3550pifl.doc/008 β? 五、發明説明（（） (請先閲讀背面之注意事項再填寫本頁) 本發明是有關於一種具有細緻均勻結構與組織的金屬 物品及其製造程序’尤其，對典型的金屬物品而言，將其 做成濺鍍靶會是特別有用的。 在電子工程學和半導體工業上，高純度之金屬和合金 的濺鍍靶，已被廣泛地用於灑鍍薄膜。因此，獲得大尺寸 的靶是很好的。 根據本發明的一較佳實施例，提供一種製程用於生產 具有細緻均句冶金的結構和組織之金屬物品，比如濺鑛 靶，包括： 1) 提供一四方形金屬條； 2) 將此四方形金屬條加熱至低於金屬再結晶溫度的 鍛造溫度； 3) 在被鍛造之金屬條的末端和用於鍛造金屬條之鍛 造機器的加壓板之間使用固態潤滑劑，以在鍛造期間降低 摩擦； 4) 將金屬條鍛造成具有約70%至90%之減少量的預定 金屬條之厚度； 5) 將已锻造的金屬條置放於約室溫下； 經濟部智慧財產局員工消費合作社印製 6) 將金屬條輾壓成金屬板，而每輾壓一輪回會使其 厚度減少，且每一輪回的輾壓足以提供近乎均勻之應變應 變分佈將；以及 7) 將金屬板再結晶回火。 在使用足夠厚度的固態潤滑劑之前，在四方形金屬條的兩 末端以機器製造淺開口（Shallow Packet)亦是有利的。 4 本紙張尺度適.用中國國家標準（CNS ) A4規格（210X297公釐） 3550pifl .doc/008 g-y --- _ 五、發明説明（') 較佳的是，在低於靜態再結晶之最小溫壞卞，锻造四方形 金屬條，然後在一段時間和溫度下輾壓（R〇n)和回火， 以提供靜態再結晶的初始階段。 根據每輾壓一輪回減少的量之最小値、輾壓輕的直徑 .和鍛造後預定的四方形金屬條厚度的關係，每運轉一輪回 .輾壓減少的量是可預期的。通常，在輾壓期間每輾壓—輪 回減少的量約爲10%至20%。 本發明的另一實施例包括金屬物品，比如濺鍍靶，具 有接近靜態再結晶的晶粒大小之最小値，在住何位置之晶 粒大小的差異小於約±3%，且在任何位置之組織的方位容 積比的分佈小於約±4%。 本發明能夠應用在不同金屬和合金上，其中此合金在 低於靜態再結晶的相對溫度下之溫度，表現好的延展性和 可加工性。在金屬之中可以應用在本發明的是Al、Ti、Ta、 Cu、Nb、Ni、Mo、Au、Ag、Re、Pt和其他類似此性質者， 及其合金。本方法的實施例包括將金屬錠塊製成半成品的 四方形金屬條之步驟，此步驟比如包括，融解、金屬錠塊 鑄件、均質化/溶解化熱處理、高溫加工到使鑄造結構崩 潰（Break Down)、以及在經四方形金屬條塑造和熱機械 處理而製造出產品後，此產品比如是濺鍍靶，之後完成四 方形金屬條的準備，且精煉冶金的結構和生產預定的組 織。藉由本發明的製程之實施例，使用冷/熱加工和回火 發展極細緻均勻的結構和堅固均勻的組織，如此可改善濺 鍍靶之效能。 5 本紙張尺度適用中國國家；^準（CNS ) A4規格（210X297公釐） ~~~ (請先閲讀背面之注意事項再填寫本頁) ---1----:-------P 裝. I I V - -6 經濟部智慧財產局員工消費合作社印製 經濟部智慧財產局員工消費合作社印製 A7 3550pifl.doc/008 扣 五、發明説明（、） 爲讓本發明之上述和其他目的、特徵、和優點能更明 顯易懂，下文特舉一較佳實施例，並配合所附圖式’作詳 細說明如下： 圖式之簡單說明： 第1圖係繪示在鎚打之初，四方形金屬條-薄膜潤滑 .劑的裝配； 第2圖係繪示在鎚打期間第1圖的剖面圖“C” ； 第3圖係繪示用於較長的圓柱狀金屬條之輾壓輥的起 始； 第4圖係繪示用於較短的圓柱狀金屬條之輾壓輥輾壓 車昆的起始； 第5圖係繪示再結晶的結構之晶粒大小和溫度的關係 圖，顯示在無摩擦鍛造/輾壓之後’再結晶回火對鈍Ti 合金的晶粒大小之影響； 第6A圖係顯示在無摩擦鍛造/輾壓和在375°C回火2 小時之後，鈍Ti的顯微結構（x200倍率）； 第6B圖係顯示在無摩擦鍛造/輾壓和在675°C回火2 小時之後，鈍Ti的顯微結構（x2.00倍率）； 第7A圖係繪示在無摩擦鍛造/輾壓和在375°C回火2 小時之後，鈍Ti的晶粒大小之分佈； 第7B圖係繪示在無摩擦鍛造/輾壓和在675°C回火2 小時之後，鈍Ti的晶粒大小之分佈；以及 第8圖保繪示在無摩擦鍛造/輾壓的製程之後，回火 溫度對鈍Ti的組織（X-射線強度比）的影響。 6 本紙張尺度適，用中國國家標準（CNS ) A4規格（210X297公釐） ---：------.1 袈 —------訂---Ί---Θ (請先閲讀背面之注意事項再填寫本頁) . A7 3550pifl.doc/008 五、發明説明（α) 其中，各圖標號與構件名稱之關係如下： (請先閲讀背面之注意事項再填寫本頁) H。：金屬條之初始厚度 h:金屬條之最後厚度 1 :初始的金屬條 2 :淺開口 3:薄片狀的固態潤滑劑 4 :鍛造平板 5 :開口的邊界 δ:薄膜厚度 D。：金屬條的直徑 δ。：開口深度 Τ :變形的區域 L:金屬條-輾壓輥的接觸長度 lu :金屬條的厚度 Φ:是輾壓輥的直徑 實施例 經濟部智慧財產局員工消費合作社印製 爲了使熱力學的處理達到最佳化，必須在再結晶回火 (Recrystallization Annealing )之即，獲得徹底 (Intensive)且均勻的應變（Strain)。典型上，耙是 從單一金屬條所製造的薄金屬圓盤，進行輾壓（Rolling) 或鎚打鍛造（Upsetting-forging)的操作。在兩種例子 中，初始的金屬條之厚度（H。）降低至最後厚度（h)，平 均的應變可以藉由下式計算： (1 ) ε = (1 - h/Ho)l00 % = [l - (M/M0)2/3]x 100 % 7 本紙張尺度適用中國國家標準（CNS ) A4規格（21 OX297公釐） A 7 3550pifl.doc/008 ^ 五、發明説明（〇 (請先閲讀背面之注意事項再填寫本頁) 其中M〇= Ho/D。和Μ = h/d分別是初始金屬條和加工產物 的高度-直徑比（Height-to-diameter Ratio)。加工產 物的高度-直徑比（M)由預定之靶的形狀而定的，初始金 屬條的高度-直徑比M。可能的範圍是從約1.0到〇·5時， .加工產物的高度-直徑比的範圍是從Μ = 0.07到Μ = 0.3， 且在先前描述的方程式（1)中應變的產率極限如下所示： (2) 73% <ε<83% 僅對薄靶而言，在方程式（2)中的應變是足以高到使 靜態再結晶最佳化。但甚至對這些在整個金屬條體積中的 應變分佈上爲非均勻的靶，可能在一些區域會顯著地降低 其應變量。而且，在鍛造加壓或輾壓硏磨的能力之要求 上，需要提供上式方程式（2)的應變，對大的靶而言’金 屬條可能太大以致於不能做一些應用。而且’它們可能會 藉由輾壓或鍛造的操作而限制達到的應變。 經濟部智慧財產局員工消費合作社印製 輾壓極適合用在製造薄且大的靶。但有利之初始的金 屬條比（Μ。）應小於1，否則在長圓柱金屬條的輾壓期間 其末端的影響，會使得應變分佈非常不均勻。此外’爲了 提供近似均勻應變，甚至對薄金屬條而言，輾壓輥的直徑 應該顯著地大於金屬條的厚度，且每輾壓一輪回減少的量 會影響其結果。由於锻造之故’輾壓的金屬條可以具有似 凹陷形狀，且在接觸的表面具有最大的應變’以及在金屬 條的中間部份具有最小的應變，而金屬條的中間部份係不 足以將再結晶最佳化且不足以發展成最有用的結構。最近 發表的日本專利案號08-269701中，係描述經由普通和低 8 本紙張尺度適用中國國家標準（CNS ) Α4規格（210X297公釐） A7 3550pifl_doc/008 B7 _ 五、發明説明（（：） 溫回火之徹底的片狀冷輾壓製程，來製造Ti IE °然而’ 此技術不能應用到板狀，雖然在一些靶描述細緻晶粒尺 寸，但日本專利資料顯示其在晶粒直徑上有大的偏差。 來自於鍛造的非均勻之應變遠大於來自於輾壓的非 .均勻之應變。因爲接觸摩擦，因此在金屬條的中央區域出 現大面積的“死金屬（Dead Metal) ”帶。如此將導致在 這些帶內產生低應變，且對薄金屬條產生高壓和負載。自 具有大厚度-直徑比之大金屬條鎚打成大靶’需要非常巨 大的壓力和昂貴的工具，但卻不能產生具有均勻的晶粒直 徑之產物。此即爲锻造操作通常僅使用於鑄造錠塊的熱崩 潰之原因。 在日本專利案號08-232061中，描述一種克服這些問 題的方法。其係描述在溫度低於相轉移溫度時’ Ti靶之锻 造和輾壓的結合。此製程使用低於相轉移溫度但高於靜態 再結晶的溫度，用於大量加工的物質。結果，此製程不能 使再結晶最佳化，且不能發展非常細緻和均勻的結構/組 織。 相對於鍛造，本發明包括： 1) 進行無摩擦鎚打之鍛造步驟，以提供無物質龜裂 和壓力過負載之均勻的壓力-應變和徹底的加工；以及 2) 在低於靜態再結晶的最低溫度下進行鍛造步驟， 以提供最細緻且最均勻的結構/組織。可以將這些鍛造、 輾壓和回火的步驟最佳化，以提供成本效率的製程和靶的 效能。 