200811304 九、發明說明： 【發明所屬之技術領域】 尤其係關於一種 無樹突微結構之 本發明係關於一種製造濺鍵乾之方法 澆鑄金屬性濺鍍靶而具有一等轴、胞狀 方法。 【先前技術】 用於製造金屬性賤餘之-當前製程包括：礙碎-由金200811304 IX. Description of the Invention: [Technical Field of the Invention] In particular, the present invention relates to a method for fabricating a sputter dry bond by casting a metallic sputter target with an equiaxed, cell-like method. [Prior Art] Used to make metal balance - current process includes: hamper - by gold
屬性材料構成之厚片；將料碾碎之微㈣選並分類為恰 當之微粒大小；在一真空、密封罐中對特定大小之粒子進 行熱等靜壓（HIP)以形成;及然後加卫該經熱等靜 壓之靶體來形成所期望之靶形狀。 &當前用於製造大型！目濺餘之另一方法係將嶋粉冷等 靜壓（CIP) ’燒結經冷靜壓之本體以降低氧含量，然後將 該經燒結之本體熱軋至一具有期望長度/寬度/厚度之扁平 板或盤上。然後，將該板或盤加工至最終容差。 該等製程涉及製造該濺鍍靶之數個加工步驟及相當高之 成本。 【發明内容】 本發明提供一種用於製造一精細顆粒、澆鑄濺鍍靶之方 法本發明於一實施例中提供一種藉由如下作業製造一濺 方法·溶化一金屬性乾材料；以使該熔化之把材料 歲乎/又有過熱之方式來控制該溶化之把材料之溫度；將該 熔化之靶材料引入到一具有内壁之模具中，該等内壁形成 所期望之鞑形狀之模穴；及藉由以一速度從該靶材料處 122261.doc 200811304 吸取熱量以將該熔化之乾材料固化在該模具中，以使其固 化形成-在該靶中均勻地具有大致等軸、胞狀、無樹突之 微結構之濺鍍靶。可視需要將該模具加熱至一足夠高之升 门之模度，此防止直接在該模具内壁附近實質形成柱 狀顆粒。 ' 本發明亦於另-實施{列中提供一金屬性濺錢&，在該乾 中均勻地具有-大致等軸、胞狀之無樹突之微結構。該錢 鍍靶可於剛鑄成之情況下即供使用而無需除精加工外之進 步鑄後處理，或可在該剛鑄成之靶進行熱等靜壓以增加 該鑄態靶之密度後即供使用。 本發明有利之處為無需本業界所採用之諸多處理步驟即 可提供一洗鑄濺鍍靶，且有利之處為能提供一具有對濺鍍 有益之微結構性質之濺鍍靶。 本發明亦提供對純之顆粒大小之㈣；減少自材料選 擇至靶製造之製造訂貨交付時間；及增加材料選擇之靈活 性（例如更多之合金選項）。 閱讀下文說明可清楚瞭解本發明之其他優點、特徵及實 施例。 【實施方式】 本發明提供-種製造-包括金屬性乾材料之減鍛乾之方 法。該金屬性乾材料可包括—金屬或由兩種或多種金屬構 成之合金。就例示說明之目的而言（並無限制之意）該把材 料可包括鉬、鎢及其他金屬及高溫融化合金，例如以鎳為 主、以鉻為主、以鈷為主、以鐵為主、以鈕為主、以鉬為 122261.doc 200811304 主、以鶴為主之合金、及其他合金材料。就例示說明之目 的（並無意限制）而t ’-乾合金可包括—以料主之合 金，該合金包括-選自由硼'鉻、鉑、鈕、釕、鈮、銅、 飢、石夕、銀、金、鐵、銘、锆、及錄組成之群組之合金元 素。舉例而言包括以銘為主之合金，纟包括作不 限於-c〇-Ta-Zr合金、C0_Ta_B合金、c〇 Cr_pt B合金、 c〇-Cr-Pt-B_Cu合金及其他。此等靶金屬或合金可自原材料 供應商購得’其中適當之純度用於特定義㈣途。該等 金屬或合金係以堪塊、粉末、厚塊等形式提供。 參照圖1 ’本發明之-實施例涉及使用諸如真空感應溶 化(vIM)或電子束_熔化等一適當之熔化製程將所選金 屬性（金屬或合金）靶材料熔化在一坩鍋或其他恰當之熔器 中。可依欲熔化之特定金屬或合金來選擇坩鍋或熔器。熔 化可在一惰性氣氛中或在真空中進行（如果欲熔化的特定 金屬或合金要求此等熔化條件）。在金屬或合金在熔化期 間要求一惰性氣氛或真空之情況下，可使用習用之真空感 應熔化設備。 該實例中所用之一特定習用之真空感應熔爐使用一直接 澆注到一下方模具中之熔化坩鍋。然而，本發明涵蓋使用 一澆注容器（例如一洗注坩鍋），視需要將其作為該澆注容 器與該欲予以澆鑄之模具之間的一中間容器。 較佳地’將該熔化容器中或該灌注容器中之該已熔化之 無材料保持在一大致靜止之狀態，以允許任何低濃度之非 金屬性夾雜物漂浮至表面，可在該表面上對該夾雜物進行 I2226I.doc 200811304 處理或將其從熔液中清除。舉例而言，當使用真空感應熔 化來熔化靶材料之一裝料時，可在感應線圈與該熔化容器 之間放置一感叉器（例如石墨）以便加熱該感受器且依次加 熱該裝料，且使得不會攪動該熔化之靶材料。或者，可使 用極面之頻率或電阻加熱來達到相同之效果。a thick sheet of attribute material; the micro-milled material is selected and classified into the appropriate particle size; hot isostatic pressing (HIP) is formed on a specific size of the particles in a vacuum, sealed can; and then The hot isostatically pressed target forms the desired target shape. & currently used to make large! Another method of splashing is to freeze the isostatic pressing (CIP) of the crucible powder to cool the body to reduce the oxygen content, and then hot-roll the sintered body to a flat shape having a desired length/width/thickness. On a tablet or plate. The plate or disk is then machined to the final tolerance. These processes involve several processing steps to produce the sputter target and a relatively high cost. SUMMARY OF THE INVENTION The present invention provides a method for manufacturing a fine particle, casting a sputtering target. In one embodiment, the present invention provides a sputtering method for dissolving a metallic dry material by the following operation; The material is aged/overheated to control the temperature