆積層）之中心部成爲不足夠，因此A 1與 N間之反應比較容易生成，由於此反應之故大量生成氮化 物，結果所得的A 1或A 1合金濺潑靶材料成爲氮濃度高 且超過0 . lma s s%。 且，於本發明，夾雜物之最大長度係指夾雜物之最大 長度部分之長度。例如夾雜物之形狀爲球狀的情形指直徑 ，約略長方體之情形則指最大邊之長度。內存的夾雜物之 最大長度全部在2 0 /i m以下，則指材料中內存的夾雜物 之任者之最大長度均在2 0 以下。 於在噴布形成法之氣體霧化步驟的熔液流出量，係指 由已有熔液進入的容器之熔液流出口流出的熔液之每單位 時間之量。在相同步驟之氣體流出量係指爲使上述流出的 本纸張尺度適用中國國家標準（CNS ) A4規格（210X297公釐）_ 13 (請先閱讀背面之注意事項再填寫本頁)Nm3) / melt outflow (kg) is set to 1 ON m 3 / ........ ........ "Kg, the nitrogen concentration will be 0.1 mass% The following A 1 " " _________ a-, 〆, 'or A 1 alloy splash target material. This is a droplet of A 1 or A 1 alloy (fused or semi-fused) obtained by gas atomization After small particles are accumulated on the bottom plate or in the model, the droplet is affected by the LiJiJiJiJ-MMJt, so the reaction between A 1 and N is more difficult to generate, and the formation of nitrides _iL becomes less. I. — —… One by one ..... …… ——......... -... one by one... ....... At this point, if the above nitrogen When the flow rate (N m 3) / melt flow rate (kg) is set to less than 10 N m 3 / kg, the cooling of liquid droplets that have accumulated on the bottom plate or in the mold becomes insufficient, especially The center portion of the deposit (the droplet deposit layer) is not sufficient, so the reaction between A 1 and N is relatively easy to generate. As a result of this reaction, a large amount of nitride is generated. As a result, the obtained A 1 or A 1 alloy splashes. The target material becomes high in nitrogen concentration and exceeds 0.1 lma ss%. In the present invention, the maximum length of the inclusions refers to the length of the maximum length of the inclusions. For example, when the shape of the inclusions is spherical, it means the diameter, and in the case of approximately rectangular parallelepipeds, it means the length of the largest side. If the maximum length is all less than 20 / im, it means that the maximum length of any one of the inclusions in the material is less than 20. For the melt outflow in the gas atomization step of the spray formation method, it refers to the The amount of melt per unit time flowing out of the melt outflow of the container where the melt has entered. The gas outflow in the same step refers to the Chinese paper standard (CNS) A4 for the above paper size (210X297mm) _ 13 (Please read the notes on the back before filling in this page)
T 經濟部智慈財1局員工消費合作社印製 476797 A7 B7 經濟部智慧財產芍資工消費合作社印製 五、發明説明（11 ) 熔液予以氣體霧化，使由氣體霧化用氣體源之氣體流出口 流出的氣體之每單位時間之量。 於在噴布形成法之氣體霧化步驟的氣體流出量（N m 3 )/熔液流出量（k g )之値，係指熔液流出量之單位爲 k g /單位時間，指氣體流出量之單位爲表示成N m 3 /單 位時間之時之氣體流出量與熔液流出量之比，亦即氣體流 出量（k g /單位時間）/熔液流出量（N m 3 /單位時間 )。惟，此時單位時間之單位係與在熔液流出量之情形及 在氣體流出量之情形相同，上述氣體流出量（N m 3 )/熔 液流出量（k g )之値，亦被稱作氣體/金屬比。 例如若氣體流出量爲4 0 N m 3 /分鐘、熔液流出量爲 4 2 k g /分鐘時，則氣體流出量（N m 3 ) /熔液流出量 (kg)之値爲40 (Nm3/分鐘）/ 4 (kg/分鐘） ，故成爲40 (Nm3) / 4 (kg)，因此成爲 1 〇 N m 3 / k g。 實施例1〜3 將A 1 - 2 U % N d合金熔解，採用此，利用噴 布形成法製作鑄塊。亦即，將A 1 - 2 a t % N d合金 之熔液予以氣體霧化，使堆積於鑄模內，而得A 1 - 2 a t % Nd合金鑄塊。此時，採用氮氣作爲於在噴布 形成法的氣體霧化步驟之霧化用氣體。