9 (請先閲讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 ---------------ΰ —-----1TU---------:---r----- 本紙^尺度適用中國國家標準（€奶）人4規格(210父297公釐） ~ ~ A7 B73550pifl.doc / 008 β? 5. Description of the invention (() (Please read the notes on the back before filling out this page) The present invention relates to a metal article with a fine and uniform structure and organization and its manufacturing process. Sputtering targets can be particularly useful for typical metal objects. Sputtering targets for high-purity metals and alloys have been widely used for sputtering thin films in the electronics engineering and semiconductor industries. Therefore, it is very good to obtain a large-sized target. According to a preferred embodiment of the present invention, a process is provided for producing metal objects with fine homogeneous metallurgical structure and organization, such as splatter targets, including: 1) Provide a square metal bar; 2) heat this square metal bar to a forging temperature below the metal recrystallization temperature; 3) at the end of the forged metal bar and the pressure plate of the forging machine for forging the metal bar Use a solid lubricant between them to reduce friction during forging; 4) Forge metal bars to a predetermined metal bar thickness with a reduction of about 70% to 90%; 5) Place the forged metal bars At about room temperature; printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs 6) Rolling metal strips into metal plates, and each round of rolling will reduce its thickness, and the rolling of each round is sufficient to provide almost uniform The strain-strain distribution will be; and 7) the metal plate will be recrystallized and tempered. Before using a solid lubricant of sufficient thickness, it is also advantageous to machine the shallow openings at both ends of the square metal strip. 4 The paper size is appropriate. Use Chinese National Standard (CNS) A4 specification (210X297 mm) 3550pifl.doc / 008 gy --- _ 5. Description of the invention (') Preferably, the minimum Warm badly, forged a square metal bar, and then rolled (Ron) and tempered at a time and temperature to provide an initial stage of static recrystallization. According to the relationship between the minimum amount of rolling reduction per rolling cycle, the light rolling diameter, and the predetermined thickness of the square metal bar after forging, the rolling reduction is expected per rotation. Generally, the reduction in each rolling-round cycle during rolling is about 10% to 20%. Another embodiment of the present invention includes a metal article, such as a sputtering target, which has a minimum grain size close to static recrystallization, where the difference in grain size is less than about ± 3%, and the structure at any location The distribution of the azimuthal volume ratio is less than about ± 4%. The present invention can be applied to different metals and alloys, where the alloy exhibits good ductility and processability at a temperature lower than the relative temperature of static recrystallization. Among the metals that can be used in the present invention are Al, Ti, Ta, Cu, Nb, Ni, Mo, Au, Ag, Re, Pt and others with similar properties, and alloys thereof. An embodiment of the method includes the step of making a metal ingot into a semi-finished square metal bar. This step includes, for example, melting, metal ingot casting, homogenization / dissolution heat treatment, and high temperature processing to break down the casting structure (Break Down ), And after manufacturing a product by shaping and thermomechanical processing of a square metal strip, this product is, for example, a sputtering target, after which the preparation of the square metal strip is completed, and the metallurgical structure and the predetermined organization are refined. With the embodiment of the process of the present invention, the use of cold / hot working and tempering to develop an extremely fine and uniform structure and a strong and uniform structure can improve the effectiveness of the sputtering target. 