1227279 玖、發明說明： 【發明所屬之技術領域】 本發明係關於一種可熱安定地形成矽化物（NiSi)膜、 且靶之塑性加工性良好之特別適用於閘極材料（薄膜）之製 造之鎳合金濺鍍靶及其製造方法。 、 【先前技術】 最近，在閘極材料方面藉由自動對準矽化物 (sal1C1de)程序之NiSi膜的利用逐漸受到重視。錄相較於 始在自動對準石夕化物程序中能以較少之石夕的消耗量來形成 石夕化物膜，此為其特徵所在。又，NiSi與石夕化刪樣具 有細線電阻不易因配線之微細化而上升之特徵。 基於前述理由，在閘極材料方面乃考慮以鎳來取代昂 貴的鈷。 —仁疋使用NlSl的情況，容易發生相轉變而成為更安 疋的相NiSh ’存在著界面粗糙度之惡化與高電阻化之問 題。又，尚有容易發生膜之凝集或出現過多之石夕化物化之 問題。 以往，使用石夕化錄等膜的情況，係採用於Ni或c〇膜 匕设以T i N等之金屬氧化物膜後進行退火，藉此，來防 切化物膜形成時與氧發生反應而形成絕緣膜之技術。此 日t ’為了防止氧與Ni起反應而形成具凹凸之絕緣膜，乃 使用了 TiN。 田凹凸小的h況，由於到NiSi膜與源極/汲極擴散層 之接合處的距離變長’所以可抑制接合漏茂。其他之包覆 1227279 膜尚有 TiC、TiW、TiB、WB2、WC、BN、AIN、Mg3N2、CaN、 Ge3N4、TaN、TbNi2、VB2、VC、ZrN、ZrB 等（參見日本專利 特開平7 - 3 81 Ο 4號公報）。 又’習知技術被質疑N i S i在石夕化物材料中非常容易氧 化，於NiSi膜與Si基板之界面區域形成大的凹凸，會造 成接合漏泡。 針對此情況，曾提出於Ni膜上濺鍍TiN膜做為包覆膜 ，且將其加以熱處理以使得NiSi膜之表面氮化。藉此，來 達成防止N i S i之氧化、抑制凹凸的形成之目的。 但是，於Ni上堆積TiN形成之NiSi上的氮化膜由於 厚度缚，所以難以長時間維持防護性，此為問題所在。 是以，乃提出在添加有氮氣之混合氣體（2·5〜1〇%)環境 氣氛中形成石夕化物膜’以將石夕化物膜之粗輪度控制在他m 以下、粒徑控制在20〇nm以上。進一步於Ni上包覆n、w 、TiNx、WNx中一者更佳。 另外也提出，此時，亦可 Ni，接著濺鍍TiN之包覆膜之 方式植入Ni膜，藉此，在Ni 1 5 3 61 6號公報）。 僅以不含氮氣之氬氣來濺鍍 後，將N離子以離子植入的 膜中添加N(參見特開平9一 〆 且衣罝及其製造方g1227279 发明 Description of the invention: [Technical field to which the invention belongs] The present invention relates to a method capable of forming a silicide (NiSi) film thermally and stably, and the target has good plastic processability, and is particularly suitable for manufacturing gate materials (thin films). Nickel alloy sputtering target and manufacturing method thereof. [Previous Technology] Recently, the use of NiSi film by the process of auto-aligned silicide (sal1C1de) in the gate material has been paid more and more attention. Compared with the process of auto-aligning Shi Xihua, the video can form Shi Xi Xi film with less consumption of Shi Xi Xi, which is its feature. In addition, the NiSi and Shi Xihua samples have the characteristic that the fine wire resistance is not easily increased due to the miniaturization of the wiring. For the foregoing reasons, nickel is considered to replace the expensive cobalt in terms of gate materials. —In the case of using NlSl by Renmin, the phase transition is likely to occur and the more secure phase NiSh 'has problems of deterioration of interface roughness and higher resistance. In addition, there is a problem that membrane aggregation is likely to occur or excessive stone formation occurs. Conventionally, in the case of using a film such as Shi Xihua, a metal oxide film such as T i N or Ni film was used and then annealed to prevent reaction with oxygen during the formation of a cut compound film. And the technology of forming an insulating film. On this day, t 'is used in order to prevent oxygen from reacting with Ni to form an uneven insulating film. In the case where the unevenness is small, the distance to the junction between the NiSi film and the source / drain diffusion layer becomes longer ', so that the joint leakage can be suppressed. Other coated 1227279 films include TiC, TiW, TiB, WB2, WC, BN, AIN, Mg3N2, CaN, Ge3N4, TaN, TbNi2, VB2, VC, ZrN, ZrB, etc. (see