又此一於在噴布形 成法的氣體霧化步驟之氮氣流出量（N m 3 )/熔液流出量 (kg)之値，設成如第2圖所示之6Nm3/kg、 1〇 (請先閱讀背面之>i意事項再填寫本頁) fe衣.T Printed by the Intellectual Property Cooperative Bureau of the Ministry of Economic Affairs 1st employee 476797 A7 B7 Printed by the Intellectual Property Cooperative Consumers' Cooperative of the Ministry of Economic Affairs 5. Description of the invention (11) The melt is gas atomized, and the gas source The amount of gas flowing out of the gas outlet per unit time. The gas outflow (N m 3) / melt outflow (kg) in the gas atomization step in the spray formation method refers to the unit of the melt outflow in kg / unit time and the The unit is expressed as the ratio of the gas outflow to the melt outflow at the time of N m 3 / unit time, that is, the gas outflow (kg / unit time) / melt outflow (N m 3 / unit time). However, the unit of unit time at this time is the same as that in the case of melt outflow and gas outflow. The above-mentioned gas outflow (N m 3) / melt outflow (kg) is also called Gas / metal ratio. For example, if the gas outflow is 40 N m 3 / min and the melt outflow is 4 2 kg / min, then the gas outflow (N m 3) / melt outflow (kg) will be 40 (Nm3 / Minutes) / 4 (kg / minute), so it becomes 40 (Nm3) / 4 (kg), so it becomes 10N m 3 / kg. Examples 1 to 3 An A 1-2 U% N d alloy was melted, and an ingot was produced by a spray forming method using this. That is, the melt of the A 1-2 at t% N d alloy is gas-atomized to be deposited in a mold, and an A 1-2 at% Nd alloy ingot is obtained. At this time, nitrogen was used as the atomizing gas in the gas atomizing step in the spray forming method. In addition, the amount of nitrogen outflow (N m 3) / melt outflow (kg) in the gas atomizing step in the spray forming method is set to 6Nm3 / kg, 10 (see Figure 2). (Please read the > i notice on the back before filling this page) fe clothing.
IT 本纸張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -14- 476797 A7 B7 五、發明説明（12IT This paper size applies to China National Standard (CNS) A4 specification (210X297 mm) -14-476797 A7 B7 V. Description of the invention (12
Nm /kg 又 15Nm3/g。且，上述 Ai—2at% N d合金鑄塊（濺潑靶材料）之製造方法，係相當於本 實施形態之製造方法。 將上述鑄塊鍛造、壓延後，經機械加工，製作出0 4 英吋形狀之A 1 - 2 a t% Nd合金濺潑靶材料。 對於如此製作的A 1 - 2 a t % N d合金濺潑祀材 料’調查內存的夾雜物之大小（最大長度）及氧量，又， 調整濺潑時的噴濺發生之程度。 此時’對夾雜物之大小的調查，由上述濺潑靶材料採 取顯微鏡試料，硏磨此試料後，用光學顯微鏡觀察，利用 測定夾雜物之大小的方法進行。氧量之調查係由上述濺潑 靶材料採取氣體分析用試料，對此試料利用氣體分析的方 法進行。 至於噴濺發生之程度之調查，採用上述濺潑靶材料， 依第1圖所示的濺潑條件進行1小時之濺潑，於基片上形 成A1 - 2a t% Nd合金薄膜後，採用光學顯微鏡觀 察此薄膜之表面利用測定大小（最大長度）在1 0 // m以 上的噴濺個數之方法進行。此時，在噴濺之中作成能測定 大小在1 0 //m以上者，尤其大小在1 0 以上之噴濺 對薄膜之性能帶來重大的妨礙，乃成爲問題所致。 對上述夾雜物之大小、氧量及大小1 0 # m以上的噴 濺之發生數調查的結果示於第2圖。亦即以於在噴布形成 法的氣體霧化步驟之氮氣流出量（N m 3 )/熔液流出量（ kg)之値爲 6Nm3/kg 而得的 Al— 2a t% Nd 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐）· 15 請 先 閱 讀 背 面 Ϊ 事 項 再 頁 經濟部智慧財產局8工消費合作社印製 476797 A7 B7 五、發明説明（13 ) (請先閱讀背面之*注意事項再填寫本頁) 合金濺潑靶材料之夾雜物的大小（最大長度）爲1 6 ，以，氮氣流出量（N m 3 ) /熔液流出量（k g )之値爲 1 5Nm3/kg而得的A 1 - 2 a t% Nd合金潑潑IE 材料之夾雜物的最大長度爲4 V m。以下，依此順序各別 將此等的A 1 - 2 a t% Nd合金濺潑靶材料稱作與實 施例1有關的濺潑靶材料’與實施例2有關的濺潑靶材料 ，與實施例3有關的濺潑靶材料。 大小（最大長度）在1 0 以上的噴濺之個數，在 與實施例1有關的濺潑靶材料之情形爲1 0個，實施例2 之情形爲5個，實施例3之情形爲3個。亦即，對薄膜之 性能有惡劣影響1 0 // m以上的噴濺發生之程度如第2圖 所示，實施例1〜3之任一情形亦極少。若能將1 〇 " m 以上的噴濺之個數設成1 0個以下時’在能消除所謂習知 技術未能達成的配線寬度之大幅的微細化之課題的方面而 言，其技術性意義係較大的。 比較例1 經濟部智¾財產局Μ工消費合作社印製 將A 1 - 2 a t % N d合金大氣熔解、鑄造，經予 壓延後，機械加工，製作^4英吋形狀之A1 - 2a t% N d合金濺潑靶材料（以下稱作與比較例1有關的濺潑 靶材料）。 對於上述比較例1，利用與前述實施例1〜3之情形 相同的方法。調查夾雜物之最大長度寺。此寺調查之結果 示於第2圖。如由第2圖可知般，與比較例1有關的濺潑 本紙乐尺度適用中國國家標準（CNS ) Α4規格（210X297公釐）· 16 · 476797 A7 B7 五、發明説明（14 ) 靶材料之夾雜物的最大長度爲6 0 // 以上的噴濺之個數爲5 4個、極多。 大小在1 0 # m 比較例2 將A 1 壓延後，機 N d合金 靶材料）。 對於上 相同的方法 示於第2圖 靶材料之夾 以上的噴濺 由上述 法，未能將 以下。 一 2a t% Nd合金真空熔解、鑄造，經予 械加工，製作 濺潑靶材料1 述比較例2， ，調查夾雜物 。