of the molten material; the molten target material is introduced into a mold having an inner wall that forms a desired shape of the cavity; and The molten dry material is solidified in the mold by drawing heat from the target material at 122261.doc 200811304 at a rate to solidify it - uniformly equiaxed, cell-like, and uniformly in the target The sputtered microstructure of the dendrites. The mold can be heated to a sufficiently high lift mode as desired to prevent substantial formation of columnar particles directly adjacent the inner wall of the mold. The present invention also provides a metal splashing & in the column {which provides a uniform, substantially equiaxed, cell-like, dendritic microstructure in the stem. The money plating target can be used immediately after casting without the need for advanced post-casting treatment except for finishing, or can be subjected to hot isostatic pressing at the newly cast target to increase the density of the as-cast target. That is for use. The present invention is advantageous in that it provides a wash cast target without the need for many processing steps employed in the industry, and is advantageous in that it provides a sputter target having microstructural properties that are beneficial for sputtering. The present invention also provides (4) for pure particle size; reduced manufacturing order delivery time from material selection to target manufacturing; and increased flexibility in material selection (e.g., more alloy options). Other advantages, features, and embodiments of the invention will become apparent from the description. [Embodiment] The present invention provides a method of manufacturing a reduced dry forging comprising a metallic dry material. The metallic dry material may include a metal or an alloy composed of two or more metals. For the purposes of illustration (without limitation), the material may include molybdenum, tungsten and other metals and high temperature melting alloys, such as nickel, chromium, cobalt, and iron. Mainly to the button, molybdenum is 122261.doc 200811304 main, crane-based alloy, and other alloy materials. For the purpose of illustration (not intended to be limiting) and t '-dry alloy may include - a master alloy, the alloy includes - selected from the group consisting of boron 'chromium, platinum, button, bismuth, antimony, copper, hunger, Shi Xi, Alloying elements of the group consisting of silver, gold, iron, inscription, zirconium, and recorded. For example, alloys based on the name are included, and are not limited to -c〇-Ta-Zr alloy, C0_Ta_B alloy, c〇Cr_pt B alloy, c〇-Cr-Pt-B_Cu alloy and others. Such target metals or alloys are commercially available from the raw material supplier' where the appropriate purity is used for the specific definition (iv). The metals or alloys are provided in the form of cans, powders, chunks, and the like. Referring to Figure 1 'The present invention - embodiments relate to melting a selected metallic (metal or alloy) target material in a crucible or other suitable using a suitable melting process such as vacuum induction melting (vIM) or electron beam melting In the fuser. The crucible or melter can be selected depending on the particular