Japanese Patent Laid-Open No. 7-3 81 〇 Bulletin 4). Also, the conventional technique is questioned. NiSi is very easy to be oxidized in the petrochemical material, and large irregularities are formed in the interface region between the NiSi film and the Si substrate, which may cause joint leakage. In view of this situation, it has been proposed that a TiN film be sputter-coated on the Ni film as a coating film, and heat-treated to make the surface of the NiSi film nitride. Thereby, the purpose of preventing oxidation of N i S i and suppressing the formation of unevenness is achieved. However, since the nitride film on NiSi formed by depositing TiN on Ni has a thickness constraint, it is difficult to maintain the protective property for a long time, which is a problem. Therefore, it is proposed to form a stone oxide film in an ambient atmosphere of a mixed gas (2.5 to 10%) added with nitrogen, so as to control the thickness of the stone oxide film to less than 1 m and the particle size to Above 200nm. Further, Ni is preferably coated with one of n, w, TiNx, and WNx. It is also proposed that, at this time, a Ni film may be implanted by Ni, followed by sputtering a coating film of TiN, and this is disclosed in Ni 1 5 3 6 6). After sputtering with argon gas containing no nitrogen only, add N to the ion-implanted membrane (see Japanese Patent Application Laid-Open No. Hei 9 and 〆, and its manufacturer g).
係記載了第-金屬：CG、Ni、HPd_HTDepartment records the first-metal: CG, Ni, HPd_HT
Hf、V、Nb、Ta或Cr之組合。在實施例中有c〇—η之组/ 链相較於鈦在使得石夕氧化膜還原之能力上較差:^ 積姑之際若於#板或聚㈣表面存在著Μ氧化膜: 1227279 況，會妨礙石夕化物反應。再者耐熱性也較石夕化鈦膜差，石夕 化銘a〇sl2)膜會因為自動對準錢物程序結束後之層間膜 用石夕氧化膜堆積時之熱而凝集導致 守双蛋阻上升（參見特開平 1 1 -204791 號公報（USP5989988))。 又，在習知技術申，揭示 「 , 询不f +導體裝置之製造方法 」’當中^出了為了防止自動對準石夕务必# Λ、 切5了 +矽化物形成之際之過度 生長所造成之短路，艿花；4、力丄+ μ 丑塔乃形成始或鎳之與擇自鈦、錯、鈕、 銷、銳、給以及鎢之金屬所 興，力乂心非日日貝合金層之技術。針 對此種情況，有始合古旦^ η . 里50〜75at%、Ni40Zr60之實施例， 但為了做出非晶曾胺 、、而3有大罝之合金（參見特開平5- 94966號公報）。 士上述身又’所揭示之先前技術中皆是針對成膜程序做 =而非關於賤鑛乾。又，以往之高純度鎳係不計氣體 心刀達接a4N程度之氧高達1〇〇卿之物。 土於此種以在之鎳來製作鎳合金靶的結果，塑性加工 、未此裝作出品質佳的靶。又濺鏟之際會出現許多粒 :...’均一性也不佳，此為問題所在。 【發明内容】 本發明之目& / 卩在於提供一種鎳合金濺鍍靶及其製造方 法，可形成埶卑中从# 1隹^ …女疋性仏之矽化物（NiSi)膜、不易發生膜之 綾集與過度之 白丄 物化、均一性良好、且靶之塑性加工性 、特別適用於閘極材料(薄膜)之製造。 铉夭為了解決上述問題，得到了下述見解：藉由於高純度 錄添加特殊之金屬 蜀兀素，可製造出一種濺鍍靶，其可形成 1227279 熱安定性矽化物（NiSi)膜，於濺鍍之際少有粒子之產生， 且均一性良好，再者富有塑性加工性。 基於上述見解，本發明乃提供： 1. 一種鎳合金濺鍍靶，其特徵在於：鎳中含有鈕 0·5〜1 Oat% 〇 2. —種鎳合金濺鍍靶’其特徵在於：鎳中含有鈕 1〜5at% 〇 上述1或2之鎳合金濺鍍靶，其中，不計氣體成 刀之不可避免之雜質在1 〇〇wtppm以下。 上述1或2之鎳合金濺鍍靶，其中，不計氣體成 分之不可避免之雜質在lOwtppm以下。 5.如上述1或2之鎳合金濺鍍靶，其中，氧在 50wtppm以下、麵 卜 ^ 山、 鼠、虱以及碳分別在1〇wtppm以下。 6 士 述1或2之鎳合金濺鐘革巴，其中，氧在 1 Owtppm 以下。 rj 士 述1或2之鎳合金濺鍍革巴，其中，把面内方向 之初導磁率在50以上。 8·如上流 1 + ^ 〆2之鎳合金錢錄革巴，其中，革巴面内方向 之初磁化曲綠卜& p 、、灵上之僉大導磁率在1〇〇以上。 y. 士口上 izR 1 4、 < i或2之鎳合金濺鍍靶，其中，靶之平均矣 晶粒徑在80“ m以下。 ’、 " ，係用以製造上述 於·以再結晶溫度 m螺合金濺鍍靶 < 衣： 1 9中任一之鎳合金濺鍍靶；其 〜95rC進行最終熱處理。 1227279 【實施方式j 本务明之輕，係將粗Ni(,等級）加以電解 去除金屬雜質成分之後1EB熔解進一步精d在 度錄鍵塊，然後將此鍵塊與高純度起予以真空炫解：：： 出高純度鎳合金錢塊。 於真空熔解之際，使用水冷銅製坩堝之冷坩禍熔解法 為適宜者。將此合金錠塊以鍛造、壓延等製程做成板狀物 ，最後以再結晶溫度（約500°C)〜950°C進行熱處理以製作 輕。