如由第2圖 雜物的最大長 之個數爲2 7 比較例1、2 全部的夾雜物 必4英吋形狀之A 1 — 2a t% 以下稱作與比較例2有關的濺潑 利用與前述實施例1〜3之情形 之最大長度等。此等調查之結果 可知般，與比較例2有關的濺潑 度爲3 0//m。大小在1 〇 個，甚多。 可知，在大氣熔解法或真空熔解 之大小如本發明般設成2 0 yt/m 請 先 閱 背 ιέ 之 ί ψ 項 再 m 本 頁 經濟部智慧財產局員工消費合作社印製 比較例3 將在噴布形成法的氣體霧化步驟之氮氣流出量（N m )/熔液流出量（k g )之値設成如第2圖般之4 N m 3 / k g。除此點外，藉由與前述實施例1〜3之情形相同的 方法’製作出04英吋形狀之A 1 - 2 a t% Nd合金 濺潑靶材料（以下稱作與比較例3有關的濺潑靶材料）。 對於上述比較例3，利用與前述實施例1〜3之情形 本紙張尺度適用中國國家標準（CNS ) A4規格（210 X 297公釐） -17- )797 A7 B7 五、發明説明（15 ) (請先閱-讀背面之注意事項再填寫本頁) 相同的方法，調查夾雜物之最大長度等。此等調查之結果 示於第2圖。如第2圖可知般，與比較例3有關的濺潑靶 材料之夾雜物的最大長度爲2 5 //m，大小在1 〇 "m以 上的噴濺之個數爲2 3個，甚多。 复直例4 利用與前述實施例1〜3之情形同樣的方法，製作 A 1 - 2 a t % Nd合金濺潑靶材料。惟，爲使濺潑靶 材料中的夾雜物之最大長度變化，以在噴布成形法之氣體 霧化步驟的氮氣流出量（N m 3 ) /熔液流出量（k g )之 値爲參數予以變化。 至於上述濺潑靶材料，利用與前述實施例1〜3之情 形同樣的方法，調查夾雜物之最大長度及濺潑時之1 〇 β m以上的噴濺發生之個數。因此，以表示此等調查之結 果的第5圖爲準，將夾雜物之最大長度及大小在1 0 //m 以上的噴濺之個數間之關係示於第6圖。 經濟部智慈財產局8工消費合作社印製 由第6圖可知，在夾雜物之最大長度在超過2 0 /im 之領域隨著夾雜物之最大長度變大，1 0 // m以上的噴濺 之個數雖然劇烈增加，但是夾雜物之最大長度在2 0 // m 以下的領域時在1 〇 // m以上的噴濺之個數變成極少，會 較難引起噴濺之發生。 且，在以上的實施例1〜4，比較例3採用氮氣作爲 於在噴布形成法的氣體霧化步驟之霧化用氣體，如前述般 雖可得結果，然而採用氬氣等其他霧化用氣體取化此氮氣 本纸張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） •18- 476797 A7 _B7_______ 五、發明説明（16 ) 之情形，亦可得同樣的結果。 實施例5〜7 將A1 - Ti合金（含有Ti之A1合金），採用此 合金利用噴布形成法製作鑄塊。此時採用氮氣作爲於在噴 布形成法的氣體霧化步驟之霧化用氣體。又，將此氣體霧 化步驟之氮氣流出量（Nm3) /熔液流出量（k g )之値 變化成如第3圖所示般的1 4 · 3Nm3/kg、1 2 · 9 Nm3/kg、10.0Nm3/kg。 由上述鑄塊採取氣體分析用試料，對此試料利用氮氣 分析的方法，調查鑄塊之含氮量（氮濃度）。此調查之結 果不於第3圖。含氮量各自極低至〇 . 〇 1 5、 0.018、〇· 027 ma s s%，不論何者均在 〇· 1 m a s s %。結果，歸因於各自的含氮量之電阻係 數的增加可予抑制在0 · 1 1、〇 . 1 3、 〇· 20//Qcm與0 · 75//Qcm以下（含氮量在 經濟部智慧財產芍員工消費合作社印製 實施例8〜9 將A 1 - N d合金熔解，採用此合金利用噴布形成法 製作鑄塊。此時採用氮氣作爲於在噴布形成法的氣體霧化 步驟之霧化用氣體。又，將此氣體霧化步驟之氮氣流出量 (N m 3 ) /熔液流出量（k g )之値變化成如第3圖所示 般的 14.3、 10.0Nm3/kg。 以與實施例5〜7之情形同樣的方法調查上述實施例 -19- 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公楚） 476797 A7 B7 五、發明説明（17 ) 8、 9之鑄塊之含氮量。此調查之結果示於第3圖’含氮 量係各自極低至0.012、0.020niass%。 (請先閱讀背面之注意事項再填寫本頁) 以氮量較少者由於電阻係數會下降較宜，惟對含氮量 以參考例1〜4爲準附加以下說明。 參考例1、2 將於噴布形成法之氣體霧化步驟的氮氣流出量（N m 3 )/熔液流出量（k g )之値設成如第3圖所示般的 8.88、 8.93Nm3/kg。去除相關點外，利用與 實施例5〜7之情形同樣的方法製作A 1 - T i合金鑄塊 〇 利用與實施例5〜7之情形同樣的方法調查上述參考 例1、 2之鑄塊之含氮量。此調查之結果示於第3圖，含 氮量係各爲0 · 1 3、0 · 41ma s s%，任一者均超 過 0.1m ass%。 參考例3、4 經濟部智慧財產局員工消費合作社印製 將於噴布形成法之氣體霧化步驟的氮氣流出量（N m 3 )/熔液流出量（k g )之値設成如第3圖所示般的 9.0、8 · 9 N m 3 / k g。去除相關點外，利用與實施 例8〜9之情形同樣的方法製作A 1 — N d合金鑄塊。 利用與實施例8〜9之情形同樣的方法調查上述參考 例3、 4之鑄塊之含氮量。此調查之結果示於第3圖。含 氮量係各爲0.11、 0.33mass%，任一者均超 本纸張尺度適用中國國家標準（CNS ) A4規格（210X297公釐）~「20- 一 476797 A7 __—_B7 五、發明説明（18 ) 過 O.lmass%。 實施例1 0 利用與前述實施例1〜3之情形同樣的方法，製作 A 1合金濺潑靶材料，然而採用A 1 -丁 i合金取化A 1 - N d合金作爲A 1合金。又，爲使濺潑靶材料中的含氮 量變化，以在噴布成形法之氣體霧化步驟的氮氣流出量（ N m 3 ) /熔液流出量（k g )之値爲參數予以變化。 採用上述濺潑靶材料，利用第4圖所示的濺潑條件， 進行1小時之濺潑，於基片上形成A 1 - T i合金薄膜。 於是，在通常的熱處理之後，測定此薄膜之電阻係數。此 測定係利用微影（.photolithography )方式加工成寬度 1 0 0 A m、長度1 0 m m之比電阻測定用圖形，利用四 探針法藉由測定比電阻之方法進行。 另一方面，利用與實施例5〜7之情形同樣的方法測 定上述實施例1 0之濺潑靶材料之含氮量。 經濟部智慈財產苟員工消費合作社印製 因此，基於上述測定之結果，求取濺潑靶材料中的含 氮量及所得的薄膜之電阻係數間的關係。此結果示於第7 圖。由第7圖可知若濺潑靶材料之N量愈低，所形成的 A 1合金薄膜之電阻係數變成變小。 且，在以上的實施例1〜1 0，比較例1〜3及參考 例1〜4，採用A1 - Nd合金、A1 - Ti合金作爲 A 1合金，如前述般可得結果，惟對採用A 1 - T a、 A1 - Fe、Al-Co、A1 - Ni、A1 - REM( 稀土類元素）等的其他A 1合金取代此等A 1合金亦可得 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐）· 21 _ 476797 A7 _____B7 _ __五、發明説明（19 ) 同樣的傾向之結果。 以上本發明係以具體實施例詳細說明，對熟習此項技 藝者而言顯而可知在不偏離本發明之精神及範疇下可作各 種變化及修飾。 本案之日本專利申請案特願平1 〇 - 4 0 5 2 0號係 於1998年（平成8年）2月23日提出，包括詳細說 明書、申請專利範圍、圖式及摘要在此一倂提出供參考。 