5 This paper size is applicable to China; ^ Standard (CNS) A4 size (210X297 mm) ~~~ (Please read the precautions on the back before filling this page) --- 1 ----: ----- --P Pack. IIV--6 Printed by the Consumers 'Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs Printed by the Consumers' Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs Printed A7 3550pifl.doc / 008 Other objects, features, and advantages can be more clearly understood. The following is a detailed description of a preferred embodiment in conjunction with the accompanying drawings' as follows: Brief description of the drawings: Figure 1 is shown in the hammer At the beginning, the square metal bar-film lubrication. Assembly of the agent; Figure 2 shows the sectional view "C" of Figure 1 during hammering; Figure 3 shows the use of longer cylindrical metal bars The beginning of the rolling roll; Figure 4 shows the starting of the rolling roller rolling car for a short cylindrical metal strip; Figure 5 shows the grain size and temperature of the recrystallized structure , Showing the effect of 'recrystallization tempering on the grain size of blunt Ti alloys after frictionless forging / rolling; section 6A Figure 6 shows the microstructure (x200 magnification) of blunt Ti after frictionless forging / rolling and tempering at 375 ° C for 2 hours. Figure 6B shows the frictionless forging / rolling and tempering at 675 ° C. After 2 hours, the microstructure of the passive Ti (x2.00 magnification); Figure 7A shows the distribution of the grain size of the passive Ti after frictionless forging / rolling and tempering at 375 ° C for 2 hours; Fig. 7B shows the distribution of grain size of blunt Ti after frictionless forging / rolling and tempering at 675 ° C for 2 hours; and Fig. 8 is a drawing showing after the frictionless forging / rolling process The effect of tempering temperature on the structure (X-ray intensity ratio) of blunt Ti. 6 The size of this paper is appropriate, using the Chinese National Standard (CNS) A4 specification (210X297 mm) ---: ------. 1 袈 -------- order --- Ί --- Θ ( Please read the precautions on the back before filling this page). A7 3550pifl.doc / 008 V. Description of the Invention (α) Among them, the relationship between each icon number and component name is as follows: (Please read the precautions on the back before filling out this page ) H. : Initial thickness of the metal strip h: final thickness of the metal strip 1: initial metal strip 2: shallow opening 3: thin flake solid lubricant 4: forged flat plate 5: opening boundary δ: film thickness D. : Diameter δ of the metal strip. : Depth of opening T: Deformed area L: Contact length of metal bar-rolling roller lu: Thickness of metal bar Φ: Diameter of rolling roller To achieve the optimization, an intensive and uniform strain (Strain) must be obtained during the recrystallization annealing (Recrystallization Annealing). Typically, a harrow is a thin metal disc made from a single metal strip, which is subjected to rolling or upsetting-forging operations. In both examples, the initial thickness (H.) of the metal strip is reduced to the final thickness (h), and the average strain can be calculated by the following formula: (1) ε = (1-h / Ho) 100% = [ l-(M / M0) 2/3] x 100% 7 This paper size is applicable to the Chinese National Standard (CNS) A4 specification (21 OX297 mm) A 7 3550pifl.doc / 008 ^ 5. Description of the invention (〇 (please first Read the notes on the back and fill in this page) where M〇 = Ho / D. And M = h / d are the height-to-diameter ratio of the original metal bar and the processed product. The height of the processed product -The diameter ratio (M) is determined by the shape of the predetermined target. The height of the initial metal strip-the diameter ratio M. The possible range is from about 1.0 to 0.5. The range of the height-diameter ratio of the processed product is From M = 0.07 to M = 0.3, and the yield limit of strain in the previously described equation (1) is as follows: (2) 73% < ε < 83% For thin targets only, in equation (2 The strain in) is high enough to optimize static recrystallization. But even for these targets where the strain distribution is non-uniform throughout the volume of the metal strip, it may be some The area will significantly reduce its strain. Also, in terms of the ability to forge pressure or roll honing, the strain of equation (2) above needs to be provided. For large targets, the 'metal strip may be too large to cause It cannot be used for some