此代表性高純度鎳I巴之分析值顯示於表1。 1227279 表1 元素 (wtppin) 元素 .(WtppiD) Li <0.001 \ Ag <0.01 Be <0.001 Cd <0.01 B 0.02 In <0.05 F <0.G1 Sn* 0.2 Na <0.01 Sb <0.01 Mg , 0.57 Te <0.01 A) 0.14 I <0.01 Si 2.7 Cs .<0.01 P <0.01 Ba ‘ <0:005 s 0.02. La 1 <0.005 Cl 難0顧 ^ ： Ce : ："<0: 005 K <0.01 Pr <0.005 Ca <0.01 Nd <0.005- Sc <0.001 Sm <0.005 Ti .0.24 ;Ell· <0. 005 V 0.01 Gd <0.005 Cr . 0.02 Tb · ..<0.005 ,Mn 0,12 .Dy . ./ > <0. 005 Fe …m. :⑽5 , Co 0: 66 -<0.005 Ni Matrix . TlD ^ <0. 005 Cu 0.13 Yb . <0.005 Zn <0.01 Lu <0.005 Gci mm Hi <0:01 Ge <0.05 Ta 10.01； As， <0.01 W 0,02 Se <0.01 * Re； -<0.01 Br <0.05 Os <0.01 Rb <0.005 Ir <0.01 Sr <0.005 PI 0. 07 Y <0.005 ‘An <0.01 It <0.01 Hg <0.01 Nb 0.2 11 <0.01 Mo 0.03 Pb 0.04, Ru <0.01 Bi <0.005 Rh <0.01 Th <0.0001 Pd <0.01 U <0.0001 H <10 C <10 N <10 0 <10A combination of Hf, V, Nb, Ta or Cr. In the example, the group / chain of c0-η is inferior to titanium in its ability to reduce the oxidized oxide film compared to titanium: ^ If there is an oxidized film on the #plate or polyfluoride surface on the occasion of product: 1227279 , Will hinder the reaction of Shi Xihua. In addition, the heat resistance is also worse than that of Shixihua titanium film. Shixi Huaming a0sl2) film will condense due to the heat when the interlayer film is stacked with the Shixi oxide film after the auto-alignment procedure is completed. Resistance rise (see Japanese Patent Application Laid-Open No. 1 1-204791 (USP5989988)). In addition, in the conventional technology application, the "manufacturing method of the f + conductor device" has been revealed, "In order to prevent the automatic alignment of Shi Xi must be # Λ, cut 5 + silicide formation excessive growth place The short circuit caused by it is 艿 flower; 4. Li 丄 + μ The ugly tower is formed by the formation of nickel or nickel, which is selected from the metals of titanium, copper, button, pin, sharp, and tungsten. Layer of technology. In view of this situation, there are examples of Sihe Gudan ^ η. 50 ~ 75at%, Ni40Zr60, but in order to make amorphous alloys, and 3 alloys with large hafnium (see Japanese Patent Application Laid-Open No. 5-94966). ). The previous techniques disclosed in the above-mentioned examples are directed to the film-forming process, not to the low-level mine. In addition, the conventional high-purity nickel is irrespective of the gas, and the heart knife reaches a level of a4N with oxygen as high as 100%. As a result of making nickel alloy targets with nickel in this way, plastic processing has not been done to make good quality targets. When the shovel is splashed again, a lot of grains will appear: ... ’Poor uniformity is the problem. [Summary of the Invention] The purpose of the present invention is to provide a nickel alloy sputtering target and a manufacturing method thereof, which can form a silicide (NiSi) film from # 1 隹 ^… female sex-prone, which is not easy to occur. The integration of the film and the excessive physical properties of the pebbles, the uniformity is good, and the plastic processability of the target is particularly suitable for the manufacture of gate materials (thin films).