t 背 面 意 項 再Nm / kg and 15Nm3 / g. In addition, the manufacturing method of the Ai-2at% N d alloy ingot (sputter target material) is equivalent to the manufacturing method of this embodiment. The ingot was forged and rolled, and then machined to produce a 0 4 inch A 1-2 a t% Nd alloy sputtering target material. For the A 1-2 a t% N d alloy sputtering target material thus prepared ', the size (maximum length) of the inclusions in the memory and the amount of oxygen were investigated, and the degree of splashing during the sputtering was adjusted. At this time, the investigation of the size of the inclusions was carried out by taking a microscope sample from the sputtering target material, honing the sample, observing with an optical microscope, and measuring the size of the inclusions. The oxygen amount was measured by using the sputtering target material for a gas analysis sample, and the sample was analyzed by a gas analysis method. As for the investigation of the extent of sputtering, the sputtering target material was used, and sputtering was performed for 1 hour under the sputtering conditions shown in FIG. 1 to form an A1-2a t% Nd alloy thin film on the substrate, and then an optical microscope was used. Observe the surface of this film by measuring the number of splashes (maximum length) above 1 0 // m. At this time, it is possible to make a measurement that can be measured in a size of 10 / m or more during the spray, especially a spray of a size of 10 or more, which causes a major obstacle to the performance of the film, which is a problem. The results of the investigation on the number of inclusions, the amount of oxygen, and the number of spatters above 10 # m are shown in FIG. 2. That is, Al—2a t% Nd obtained when the nitrogen outflow (N m 3) / melt outflow (kg) is 6Nm3 / kg in the gas atomization step of the spray formation method. This paper is applicable to the paper size. China National Standard (CNS) A4 Specification (210X297 mm) · 15 Please read the back page 事项 Matters and then the page printed by the Ministry of Economic Affairs Intellectual Property Bureau 8 Industrial Consumer Cooperatives 476797 A7 B7 V. Description of the invention (13) * Notes, please fill in this page again.) The size (maximum length) of the inclusions of the alloy splash target is 16 and the amount of nitrogen outflow (N m 3) / melt outflow (kg) is 1 5Nm3 / The maximum length of inclusions in A 1-2 at% Nd alloy splashed IE material obtained from kg is 4 V m. Hereinafter, these A 1-2 at% Nd alloy sputtering target materials are referred to in this order as the sputtering target materials related to Example 1 ', the sputtering target materials related to Example 2, and the examples 3 Related splash target materials. The number of splashes with a size (maximum length) of 10 or more is 10 in the case of the sputtering target material related to Example 1, 5 in Example 2, and 3 in Example 3. Each. That is, the degree of spatter that has a bad influence on the performance of the film above 10 // m is as shown in Fig. 2, and there are very few cases of Examples 1 to 3. If it is possible to set the number of spatters of 10 mm or more to 10 or less, the technology will be able to eliminate the problem of large and miniaturization of the wiring width that cannot be achieved by the