metal or alloy to be melted. Melting can be carried out in an inert atmosphere or in a vacuum (if such a melting condition is required for the particular metal or alloy to be melted). In the case where the metal or alloy requires an inert atmosphere or vacuum during the melting, a conventional vacuum induction melting apparatus can be used. One of the conventional vacuum induction furnaces used in this example uses a melting crucible that is directly poured into a lower mold. However, the invention contemplates the use of a pouring container (e.g., a laundering crucible) as needed as an intermediate container between the casting container and the mold to be cast. Preferably, the melted material in the molten vessel or in the infusion vessel is maintained in a substantially stationary state to allow any low concentration of non-metallic inclusions to float to the surface on which the surface may be The inclusions were treated with I2226I.doc 200811304 or removed from the melt. For example, when vacuum induction melting is used to melt one of the target materials, a fork (eg, graphite) may be placed between the induction coil and the melting vessel to heat the susceptor and sequentially heat the charge, and This does not agitate the molten target material. Alternatively, the pole face frequency or resistance heating can be used to achieve the same effect.
而且，使用底部灌注坩鍋允許將熔化之靶材料引入一模 具，而不會夾帶漂浮於該熔液表面上之非金屬性夾雜物。 或者可使用一余壺式坩鍋阻斷漂浮於該熔液上的非金屬 性夾雜物進入該模具，美國專利4,832，112中闡述了使進入 錢具之非金屬性夾雜物之數量最小化之其他技術，該專 利係以參考形式完整併入本文中。 本發明進—步涉及以—在引人該模具之前㈣化之乾材 料成乎不過熱之形式控制該溶化或灌注容器中該溶化之乾 材料之溫度。降低該熔化之靶材料之溫度，直至清除該熔 化之乾材料中大致上所有之過熱量。該降低之 絲材料中應大致均心且對於大多數Μ料，將該降低 :度控制在高於該㈣金屬或合絲材料之所量測炼點之 二至20度F内’儘管該範圍可相依於特定乾金屬或合金而 調即。該量社熔點可如美时利（mm巾所述確定。 逐漸減少供應至該溶化容器位於其中之溶爐之動 =犯量來降低該熔化容器中炼化之乾材料之溫度。舉例 材二之2下文中之實例所述藉由以感聽化來熔化無 降==可逐漸減少供應至職應㈣之電功率以 之乾材料之溫度，以便在將熔化之免材料引入至 122261.doc 200811304 模具中前，清除大致所有之過熱量。 該模具可包括一包括多個内壁之金屬或陶瓷模具，該等 内壁界具有期望之濺㈣形狀之模穴。可製造之減鐘 靶之典型形狀包括，但不限於’矩形、正方形或其他多邊 形形狀之平板及圓盤。 除非在製造熔模洗㈣時，否則本發明預想在將溶 化之乾材料引人至模具中後，視需要在該炼化之托材料中Moreover, the use of a bottom-filled crucible allows the molten target material to be introduced into a mold without entrainment of non-metallic inclusions floating on the surface of the melt. Alternatively, a multi-pot type crucible can be used to block non-metallic inclusions floating on the melt from entering the mold. U.S. Patent 4,832,112 describes minimizing the amount of non-metallic inclusions entering the currency. Other techniques are hereby incorporated by reference in their entirety. The invention further involves controlling the temperature of the melted dry material in the melted or poured vessel in a form that is not too hot prior to introduction of the mold. The temperature of the molten target material is lowered until substantially all of the excess heat in the melted dry material is removed. The reduced filament material should be substantially uniform and for most of the dip, the degree of reduction is controlled to be within two to 20 degrees F of the measured point of the (iv) metal or filament material, although the range is It can be adjusted according to the specific dry metal or alloy. The melting point of the amount can be determined as described in the US towel. The supply to