铉 夭 In order to solve the above problems, the following insights were obtained: By adding a special metal succinate to the high-purity record, a sputtering target can be manufactured, which can form a 1227279 thermally stable silicide (NiSi) film, and During the plating, few particles are generated, and the uniformity is good. Moreover, it is rich in plastic workability. Based on the above findings, the present invention provides: 1. A nickel alloy sputtering target, characterized in that nickel contains a button of 0.5 to 1 Oat% 〇2. A nickel alloy sputtering target 'characterized in that: in nickel The nickel alloy sputtering target containing 1 to 5 at% of the button 1 or 2 above, wherein the inevitable impurities excluding gas to form a knife are 100 wtppm or less. The nickel alloy sputtering target of 1 or 2 above, wherein the inevitable impurities excluding gas components are 10 wtppm or less. 5. The nickel alloy sputtering target according to 1 or 2 above, wherein the oxygen is below 50 wtppm, the surface area, rat, lice and carbon are below 10 wtppm, respectively. 6 Nickel alloy splash bell leather of 1 or 2, wherein the oxygen is below 1 Owtppm. rj The nickel alloy sputtered leather of 1 or 2 mentioned above, wherein the initial magnetic permeability in the in-plane direction is 50 or more. 8. The nickel alloy Qianlu Geba of the upper class 1 + ^ 〆2, in which the initial magnetization curve in the direction of the Geba in the plane is greater than 100. y. Nickel alloy sputtering targets izR 1 4, < i or 2 on Shikou, where the average crystal grain size of the target is below 80 "m. ', " are used to make the above-mentioned for recrystallization Temperature Spiral Alloy Sputtering Target < Clothing: Nickel alloy sputtering target of any one of 9; its final heat treatment is ~ 95rC. 1227279 [Embodiment j The light of the matter is that the crude Ni (, grade) is electrolyzed After removing the metal impurities, 1EB is melted to further record the key block, and then the key block and the high purity are vacuum-darkened. :: High-purity nickel alloy coin block is used. For vacuum melting, a water-cooled copper crucible is used. The cold craze melting method is suitable. This alloy ingot is made into a plate by processes such as forging and rolling, and finally heat-treated at a recrystallization temperature (about 500 ° C) to 950 ° C to make light. This representative The analytical value of the high-purity nickel Ibar is shown in Table 1. 1227279 Table 1 Element (wtppin) Element. (WtppiD) Li < 0.001 \ Ag < 0.01 Be < 0.001 Cd < 0.01 B 0.02 In < 0.05 F < 0.G1 Sn * 0.2 Na < 0.01 Sb < 0.01 Mg, 0.57 Te < 0.01 A) 0.14 I < 0.01 Si 2.7 Cs. ≪ 0.01 P < 0.01 Ba '< 0: 005 s 0.02. La 1 < 0.005 Cl Difficulty and care ^: Ce: ： " < 0: 005 K < 0.01 Pr < 0.005 Ca < 0.01 Nd < 0.005- Sc < 0.001 Sm < 0.005 Ti .0.24; Ell · < 0. 