so-called conventional technology. Sexual significance is greater. Comparative Example 1 Printed by the Ministry of Economic Affairs, the Intellectual Property Bureau, and the Industrial and Industrial Cooperatives. A 1-2 at% N d alloy was melted and cast into the atmosphere. After rolling, it was machined to produce ^ 4-inch A1-2a t%. N d alloy sputtering target material (hereinafter referred to as a sputtering target material related to Comparative Example 1). For Comparative Example 1, the same method as in the case of the foregoing Examples 1 to 3 was used. Investigate the maximum length temple for inclusions. The results of this temple survey are shown in Figure 2. As can be seen from Figure 2, the splattered paper scale related to Comparative Example 1 is in accordance with the Chinese National Standard (CNS) A4 specification (210X297 mm) · 16 · 476797 A7 B7 5. Description of the invention (14) Inclusion of target materials The maximum length of the object is 6 0 // The number of splashes is 5 4 and very many. The size is 1 0 # m Comparative Example 2 After rolling A 1, the target material is N d alloy). For the same method shown in Figure 2 above, the target material is clipped above. The above method fails to apply the following method. A 2a t% Nd alloy was vacuum melted, cast, and pre-processed to produce a sputtering target material. Comparative Example 2 described above, and investigated for inclusions. As shown in Figure 2, the maximum number of debris is 2 7 Comparative Examples 1 and 2 All inclusions must have a 4-inch shape of A 1-2a t%, which is hereinafter referred to as Comparative Example 2 The maximum length in the case of the aforementioned embodiments 1 to 3, etc. As a result of these investigations, it was found that the splash rate related to Comparative Example 2 was 30 // m. The size is 10, many. It can be seen that the size of atmospheric melting method or vacuum melting is set to 20 yt / m as in the present invention. Please read the item of ψ and then m on this page. Comparative Example 3 printed by the Employees ’Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs will be printed on The nitrogen outflow (N m) / melt outflow (kg) of the gas atomization step of the spray forming method is set to 4 N m 3 / kg as shown in FIG. 2. Except for this point, a 04-inch-shaped A 1-2 at% Nd alloy sputtering target material (hereinafter referred to as the sputtering related to Comparative Example 3) was produced by the same method as in the case of the foregoing Examples 1 to 3. Splash target material). For the above Comparative Example 3, using the same conditions as in the foregoing Examples 1 to 3, the paper size is applicable to the Chinese National Standard (CNS) A4 specification (210 X 297 mm) -17-) 797 A7 B7 V. Description of the invention (15) ( Please read-read the precautions on the reverse side before filling out this page.) The same method is used to investigate the maximum length of inclusions. The results of these investigations are shown in Figure 2. As can be seen from FIG. 2, the maximum length of the inclusions of the sputtering target material related to Comparative Example 3 is 2 5 // m, and the number of splashes having a size of more than 1 〇 " m is 2 3, even many. Compound Straight Example 4 A 1-2 a t% Nd alloy sputtering