applications. And 'they may limit the strain reached by rolling or forging operations. The printing of printed materials by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs is very suitable for manufacturing thin and large targets. But it is advantageous The initial metal bar ratio (M.) should be less than 1, otherwise the influence of the ends during the rolling of the long cylindrical metal bar will make the strain distribution very uneven. In addition, in order to provide approximately uniform strain, even thin metal bars In terms of diameter, the diameter of the rolling roller should be significantly larger than the thickness of the metal strip, and the reduction in the number of rounds per rolling will affect the result. Due to forging, the 'rolled metal strip can have a concave shape and be in contact with The surface has the largest strain 'and the smallest strain in the middle part of the metal strip, which is not enough to optimize the recrystallization and not enough Developed into the most useful structure. In the recently published Japanese patent case No. 08-269701, it is described that the standard of the Chinese paper (CNS) A4 (210X297 mm) is applicable through ordinary and low 8 paper sizes A7 3550pifl_doc / 008 B7 _ 5 2. Description of the invention ((:) A thorough sheet cold rolling process of warm tempering to make Ti IE ° However, 'This technology cannot be applied to the plate shape. Although the fine grain size is described in some targets, Japanese patent data show that It has a large deviation in grain diameter. The non-uniform strain from forging is much larger than the non-uniform strain from rolling. Due to contact friction, a large area of "dead metal" bands appeared in the central area of the metal strip. This will result in low strain in these bands and high pressure and load on thin metal strips. Hammering a large metal bar with a large thickness-to-diameter ratio into a large target 'requires very large pressure and expensive tools, but cannot produce a product with a uniform grain diameter. This is why forging operations are usually used only for the thermal collapse of cast ingots. In Japanese Patent No. 08-232061, a method for overcoming these problems is described. It describes the combination of forging and rolling of a 'Ti target at temperatures below the phase transfer temperature. This process uses substances that are below the phase transfer temperature but above the static recrystallization temperature for mass processing. As a result, this process cannot optimize recrystallization and cannot develop very fine and uniform structures / structures. With respect to forging, the present invention includes: 1) a frictionless hammering forging step to provide uniform pressure-strain and thorough processing without material cracking and pressure overload; and 2) at a temperature below static recrystallization The forging step is performed at the lowest temperature to provide the finest and most uniform structure / structure. These forging, rolling, and tempering steps can be optimized to provide cost-effective processes and target effectiveness. 9 (Please read the notes on the back before filling out this page) Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs ------- 1TU --- ------: --- r ----- The paper ^ size applies to the Chinese national standard (€ milk) person 4 specifications (210 father 297 mm) ~ ~ A7 B7
3550pifl.doc/00S 五、發明説明（？） 接著請參照第1圖，初始的金屬條（1)有圓柱狀和體 積以及長度-直徑比M。。進行鎚打之前，在金屬條的末端 製造兩個淺開口（2)。較佳的是冷鎚打，但在一些例子中， 金屬條的預熱和使其低於靜態再結晶的溫度，可以用來降 .低加工壓力和負載。將兩薄片的固態潤滑劑（3)放置在金 .屬條的末端和鍛造平板（4)之間，而鍛造平板（4)係於一壓 力下裝設。此外，並發現在加工的條件下，使用顯示兼具 黏著性與伸縮性特性的潤滑劑高分子，比如聚乙烯、聚四 氟乙烯或聚亞胺酯，有最佳的結果。 如第1圖和第2圖所示，根據金屬條的直徑D。，薄膜 厚度（δ)的變化可從0.5mm至2.5mm，然而薄膜大小（A) 應超過D。。開口深度（δ。）略小於薄膜厚度（δ)是有利的， 且開口的邊界（5)具有約5腿至20mm的寬度S。 根據本發明，使用兼具黏著性與伸縮性的高分子薄膜 來完全分離金屬條和工具。在鎚打的期間，高分子塡滿開 口，且流入與金屬條接觸。一些多餘的高分子從開口（如 第2圖所示）流出，且沿著金屬條末端在流動的方向提供 低正摩擦，結果消除死金屬帶且改善金屬條的穩定度。其 中發現本發明初始的金屬條比（M。）可與Μ〇= 1.5 —樣大’ 且高分子潤滑劑薄膜能夠使部份減少的量提髙至ε〜 75%。因爲初始金屬條比Μ。增加至1.5,對可達到的應變之 限制（請看方程式（1) ’其遠好於方程式（2)) (3) 87% < ε < 92% 與均勻應變分佈相連結，提供在大部份的例子中一種最佳 10 本紙張尺度適用中國國家標準（CNS ) Α4規格（210Χ297公釐） —.1.—!I-υ-----i.