005 V 0.01 Gd < 0.005 Cr. 0.02 Tb · .. & 0.005, Mn 0,12 .Dy. ./ > < 0. 005 Fe… m.: ⑽5, Co 0: 66-< 0.005 Ni Matrix. TlD ^ < 0. 005 Cu 0.13 Yb. ≪ 0.005 Zn < 0.01 Lu < 0.005 Gci mm Hi < 0: 01 Ge < 0.05 Ta 10.01; As, < 0.01 W 0,02 Se < 0.01 * Re;-< 0.01 Br < 0.05 Os < 0.01 Rb < 0.005 Ir < 0.01 Sr < 0.005 PI 0. 07 Y < 0.005 'An < 0.01 It < 0.01 Hg < 0.01 Nb 0.2 11 < 0.01 Mo 0.03 Pb 0.04, Ru < 0.01 Bi < 0.005 Rh < 0.01 Th < 0.0001 Pd < 0.01 U < 0.0001 H < 10 C < 10 N < 10 0 < 10
ιβιιβι
註：進行除了 H，C，Ν，0與Ta以外之GDMS分析 註：Ta為wt% 註：〈係表示測定極限以下 10 1227279 1 旦之添加量為0.5〜l〇at% 過少，則鎳合金層之熱安定性 膜電阻會變得過大而不適當， k成塑性加工的困難，賤鍍時 問題。 、更佳為1〜5at%。若添加量 無法提昇。若添加量過多， 且金屬間化合物的量會增多 之粒子也會增多，這些都是 使用本發明之添加有組之鎖合金進行減錢，進— ㈣鍍成膜於氮氣環境氣氛中加熱之後，卩m繞射㈣ 疋結晶結構之變化溫度，結果發現因為㈣添加而增/了 50〜90〇C之相變化溫度，確認了顯著的熱安定性。n 為了減少賤鍍之際之粒子的產生，使得均—性 成分以外之不可避免的雜質控制在丨。。对卿以 為所希望者。更佳為將氣體成分以外之 制在i〇wt卿以下。 t光的雜貝控 ，所 將氮 、進 重要 又，由於氣體成分亦為粒子產生增加的主要原因 以，氧控制在5Gwt卿以下（更佳為1Gwtppm以下）、 氫以及奴分別控制在1 0wtPPm以下乃為所希望者。 將靶之初導磁率調整至50以上（更佳為1〇〇左右） 而將最大導磁率調整至⑽以上對於_特性是相當 以再結晶 實質的再結晶 到充分之再結 磁率提昇。 溫度(請。C)〜95(TC進行最終熱處理成為 組織。若熱處理溫度未㈤5⑽。C，則無法得 晶組織。又，亦無法使得導磁率以及最大導 於本發明之革巴中 若存在著若干未再結晶之物雖不致 1227279 影響特性，惟大I的左Note: GDMS analysis other than H, C, N, 0 and Ta Note: Ta is wt% Note: <means the measurement limit is below 10 1227279 1 Once the amount of addition is 0.5 ~ 10at% is too small, the nickel alloy The layer's thermally stable film resistance will become too large and inappropriate, making it difficult for plastic processing, and problems during low-level plating. And more preferably 1 to 5 at%. If the amount cannot be increased. If the added amount is too large, and the amount of intermetallic compounds will increase, the number of particles will also increase. These are reduced by using the lock alloy added with the group of the present invention. After the arsenic coating is heated in a nitrogen atmosphere,卩 m diffraction㈣ The change temperature of 疋 crystal structure. As a result, it was found that the phase change temperature of 50 ~ 90 ° C was increased / decreased by the addition of ㈣, and significant thermal stability was confirmed. n In order to reduce the generation of particles during low plating, unavoidable impurities other than homogeneous components are controlled. . To Qing thought what he wanted. It is more preferable that the content other than the gas component is not more than 100 wt%. The control of heterogeneity of light is important for nitrogen and nitrogen. As the gas component is also the main reason for the increase in particle generation, oxygen is controlled below 5Gwt (more preferably 1Gwtppm), and hydrogen and slave are controlled at 10wtPPm. The following is what I want. Adjusting the initial magnetic permeability of the target to more than 50 (more preferably about 100) and adjusting the maximum magnetic permeability to more than ⑽ are very good for the characteristics. The recrystallization is substantially recrystallized to a sufficient re-junction to increase the magnetic permeability. Temperature (please. C) ~ 95 (TC for final heat treatment to become a structure. If the heat treatment temperature is not higher than 5 ° C., The crystalline structure cannot be obtained. Also, the magnetic permeability and the maximum conductivity in the leather of the present invention cannot be obtained. Although some unrecrystallized objects do not affect the characteristics of 1227279,