target material was produced by the same method as in the case of the foregoing Examples 1 to 3. However, in order to change the maximum length of the inclusions in the sputtering target material, the effluent amount of nitrogen (N m 3) / melt effluent amount (kg) in the gas atomization step of the spray forming method is used as a parameter. Variety. As for the sputtering target material described above, the maximum length of inclusions and the number of spatters at 10 β m or more at the time of sputtering were investigated by the same method as in the case of the foregoing Examples 1 to 3. Therefore, the relationship between the maximum length and the number of splashes with a size of 1 0 // m or more is shown in Figure 6 based on Figure 5 showing the results of these investigations. Printed by the 8th Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs. From Figure 6, it can be seen that in the area where the maximum length of the inclusions exceeds 20 / im, the maximum length of the inclusions becomes larger. Although the number of splashes has increased sharply, the number of splashes above 1 0 // m is extremely small when the maximum length of inclusions is below 20 // m, and it is difficult to cause splashes. Moreover, in Examples 1 to 4 and Comparative Example 3, nitrogen was used as the atomizing gas in the gas atomizing step in the spray forming method. Although the results were obtained as described above, other atomizing such as argon was used. Use gas to extract this nitrogen. The paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm) • 18- 476797 A7 _B7_______ 5. In the case of the invention description (16), the same result can be obtained. Examples 5 to 7 An A1-Ti alloy (A1 alloy containing Ti) was used to produce an ingot by a spray forming method. At this time, nitrogen was used as the atomizing gas in the gas atomizing step in the spray forming method. In addition, the amount of nitrogen outflow (Nm3) / melt outflow (kg) in this gas atomization step was changed to 1 4 · 3 Nm3 / kg, 1 2 · 9 Nm3 / kg, as shown in FIG. 3. 10.0Nm3 / kg. A sample for gas analysis was taken from the ingot, and a nitrogen analysis method was used for the sample to investigate the nitrogen content (nitrogen concentration) of the ingot. The results of this survey are not shown in Figure 3. Nitrogen contents were each extremely low to 0.015, 0.018, 0.027 ma s s%, and both were at 0.1 m a s s%. As a result, the increase in the resistivity attributed to the respective nitrogen content can be suppressed to less than 0 · 1 1, 0.1, 0.3, 20 · / Qcm, and 0 · 75 // Qcm (the nitrogen content is in the Ministry of Economic Affairs). Printed by Intellectual Property and Employee Consumer Cooperatives. Examples 8-9 Melt the A 1-N d alloy and use this alloy to make ingots by spraying. At this time, nitrogen is used as the gas atomizing step in spraying. The atomizing gas. The nitrogen outflow (N m 3) / melt outflow (kg) of this gas atomizing step was changed to 14.3 and 10.0 Nm3 / kg as shown in FIG. 3. Investigate the above Examples-19 in the same way as in the cases of Examples 5 to 7. This paper size applies the Chinese National Standard (CNS) A4 specification (210X297). 