^—I—：—©I (請先閲讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 A7 3550pifl .doc/008 gy 五、發明説明U ) 化的再結晶。而且，在鍛造之後（到達Μ = 0.16)，薄金 .屬條提供了隨後之輾壓的最佳條件。 輾壓初始鍛造的金屬條，以更進一步降低其厚度。可 以使用冷或熱的輾壓。輾壓可能進行二或四次，其在方向 .上是彼此相互地垂直，用以產生似圓形狀的產品。在藉由 控制輾壓輥的直徑-金屬條厚度比（Φ/Η)、金屬條厚度-直徑比（M)和每輾壓一輪回之減少的量，使在輾壓的期 間提供最均勻的應變分佈是很重要的。一個重要的觀點是 避免在開始輾壓時（如第3圖所示）沿著圓柱金屬條（+ ) 的自由表面（2)變形。其中發現在變形的區域（T)幾乎等於 金屬條-輾壓輥的接觸長度（L)，且在第一次輾壓一輪回之 後（如第4圖所示），如果接觸長度（L)超過金屬條的厚 度b時會消除變形。換句話說，如果L > Η，則 (4) ^4(1-£)2_+ £2_ ν } Η_ 2ε Φ ^ 4(l-g)2 + g2 ~Η~ Υε 其中Φ是輾壓輥的直徑，ε = (l-h/H)100%是每輾壓一輪回 輾壓減少的量。利用方程式（4)來計算不同的減少的量， 結果如表1所示。 表1 ε 5% 10% 15% 20% 25% φ/Η 36 16 9.7 6.5 4.6 就如所看到的，在平均減少的量爲15%或更低的情況 下，輾壓輥的直徑應至少約10倍（在表1中之9.7)，與 11 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） (請先閲讀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 Λ7 B7 3550pifl.doc/008 五、發明説明（气） 圓柱金屬條的厚度一樣大。換言之，使用薄金屬條用於輾 壓而沒有鎚打’降低了可能減少的量（1)。傳統的靶輾壓 可避免兩種不利的情況，即非均勻性和低減少的量在最佳 化的結構是相當不能被接受。在本發明中，藉由初始的金 .屬條鎚打到所需的厚度（H)，以提供輾壓輥直徑-金屬條 厚度（φ/H)之高比例。鎚打操作的同時，提供小於約0.3 的預輾壓金屬條比（m)，如此對獲得沿著金屬條降低均 勻的輾壓是有用的。部份輾壓每輾壓一輪回減少的量從約 10%至20%，在最後的產物對近乎均勻的應變分佈亦有用。 輾壓減少的量低於約10%時，在金屬條的表面有較高的應 變，然而減少的量大於約18%時，則在金屬條的中間部份 有較高的應變。這些所有的參數用來定義此最佳實施例， 以用於對靶進行鎚打和輾壓，以產生最佳的結果。 在靶製程的最後步驟是再結晶回火。對許多金屬和合 金而言，方程式（3)的應變已足夠做最佳化靜態再結晶° 爲了達到此目的，首先需要最低的溫度來開始靜態再結 晶，且然後應決定所需之最短的時間以完成所有金屬條的 體積。相對應的結構在每一局部的區域內具有最小的晶粒 尺寸，且最低的晶粒直徑分佈。在本發明的方法於金屬條 的任何部份亦提供均勻的應變的同時，可以獲得靜態再結 晶的最小溫度以做爲對整個金屬條在最短的時間內之蕺 佳的溫度。此結果對靶的產物而言，有非常細緻和均勻的 結構，以及堅固、均勻的組織。 本發明的另一較佳實施例，係以很少的步驟持續地降 12 (請先聞绩背面之注意事項再填寫本頁)3550pifl.doc / 00S V. Description of the Invention (?) Next, please refer to Fig. 1. The original metal strip (1) has a cylindrical shape and a volume and a length-diameter ratio M. . Before hammering, make two shallow openings at the end of the metal strip (2). Cold hammering is preferred, but in some examples, the preheating of the metal strip and its temperature below the static recrystallization temperature can be used to reduce processing pressure and load. Two pieces of solid lubricant (3) are placed between the end of the metal bar and the forged plate (4), and the forged plate (4) is installed under a pressure. In addition, it has been found that under processing conditions, the use of a lubricant polymer that exhibits both adhesion and stretch properties, such as polyethylene, polytetrafluoroethylene or polyurethane, has the best results. As shown in Fig. 1 and Fig. 2, according to the diameter D of the metal bar. The film thickness (δ) can vary from 0.5mm to 2.5mm, but the film size (A) should exceed D. . It is advantageous that the opening depth (δ.) Is slightly smaller than the film thickness (δ), and the boundary (5) of the opening has a width S of about 5 legs to 20 mm. According to the present invention, a polymer film having both adhesiveness and elasticity is used to completely separate metal bars and tools. During hammering, the polymer fills the opening and flows into contact with the metal strip. Some excess polymer flows out of the opening (shown in Figure 2) and provides low positive friction in the direction of flow along the end of the metal strip, resulting in the elimination of dead metal bands and improved metal strip stability. It was found that the initial metal strip ratio (M.) of the present invention can be as large as M0 = 1.5-and that the polymer lubricant film can reduce the amount to ε ~ 75%. Because the initial metal strip is more than M. Increase to 1.5 to limit the achievable strain (see equation (1) 'which is much better than equation (2)) (3) 87% < ε < 92% is linked to a uniform strain distribution, providing In some examples, the best 10 paper sizes are applicable to the Chinese National Standard (CNS) A4 specification (210 × 297 mm) —.1 .