9存在非所樂於見到者。靶之平均結E 粒徑以8 0 # m以下為佳。 曰1 超過950°C之：i*炊# + 取〜熱處理，由於會導致平均結晶粒据 粗a化故非所希望者。_旦平均結晶粒徑粗大化，則社曰 粒徑=差異會增大，均-性會降I '〇ΘΕ f施例斑fchUt 、下針對本發明之實施例做說明。又，本實施例僅為 ^月之 <列，本發明不因為這些實施例而受到限制。亦即 ，在本發明之技術思想的範圍内，包含了實施例以外所有 的態樣與變形。 (貫施例卜卜實施例3-2) /將粗NK〜4N等級）加以電解精製來去除金屬雜質成分 之後，以EB溶解進一步精製成為高純度錄旋塊，然後將 、疋免；、同、，、屯度！s予以真空溶解而製作出高純度鎳合金旋 塊。於真空炫解之際，係使用水冷銅製掛禍之冷掛禍溶解 法09 There are unwilling to see. The average junction E particle size of the target is preferably 80 # m or less. 1 above 950 ° C: i * ： # + Taken ~ heat treatment, because it will cause the average crystal grains to coarsen, which is not desirable. Once the average crystal grain size is coarsened, the particle size = difference will increase, and the homogeneity will decrease I′〇ΘΕ f Example spot fchUt The following describes the embodiment of the present invention. In addition, this embodiment is only a < column of the following month, and the present invention is not limited by these embodiments. That is, within the scope of the technical idea of the present invention, all aspects and modifications other than the embodiment are included. (Exemplary Example 3-2) / The crude NK to 4N grade) is electrolytically refined to remove metal impurities, and then dissolved in EB to further refine it into a high-purity recording block. ,,, Tundu! s was dissolved in a vacuum to produce a high-purity nickel alloy spin block. In the case of vacuum dazzling, it is a cold-solving method using water-cooled copper
將此合金錠塊以鍛造、壓延等製程做成板狀物，最 以500 C〜950°C進行熱處理以製作靶。 靶製“·、件之Ta s、純度、氧含量、熱處理溫度之 件以及靶與成膜特性之初導磁率、最大導磁率、平均結 粒、結晶粒徑之差異、粒子量、均一性係示於表2。 如表2所示般，實施例丨系列之Ta量為i 68at%， 施例2系列之Ta量為3」8at%，實施例3系列之Ta量 7. 50at% 〇 12 1227279 b rn m ] 1 oo - 卜 iT) m 卜 oo 寸 Z： v〇 m 二 OO m <N m ε ro 〇 if e p/in2) m <N 00 r〇 S oo 卜 C\ <N v〇 a\ P; rn wn 差異 Nw^ 1 1 VO a\ CN OO VO 1 1 1 00 !n 1 1 a\ 1 ΓΟ m < < mg < < mg m m 蝇 m fig < m m e 5Γ tt w： m tt fig a tt 张 伥 m K oo λ 张 寸 伥 12.7 CN tt r〇 ro H- 壤 fr rn p « 擗 OO VO S » » •K s s § ζ* 3 〇\ 00 oo VD m VO ^Ti v〇 a On v〇 v〇 rs m <N m 5 m 褂 瘦 If s s 5 oo oo 2 s s CN 5 二 \D rs !〇 |〇 m oo 樂 m 七 m 癒 P 500 1_ 600 650 650 650 300 450 1000 750 800 850 930 300 O 2 1050 1150 900 950 600 1250 〇- 祕 &· 1 ro <10 g s <10 <10 <10 <10 <10 <10 <10 <10 <10 <10 <10 <10 <10 <10 <10 純度 彥 2： v〇 1 ^T) 3N5 2: 寸 5 i〇 3N5 寸 ^T) yn 1_ f 00 \q § § OO vq 00 VO s OO 00 v〇 等 吞 3.48 § 吞 Η viS f—H 二 二 rn rn ΓΟ rn rn ro ΓΟ 1 <N rn 1 iN rn A (N (N rn <N <N tN (N r〇 <N 寸 <N rn <N m rA <N r〇 i i m i i i i m S 辑 辑 辑 鎰 鎰 鎰 辑 辑 辑 鎰 傲 撰 舾 U k a ΛΛ K 卹 1¾ IK i5 ±Λ AJ AJ u U jj 1227279This alloy ingot is made into a plate by processes such as forging