476797 A7 B7 V. Description of the invention (17) 8, 9 of 9 Nitrogen content in the ingot. The results of this survey are shown in Figure 3 'The nitrogen content is extremely low as 0.012 and 0.020niass% respectively. (Please read the precautions on the back before filling this page) Since the resistivity may decrease, it is better to add the following explanation to the nitrogen content based on Reference Examples 1 to 4. Examples 1 and 2 Set the nitrogen outflow (N m 3) / melt outflow (kg) in the gas atomization step of the spray forming method to 8.88, 8.93 Nm3 / kg as shown in Figure 3. Except for the relevant points, the A 1-T i alloy ingot was produced by the same method as in the case of Examples 5 to 7. The ingot of Reference Examples 1 and 2 was investigated by the same method as in the case of Examples 5 to 7. The nitrogen content. The results of this survey are shown in Figure 3. The nitrogen content is 0 · 1 3, 0 · 41ma ss%, and any one exceeds 0.1m ass%. Reference Examples 3 and 4 Wisdom of the Ministry of Economic Affairs Printed by the Consumer Cooperative of the Property Bureau. The nitrogen outflow (N m 3) / melt outflow (kg) of the gas atomization step of the spray formation method is set to 9.0, 8 as shown in Figure 3. · 9 N m 3 / kg. Except for the relevant points, an A 1 —N d alloy ingot was produced by the same method as in the case of Examples 8 to 9. The above reference was investigated by the same method as in the case of Examples 8 to 9. The nitrogen content of the ingots of Examples 3 and 4. The results of this survey are shown in Figure 3. The nitrogen content is 0.11 and 0.33 mass% each, and any of them exceeds this paper rule. Applicable to China National Standard (CNS) A4 specification (210X297 mm) ~ "20- 476797 A7 ____B7 V. Description of the invention (18) Pass O.lmass%. Example 1 0 Use the same as the previous examples 1 ~ 3 In the same way, an A 1 alloy sputtering target material is produced, but an A 1 -Nd alloy is used as the A 1 alloy. In addition, in order to change the nitrogen content in the sputtering target material, the amount of nitrogen outflow (Nm3) / melt outflow (kg) in the gas atomization step of the spray forming method was changed as a parameter. Using the sputtering target material, sputtering was performed for one hour under the sputtering conditions shown in FIG. 4 to form an A 1 -T i alloy thin film on the substrate. Therefore, the resistivity of the film was measured after a general heat treatment. This measurement was processed into a pattern for measuring specific resistance with a width of 100 μm and a length of 10 μm by using a photolithography method. The specific resistance was measured by a four-probe method. On the other hand, the nitrogen content of the sputtering target material of Example 10 was measured by the same method as in the cases of Examples 5 to 7. Printed by the Intellectual Property Department of the Ministry of Economic Affairs and the Consumer Cooperative. Therefore, based on the results of the above measurement, the relationship between the nitrogen content in the sputtering target material and the resistivity of the resulting film was determined. This result is shown in Figure 7. As can be seen from Fig. 7, if the amount of N of the sputtering target material is lower, the resistivity of the formed Al alloy film becomes smaller. Moreover, in the above Examples 1 