—! I-υ ----- i. ^ — I —: — I (Please read the notes on the back before filling out this page) Printed by A7 3550pifl .doc / 008 gy of the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs 5. Recrystallization of the invention. Moreover, after forging (reaching M = 0.16), the thin gold bars provide the best conditions for subsequent rolling. The initially forged metal bar is rolled to further reduce its thickness. Cold or hot rolling can be used. The rolling may be performed two or four times, which are perpendicular to each other in the direction. To produce a round-like product. By controlling the diameter-to-metal strip thickness ratio (Φ / Η) of the rolling roller, the thickness-to-diameter ratio (M) of the metal strip, and the amount of reduction per rolling cycle, the most uniform during the rolling is provided. The strain distribution is important. An important point is to avoid deformation along the free surface (2) of the cylindrical metal strip (+) at the beginning of rolling (as shown in Figure 3). It was found that the deformed area (T) was almost equal to the contact length (L) of the metal strip-rolling roller, and after the first rolling cycle (as shown in Figure 4), if the contact length (L) exceeded The thickness b of the metal strip eliminates deformation. In other words, if L > Η, then (4) ^ 4 (1- £) 2_ + £ 2_ ν} Η_ 2ε Φ ^ 4 (lg) 2 + g2 ~ Η ~ Υε where Φ is the diameter of the rolling roller , Ε = (lh / H) 100% is the amount of rolling reduction per rolling round. Equation (4) was used to calculate different reductions. The results are shown in Table 1. Table 1 ε 5% 10% 15% 20% 25% φ / Η 36 16 9.7 6.5 4.6 As you can see, with an average reduction of 15% or less, the diameter of the rolling roller should be at least About 10 times (9.7 in Table 1) and 11 paper sizes are applicable to Chinese National Standard (CNS) A4 specifications (210X 297 mm) (Please read the precautions on the back before filling this page) Order the intellectual property of the Ministry of Economic Affairs Printed by the Bureau's Consumer Cooperatives Λ7 B7 3550pifl.doc / 008 5. Description of the Invention (Gas) The thickness of the cylindrical metal bar is the same. In other words, using a thin metal strip for rolling without hammering ' reduces the amount that may be reduced (1). Traditional target rolling can avoid two unfavorable situations, namely non-uniformity and low reduction in the optimized structure is quite unacceptable. In the present invention, the initial thickness of the metal strip is hammered to the required thickness (H) to provide a high ratio of the rolling roll diameter to the metal strip thickness (φ / H). At the same time as the hammering operation, a pre-rolled metal strip ratio (m) of less than about 0.3 is provided, which is useful for obtaining a uniform rolling reduction along the metal strip. Partial rolling decreases from about 10% to 20% per rolling cycle, and the final product is also useful for nearly uniform strain distribution. When the rolling reduction is less than about 10%, there is a higher strain on the surface of the metal strip, while when the reduction is greater than about 18%, there is a higher strain in the middle part of the metal strip. All these parameters are used to define this preferred embodiment for hammering and rolling the target to produce the best results. The final step in the target process is recrystallization tempering. For many metals and alloys, the strain of equation (3) is sufficient to optimize static recrystallization. To achieve this, the lowest temperature is required to begin static recrystallization first, and then the shortest time required should be determined To complete the volume of all metal bars. The corresponding structure has the smallest grain size and the lowest grain diameter distribution in each local area. While the method of the present invention also provides uniform strain to any part of the metal strip, the minimum temperature for static recrystallization can be obtained as the optimum temperature for the entire metal strip in the shortest time. This result has a very fine and uniform structure and a strong, uniform structure for the target product. Another preferred embodiment of the present invention is to continuously reduce the number of steps in 12 steps (please read the notes on the back of the report before filling out this page)