and rolling, and is heat-treated at 500 C to 950 ° C to produce a target. Target system "·, Ta s of pieces, purity, oxygen content, heat treatment temperature, and initial permeability, maximum permeability, average agglomeration, crystal size difference, particle size, uniformity Shown in Table 2. As shown in Table 2, the amount of Ta in the series of Example 丨 is i 68at%, the amount of Ta in the series of Example 2 is 3 ″ 8at%, and the amount of Ta in the series of Example 3 is 7.50at% 〇12 1227279 b rn m] 1 oo-bu iT) m oo inch Z: v〇m OO m < N m ε ro 〇if ep / in2) m < N 00 r〇S oo C \ < N v〇a \ P; rn wn Difference Nw ^ 1 1 VO a \ CN OO VO 1 1 1 00! n 1 1 a \ 1 ΓΟ m < < mg < < mg mm fly m fig < mme 5Γ tt w: m tt fig a tt Zhangye m K oo λ Zhang inch 伥 12.7 CN tt r〇ro H- soil fr rn p «擗 OO VO S» »• K ss § ζ * 3 〇 \ 00 oo VD m VO ^ Ti v〇 a On v〇v〇rs m < N m 5 m Slim If ss 5 oo oo 2 ss CN 5 II \ D rs! 〇 | 〇m oo 乐 m 七 m 越 P 500 1_ 600 650 650 650 300 450 1000 750 800 850 930 300 O 2 1050 1150 900 950 600 1250 〇- secret & 1 ro < 10 gs < 10 < 10 < 10 < 10 < 10 < 10 < 10 < 10 < 10 < 10 < 10 < 10 < 10 < 10 < 10 purity 彦 2: v〇1 ^ T) 3N5 2: inch 5 i〇3N5 inch ^ T) yn 1_ f 00 \ q § § OO vq 00 VO s OO 00 v. Etc. 3.48 § Swallow viS f—H 22 rn rn rn Γ rn rn ro ΓΟ 1 < N rn 1 iN rn A (N (N rn < N < N tN ( N r〇 < N Inch < N rn < N m rA < N r〇iimiiiim S Compilation Compilation Compilation Compilation U Ka ΛΛ K-shirt 1¾ IK i5 ± Λ AJ AJ u U jj 1227279
Ta量、純度、氧含量、熱處理溫度 X <條件在本發明範 圍内之實施例1-1〜1-3、實施例2-1〜2-4、每# η。 ^ 焉施例3-1〜3-2 之初導磁率在50以上、最大導磁率在1〇〇以 » 丁、培晶 粗徑在80 // m以下、結晶粒徑之差異小、粒子量（〇 3 #爪 以上/in2)也少、均一性（％，3 σ )亦為小數值。 · 接著，使用本實施例之添加有鈕之鎳合金進行濺鍍， 進一步將此濺鍍成膜於氮氣環境氣氛中加熱之後，以^肋 繞射法測定結晶結構之變化溫度，結果發現因為鈕的添加 :增高了 50〜9(TC之相變化溫度。因而確認了顯著的熱安 定性。 户又，實施例1-1、實施例1-2、實施例因熱處理溫 X略低，所以存在著未再結晶組織，但其存在量少，故並 未影響到特性。 (比較例1-1〜3-2) 2 製程係與上述實施例相同，Ta添加量也相同、但如表 斤示般改變純度、氧含量、熱處理温度之條件來製造靶 —對所得之靶以及成膜特性之初導磁率、最大導磁率、平 二、、日日粒瓜、結晶粒控之差異、粒子量、均一性進行測定 與觀察。 ' 又’與實施例同樣，比較例1系列之Ta量為1. 68at% 息比較例2系列之Ta量為3. 48at%、比較例3系列之Ta 襄為 7. 5〇at%。 其結果，比較例1-1以及卜2之氧量過多，純度低， 戶斤q太 產生許多粒子之問題。比較例1 -3與1 -4由於熱處 14 1227279 理溫度過低，所以未能提昇初導磁率與最 能再結晶或大量存在著未再結晶組織。 未 現二二之二，，-- 比較例w與比較例2_2由於純度低 低’所以未能提昇初導磁率與最大導磁率，且未心；： 或存在著大量未再結晶組織。粒子產生也多月匕再，口日日 :較例2-3以及2-4之最終熱處理溫度過高，平均結 曰曰垃徑出現粗大化，差異變大均一性惡化。 ° 比較例3-1之熱處理溫度低， 大導磁率。且存以… 去棱昇初導磁率與最 ^ 里未再結晶組織，粒子產生也多。 比較例3-2之最終埶虛理㈤疮 一 現斗m * ‘，、、處理咖度過南，平均結晶粒徑出 現粗大化，差異變大，均一性惡化。 金有之錄中含有特…之錄合 /、有下述顯者效果：可形成熱安定性佳之矽化 (N1S1)膜、不易發生膜之凝集與過度之石夕化物 之際粒子產生少，均一性也良好，且富有㈣ 特別適用於閘極材料（薄膜）之製造。 15The amount of Ta, purity, oxygen content, and heat treatment temperature X < Examples 1-1 to 1-3, Examples 2-1 to 2-4, each # η are within the scope of the present invention. ^ Example 3-1 ~ 3-2. The initial magnetic permeability is above 50, the maximum magnetic permeability is 100%, the diameter of the crystal is less than 80 // m, the difference in crystal size is small, and the amount of particles is small. (〇3 #owl above / in2) is also small, and the uniformity (%, 3 σ) is also a small value. · Next, the nickel alloy with the button