to 10, Comparative Examples 1 to 3, and Reference Examples 1 to 4, A1-Nd alloy and A1-Ti alloy were used as the A 1 alloy, and the results were obtained as described above. Other A 1 alloys such as 1-T a, A1-Fe, Al-Co, A1-Ni, A1-REM (rare earth element), etc. Replace these A 1 alloys. This paper size can also be applied to Chinese National Standards (CNS) A4 specification (210X297 mm) · 21 _ 476797 A7 _____B7 _ __ V. Explanation of the invention (19) The result of the same tendency. The present invention has been described in detail through specific embodiments. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the spirit and scope of the present invention. Japanese Patent Application No. Hei 0- 0 5 2 0 of this case was filed on February 23, 1998 (Heisei 8), and detailed specifications, patent application scope, drawings, and abstract are filed here. for reference. t dorsal view
頁 經濟部智慧財產笱員工消費合作社印製 圖式之簡單說明 第1圖爲表示實施例記載的潑潑 第2圖爲表示與實施例1〜4及 濺潑靶材料之製造條件、夾雜物之大 噴濺之個數、氧量之調查結果之表； 第3圖爲表示與實施例5〜9及 濺潑靶材料之製造條件、夾雜物之大 噴濺之個數、氧量之調查結果之表； 第4圖爲表示與實施例1 〇有關 條件之表。 第5圖爲表示就與實施例4有關 潑靶材料之夾雜物的最大長度與1〇 間之關係表。· 第6圖爲表示就與實施例4有關 潑靶材料之夾雜物的最大長度與1〇 間之關係圖；及 條件之表； 比較例1〜3有關的 小、1 0 " m以上的 參考例1〜4有關的 小、1 0 // m以上的 的濺潑靶材料之濺潑 的A 1或A 1合金濺 // m以上之噴濺個數 的A 1或A 1合金濺 //m以上之噴濺個數 本纸張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -22- 476797 A7 B7五、發明説明（2〇 )第7圖爲表示就與實施例10有關的濺潑靶材料之N 量與所得的薄膜之電阻係數間之關係圖。 I—^-------衣— (請先閲求背面之注意事項再填寫本頁) 訂 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（210X297公釐）_ 23 _Page The Ministry of Economic Affairs, Intellectual Property, Employee Consumer Cooperative Cooperative Printed Brief Description. The first figure shows the splashes described in the examples. The second figure shows the manufacturing conditions and the inclusions of the target materials and examples 1 to 4 Table of investigation results of the number of large splashes and the amount of oxygen; Figure 3 shows the results of the investigation of the manufacturing conditions of the sputtering target materials and the number of large splashes of the inclusions and the amount of oxygen from Examples 5-9 Table 4 is a table showing the conditions related to Example 10. Fig. 5 is a table showing the relationship between the maximum length of inclusions of the sputtering target material and 10 in relation to Example 4. Figure 6 is a graph showing the relationship between the maximum length of the inclusions of the sputtering target material related to Example 4 and 10; and a table of conditions; small, 1 0 " m or more related to Comparative Examples 1 to 3. Reference examples 1 to 4 related to small, 1 0 // m or more splash target material splashes A 1 or A 1 alloy splashes // m or more A 1 or A 1 alloy splashes Number of splatters above / m is applicable to Chinese national standard (CNS) A4 specification (210X297 mm) -22-476797 A7 B7 V. Description of the invention (20) Figure 7 shows the same as in Example 10. A graph showing the relationship between the amount of N of the sputtering target material and the resistivity of the resulting film. I — ^ ------- yi — (Please read the notes on the back before filling this page) Order the paper printed by the Employees' Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs, the paper size applies to Chinese National Standard (CNS) A4 specifications ( 210X297 mm) _ 23 _