、1T 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） 經濟部智慧財產局員工消費合作社印製 Μ 3550pifl.doc/008 β? 五、發明説明（〔。） 低金屬條的厚度，以及在每一步驟薄膜潤滑劑的再回收， 來進行鍛造。鍛造的方法可以延伸到降低金屬條厚度，而 其在無摩擦情況且在相當低壓力和負載下之均勻的應變 並沒有變形。如果鍛造繼續進行至最後的靶之厚度，而沒 .有進行輾壓，則提供對應的鍛造組織做爲靶。相同地，在 特別的例子中，根據本發明，可以在沒有鍛造下進行具有 近乎均勻應變分佈之輾壓。 以下的例子描述本發明的一較佳實施例。 將高鈍度的鈦鑄造成直徑300mm的錠塊，且藉由在800 °C的高溫下以衝模打造成直徑130mm的金屬竿。然後，從 130mm的金屬竿切割成長度162mm的金屬條。在金屬條的 末端用機器製造成直徑120mm且厚度1mm的開口。在35〇 °C的溫度鎚打金屬條使其厚度變成54mm。使用150x150mm2 和厚度1.2mm的鐵氟龍薄膜，做爲無摩擦鎚打的潤滑劑。 此後，以直徑915mm的金屬乳輥之冷輾壓進行八次，在45。 的角度下沿著四個方向輾壓一輪回有12%的部份減少量。 越過輾壓金屬條的厚度之金屬試棒（Coupon)，被從 中間、半徑長度的中間和外部的區域切斷，並在不同的溫 度下回火2小時（h)。金屬試棒的兩平面，一個接近表 面而另一個接近中間部份，在此對其結構和組織做審慎地 硏究，而其顯微照片如第6A圖和第6B圖所示。 在另一例子中，則藉由以上描述的製程製造Ta濺鍍 靶。Ta靶產物的組成如表2所示’ Ta靶包括99.95%的Ta 和如所示之表2的平衡。 13 ϋ張尺度適用中國國家標準（CNS ) A4規格（210X297^^1 ~~ (請先閎讀背面之注$項再填寫本頁) 釘 3550pin.doc/008 五、發明説明（（（） A7 B7 表2 兀 素 典型 元 素 典型 C 10 Ca <5 0 15 Fe 15 N 15 Mg <5 Η <5 Μη 40 Κ 0.001 Mo 40 Li 0.001 Nb 150 Na 0.001 Ni <5 A1 <5 Si 15 B 2 Sn <5 Cu <5 Ti 5 Co <5 W 25 Cr <5 Zr <5 (諳先閲绩背面之注意事項再填寫本頁) 訂 單位爲ppm。 藉由LECO分析C、0、N和Η。 藉由SIMS分析Na、Li和Κ。 藉由ICP分析金屬元素。 第5圖顯示平均的Ti晶粒大小對回火溫度的影響。 靜態再結晶的最低溫度約爲375°C。對應於平均粒晶大小 6μιη之非常細緻的結構，亦證明晶粒直徑之低的局部分 佈，以及在垂直於靶表面具有65%的方位體積比之堅固的 組織（1013)(第8圖）。回火溫度的增加，會導致徹底 的晶粒成長，且僅中度堅固的組織之晶粒大小的分佈範圍 14 -0. 經濟部智慧財產局員工消費合作社印製 本紙張尺度適用t國國家標準（CNS ) A4規格（210X297公釐） A7 3550pifi-d〇c/008 B7 ______----- 五、發明説明（（〜） 較大。第6A圖和第6B圖所示之顯微照片’顯示分別在無 摩擦鍛造/輾壓、在375°C回火2小時、和在675。〇回火2 小時後，純Ti的結構。在靶的任何—點’對不同金屬試 棒之結構和組織進行分析’沒偵測到可顯著分辨的結果。 在不同靶位置之平均晶粒大小的分佈之精確度小於約 ±3%，且組織的方位體積比之分佈之精確度小於±4%’而此 精確度與量測的方法有關。第7A圖和第7B圖係分別描述 對應於第6A圖和第6B圖的結構之純Ti的晶粒大小分佈 圖。 本發明一項重要的優點是，製造出非常細緻和均勻的 結構以及在靶任何一點有堅固均勻的組織’而這些在以前 是無法達到的。此方法提供一種靶’其在濺鍍靶的效能上 具有顯著的改進。 . 本發明的較佳實施例的特徵描述如下： 1) 在由無摩擦力鎚打鍛造和輾壓所組合之熱機械的 製程期間，處理金屬條； 2) 在鎚打操作期間之無摩擦鍛造，其中此鎚打操作 可以改善沿接觸表面的正摩擦和增加製程的穩定性； 3) 鎚打操作的預定參數，用來增加累積的應變、降 低壓力的接受力和能夠有效輾壓； 4) 輾壓條件的預定參數，使能夠生產近於均句應變 分佈和圓柱狀（對濺鍍靶而言）的產品； 5) 使用靜態再結晶的最低溫度做爲回火的溫度；以 及 15 (請先閱讀背面之注意事項再填寫本頁)、 1T Printed by the Intellectual Property Bureau of the Ministry of Economic Affairs ’Consumer Cooperatives This paper is printed in accordance with the Chinese National Standard (CNS) A4 specification (210X297 mm) Printed by the Employee ’s Cooperatives of the Intellectual Property Bureau of the Ministry of Economy M 3550pifl.doc / 008 β? Explain ([.) The thickness of the low metal strip, and the recycling of the thin film lubricant at each step, for forging. The method of forging can be extended to reduce the thickness of the metal strip, without strain and uniform deformation under relatively low pressure and load without friction. If forging continues to the final target thickness without rolling, a corresponding forged structure is provided as a target. Similarly, in a specific example, according to the present invention, rolling having a nearly uniform strain distribution can be performed without forging. The following example describes a preferred embodiment of the present invention. High inertness titanium was cast into ingots with a diameter of 300 mm, and a metal rod with a diameter of 130 mm was punched with a die at a high temperature of 800 ° C. Then, a metal rod having a length of 162 mm was cut from a 130 mm metal rod. An opening having a diameter of 120 mm and a thickness of 1 mm was machine-made at the end of the metal bar. The metal bar was hammered to a thickness of 54 mm at a temperature of 35 ° C. Use a Teflon film with a thickness of 150x150mm2 and a thickness of 1.2mm as the lubricant for frictionless hammering. Thereafter, cold rolling was performed eight times at 45 with a metal emulsion roller having a diameter of 915 mm. Rolling a cycle in four directions at an angle of 12% has a partial reduction of 12%. A metal coupon (Coupon) over the thickness of the rolled metal strip is cut from the middle, the middle and outer areas of the radius length, and tempered at different temperatures for 2 hours (h). The two planes of the metal test rod, one near the surface and the other near the middle, are carefully examined for its structure and organization, and the photomicrographs are shown in Figures 6A and 6B. In another example, a Ta sputtering target is manufactured by the process described above. The composition of the Ta target product is shown in Table 2. The Ta target includes 99.95% Ta and the balance of Table 2 shown. 