added in this embodiment was used for sputtering, and the sputtering film was further heated in a nitrogen atmosphere, and then the change temperature of the crystal structure was measured by the ^ rib diffraction method. Addition: Increased the phase change temperature of 50 ~ 9 ° C. Therefore, significant thermal stability was confirmed. In addition, Example 1-1, Example 1-2, and Example exist because the heat treatment temperature X is slightly lower, so The structure is not recrystallized, but its existence is small, so it does not affect the characteristics. (Comparative Examples 1-1 to 3-2) 2 The process is the same as in the above example, and the addition amount of Ta is also the same, but as shown in the table Generally change the conditions of purity, oxygen content, and heat treatment temperature to make targets—the initial magnetic permeability, maximum magnetic permeability, flat second, daily melon, crystal grain control difference, particle amount, The homogeneity is measured and observed. Also, as in the examples, the Ta amount of the Comparative Example 1 series is 1. 68at%. The Ta amount of the Comparative Example 2 series is 3. 48at%, and the Ta of the Comparative Example 3 series is 7. 50〇at%. As a result, the amount of oxygen in Comparative Examples 1-1 and Bu 2 was too high. The purity is low, and there is a problem that too many particles are generated in Comparative Example 1-3 and 1-4. Due to the low temperature of the hot place 14 1227279, the initial magnetic permeability cannot be improved and the most recrystallizable or a large number of unrecovered The crystalline structure is not found. Two or two,-Comparative Example w and Comparative Example 2_2 failed to improve the initial magnetic permeability and the maximum magnetic permeability due to the low purity, and were not heart-shaped; or there was a large amount of non-recrystallized structure The particles are generated for many months, and the daily heat treatment temperature is too high in Comparative Examples 2-3 and 2-4. The average diameter is coarsened, and the difference becomes large. The uniformity deteriorates. Comparative Example 3 The heat treatment temperature of -1 is low, and the magnetic permeability is high. And ... the initial magnetic permeability and the most unrecrystallized structure are removed, and the number of particles is also large. The final irrational scabies of Comparative Example 3-2 is now a battle. m * ',,, and processed coffee through the south, the average crystal grain size appears coarse, the difference becomes larger, and the uniformity deteriorates. Jin Youluo contains the special ... /, has the following obvious effects: can form Silicified (N1S1) film with good thermal stability, less likely to cause film aggregation and excessive stone In the case of chemical compounds, there are few particles, good uniformity, and richness. It is especially suitable for the manufacture of gate materials (thin films). 15