the melting furnace in which the melting vessel is located is gradually reduced to reduce the temperature of the dry material refining in the melting vessel. According to the example in the following example, the melting of the material to the electric power of the service (4) can be gradually reduced by melting without sensing == to introduce the melting material to the 122261.doc 200811304 Before the mold, substantially all of the excess heat is removed. The mold may include a metal or ceramic mold including a plurality of inner walls having the desired shape of the splash (four) shape. Typical shapes of the manufactureable reduction target include However, it is not limited to 'rectangular, square or other polygonal shaped flat plates and discs. Unless it is used in the manufacture of investment molds (4), the present invention contemplates refining as needed after introducing the melted dry material into the mold. In the material
產生紊亂。對於大多數靶材料，將該熔化之靶材料直接灌 注到該模具中即滿足需要。可如美國專利4,832，112中所 述，可藉由電磁攪動、機械攪動及在將熔化之靶材料灌注 到該模具中時使該熔化物成為粉末（例如藉由將該熔化物 分成多個流或多個小滴）來交替地將該紊亂授予該模具中 該溶化之乾材料。 根據本發明，藉由以一速度從其中吸取熱量來使熔化之 靶材料在該模具中固化，以獲得該濺鍍靶中大致為等轴、 胞狀、無树突之顆粒結構。該固態（鑄態）賤鍍乾較佳在該 濺鍍靶中具有一為3或更小之等轴、胞狀ASTM顆粒大小。 控制該熱吸取速度以達到此等軸、胞狀顆粒結構。於某些 不例中，該熔化之靶材料與相對冷之模具之間的初始溫度 梯度高得足以在介面處產生一柱狀樹突顆粒區域。本發明 預想視需要將該模具加熱到一足夠高之升高之模具溫度， 以防止直接在該模具内壁附近形成大致為柱狀之顆粒。該 經固化之靶具有一網狀或接近網狀之期望之靶且在用作一 無之前僅需要最小之加工。 122261.doc 200811304 隨著模具縱橫比的增加，更迅速地從該固化之靶材料吸 取熱量越來越重要，以維持精細之微粒大小及相關聯之胞 狀結構及以使氣孔及可能之隔離之增加趨勢最小化。藉由 先前揭示之在將熔化之靶材料灌注到該模具中時所進行之 粉碎可促進熱量吸取之改良。 如果該固化之、鑄態濺鍍靶具有某些氣孔，則可藉由各 種技術將該氣孔清除，其包括使用習用之熱等靜氣壓製程 之對該鑄態濺鍍靶實施熱等靜壓（HIP),該熱等靜氣壓之 氣壓、溫度和時間參數將相依於所使用之特定靶金屬或合 金。美國專利4,832,112中對濺鍍靶之鑄態氣孔之控制及清 除進行了闡述。 出於進一步圖解說明本發明而不以任何形式對其進行限 制之目的’可將一具有27英吋（長度）乘以4.25英吋（寬度） 乘以0.2英吋（厚度）之矩形濺鍍靶澆鑄到一習用之預熱陶瓷 熔模模具中’該模具位於一習用之真空感應熔爐之下腔 中。該預熱溶模模具將包括一精密地複製該濺鍍把之期望 形狀之模穴。該包括（舉例而言）上文所述以鈷為主之合金 類型之靶金屬或合金可在真空條件下在該熔爐上腔1〇微米 以下被加熱至一高於其熔點約2〇_5〇度F之溫度以在一氧化 錘坩鋼中將其熔化。可逐漸減小坩鋼之感應線圈之功率直 至該炼化之靶材料係在該熔點之〇至“度^之内。然後，可 將該溶化之靶材料灌注到該模具中，該模具可包括一位於 該模具頂部之收斂管道，其強制在該模穴中心線處迅速地 局部固化。此可防止在中心線處形成相互連接之氣孔及允 122261.doc 11 - 200811304 許使鑄態濺鍍靶緻密，必要時，在29尺^氣壓下、2ι〇〇度 F下HIP該靶達1小時。產生之經HIp之濺鍍靶展示一細微、 等轴胞狀之顆粒結構。 儘管上文中闡述了本發明之特定實施例，但彼等熟悉此 項技術者應瞭解，本發明並不限於該等實施例，及在不背 4 離隨附申請專利範圍中所述之本發明之精神及範疇之情況 ' 下，可在其中作出修改及變更。 【圖式簡單說明】 _ 圖1係一在坩鍋中準備澆鑄到一鋼或陶瓷模具中之溶化 之靶材料之示意性透視圖。A disorder occurs. For most target materials, it is desirable to directly inject the molten target material into the mold. The melt can be made into a powder by electromagnetic agitation, mechanical agitation, and when the molten target material is poured into the mold, as described in U.S. Patent No. 4,832,112 (e.g., by dividing the melt into multiple streams) Or a plurality of droplets to alternately impart the disorder to the molten material in the mold. According to the present invention, the molten target material is solidified in the mold by drawing heat therefrom at a speed to obtain a substantially equiaxed, cell-like, dendritic particle structure in the sputtering target. The solid (as-cast) ruthenium plating preferably has an equiaxed, cell-like ASTM particle size of 3 or less in the sputter target. The heat extraction rate is controlled to achieve this isometric, cellular structure. In some instances, the initial temperature gradient between the molten target