13 Yee scales are applicable to Chinese National Standards (CNS) A4 specifications (210X297 ^^ 1 ~~ (Please read the note on the back before filling in this page) Nail 3550pin.doc / 008 5. Description of the invention ((() A7 B7 Table 2 Typical elements of typical elements Typical C 10 Ca < 5 0 15 Fe 15 N 15 Mg < 5 Η < 5 Μη 40 Κ 0.001 Mo 40 Li 0.001 Nb 150 Na 0.001 Ni < 5 A1 < 5 Si 15 B 2 Sn < 5 Cu < 5 Ti 5 Co < 5 W 25 Cr < 5 Zr < 5 (谙 Notes on the back of the results before filling out this page) Orders are in ppm. Analysis by LECO C , 0, N, and Η. Analysis of Na, Li, and K by SIMS. Analysis of metal elements by ICP. Figure 5 shows the effect of average Ti grain size on the tempering temperature. The lowest temperature for static recrystallization is about 375 ° C. Corresponding to a very fine structure with an average grain size of 6μιη, it also proves that the local distribution of the grain size is low, and the solid structure (1013) with an azimuth-volume ratio of 65% perpendicular to the target surface (No. 8 Figure). Increasing the tempering temperature will lead to thorough grain growth, and only the distribution range of the grain size of the moderately strong structure 14 -0. The paper size printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs applies to the national standard (CNS) A4 specification (210X297 mm) A7 3550pifi-d〇c / 008 B7 ______----- V. Invention Explanation ((~) is larger. The photomicrographs shown in Figures 6A and 6B 'show the frictionless forging / rolling, tempering for 2 hours at 375 ° C, and tempering for 2 hours at 675 °. Later, the structure of pure Ti. At any point of the target, 'analyzing the structure and microstructure of different metal test bars' did not detect a significantly distinguishable result. The accuracy of the average grain size distribution at different target locations Less than about ± 3%, and the accuracy of the distribution of the azimuth-volume ratio of the tissue is less than ± 4% ', and this accuracy is related to the measurement method. Figures 7A and 7B are respectively described corresponding to Figures 6A and 7B. The grain size distribution of pure Ti in the structure of Figure 6B. An important advantage of the present invention is that it produces a very detailed and uniform structure and a solid and uniform structure at any point of the target, which were previously unattainable This method provides a target 'its effectiveness in sputtering targets It has significant improvements. The characteristics of the preferred embodiment of the present invention are described as follows: 1) during the thermomechanical process of the combination of forging and rolling by frictionless hammering, the processing of metal bars; 2) during the hammering operation During frictionless forging, this hammering operation can improve the positive friction along the contact surface and increase the stability of the process; 3) The predetermined parameters of the hammering operation are used to increase the accumulated strain, reduce the pressure acceptance, and can effectively Rolling; 4) Predetermined parameters of the rolling conditions, which enable the production of near-uniform strain distribution and cylindrical (for sputtering targets) products; 5) Use the lowest temperature for static recrystallization as the tempering temperature ; And 15 (Please read the notes on the back before filling out this page)
---1T 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） A7 3550pifl.doc/008 五、發明説明（（，） 6)生產具有非常細緻且均勻結構和均勻堅固組織的 濺鍍靶，而這些以前是無法達到的。 (請先閱讀背面之注意事項再填窝本頁) 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（2丨0X297公釐）--- 1T The paper printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs is suitable for this paper. It uses the Chinese National Standard (CNS) A4 specification (210X297 mm) A7 3550pifl.doc / 008 V. Description of the invention ((,) 6) Production Sputtering targets with very fine and uniform structure and uniformly strong structure that were previously unattainable. (Please read the precautions on the back before filling in this page) Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs This paper applies the Chinese National Standard (CNS) A4 specification (2 丨 0X297 mm)