material and the relatively cold mold is high enough to create a columnar dendritic particle region at the interface. The present invention contemplates heating the mold to a sufficiently high elevated mold temperature as needed to prevent the formation of substantially columnar particles directly adjacent the inner wall of the mold. The cured target has a desired mesh or near mesh shape and requires minimal processing before being used as a no. 122261.doc 200811304 As mold aspect ratios increase, it is increasingly important to extract heat from the solidified target material more quickly to maintain fine particle size and associated cell structure and to isolate pores and possibly Increase the trend to a minimum. The improvement in heat extraction can be facilitated by the comminution previously disclosed in injecting the molten target material into the mold. If the cured, as-cast sputter target has certain pores, the pores can be removed by various techniques, including hot isostatic pressing of the as-cast sputter target using conventional hot isostatic gas pressure processes ( HIP), the gas pressure, temperature and time parameters of the hot isostatic gas pressure will depend on the particular target metal or alloy used. The control and removal of as-cast pores of a sputter target is described in U.S. Patent 4,832,112. For purposes of further illustrating the invention without limiting it in any way, a rectangular sputtering target having a length of 27 inches (length) multiplied by 4.25 inches (width) multiplied by 0.2 inches (thickness) can be used. Cast into a conventional preheated ceramic investment mold 'the mold is located in the cavity below a conventional vacuum induction furnace. The preheat mold will include a cavity that precisely replicates the desired shape of the sputter. The target metal or alloy comprising, for example, a cobalt-based alloy type as described above may be heated under vacuum to a furnace above 1 〇 micron to a temperature above about 2 〇 _5. The temperature of the temperature F is melted in a oxidized hammer steel. The power of the induction coil of the steel can be gradually reduced until the target material of the refining is within the range of the melting point. Then, the molten target material can be poured into the mold, and the mold can include a converging conduit at the top of the mold that is forced to partially solidify at the centerline of the mold cavity. This prevents the formation of interconnected pores at the centerline and allows the cast-off target to be cast. Dense, if necessary, HIP the target for 1 hour at 2 ft. F under a pressure of 29 ft. The resulting HIp-sputtered target exhibits a fine, equiaxed cellular structure. Specific embodiments of the present invention, but those skilled in the art should understand that the present invention is not limited to the embodiments, and the spirit and scope of the present invention described in the appended claims. Modifications and changes can be made therein. [Simplified Schematic] _ Figure 1 is a schematic perspective view of a molten target material prepared for casting into a steel or ceramic mold in a crucible.
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