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TW201103999A - Method for manufacturing nickel alloy target - Google Patents

Method for manufacturing nickel alloy target Download PDF

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Publication number
TW201103999A
TW201103999A TW98124764A TW98124764A TW201103999A TW 201103999 A TW201103999 A TW 201103999A TW 98124764 A TW98124764 A TW 98124764A TW 98124764 A TW98124764 A TW 98124764A TW 201103999 A TW201103999 A TW 201103999A
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Taiwan
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manufacturing
nickel alloy
powder
nickel
alloying element
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TW98124764A
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Chinese (zh)
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TWI387661B (en
Inventor
yin-ting Hong
Rong-Zhi Chen
zhi-long Li
Hong-Sheng Huang
Qing-Zong Chen
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China Steel Corp
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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The method for manufacturing a nickel alloy target according to this invention has the steps of vacuum melting a nickel metal and at least one alloy element into an alloy solution, then atomizing the solution to form a nickel alloy powder, then sieving and selecting the nickel alloy powder that is smaller than a predetermined particle size, and finally molding the nickel alloy powder into a nickel alloy target. The present invention does not need to use expensive Ni and W powders as raw materials and does not need to use expensive plasma sintering equipment for sintering, and furthermore the nickel alloy targets can be rapidly manufactured in large scale without experiencing a cold-rolling process and re-crystallization annealing process, thus simplifying the manufacturing method and reducing the manufacturing time. Additionally, the nickel alloy target manufactured by the method according to the present invention has no composition deviation and has fine crystal grains, uniform crystal grain distribution and complete alloying, thus having higher sputtering quality.

Description

201103999 六、發明說明: 【發明所屬之技術領域】 本發明係有關於一種靶材之製造方法,詳言之,係關於 一種鎳合金靶材之製造方法。 【先前技術】 參考中國大陸專利第200510104828.2號及第200610076274.4 號’其揭示一種粉末冶金的製造技術,其係先以球磨方式 將高純度之鎳(Ni)粉及鎢(w)粉混合後,裝入石墨模具 中’利用放電等離子燒結法於8〇〇〜12〇〇°C、壓力控制在 30〜80 MPa、持溫1〇分鐘,將粉末燒結緻密製得州_〜合 金。該等專利雖能製作出緻密之Ni-W合金,但其採用傳統 的粉末混合方式來混合Ni粉與W粉,因Ni密度為8.9 g/cm3 ’ W密度為19.3 g/cm3,二者密度相差一倍以上,在 利用球磨混粉過程中’密度較大之W粉易與密度較小Ni粉 分離,造成粉末混合不均,進一步影響燒結後合金之成分 均勻性。 另外,上述二專利之方法係採用傳統粉末冶金製程,其 必需使用價格卬貴之尚純度(純度99.99%)且粒度細小(粒度 約在3〜6 μιη)之Ni粉及W粉,因此所製備之Ni_w合金成本 較尚。再者’上述二專利中僅係以球磨方式將Ni粉及臂粉 進行混粉,Ni粉及W粉在混合時並未合金化,經過燒結 後’ Ni粉及W粉雖因燒結反應而緻密,但並未完全合金 化,仍可明顯觀察到Ni粉及W粉單獨存在。 此外,在一般習知粉末製程中,所需之粉末混合時間較 138926.doc 201103999 約費時8〜24小時不等,且粉末在混合過裎中,容易因 高炼點粉末錢較-般金屬粉末大,造成粉㈣合不均, =而影響燒結㈣材之成分均勾性。並且,在傳統炫煉製 知中’炫湯邊鑄、冷卻後,尚需再進行熱軋延以細化組 織’同樣需費時數十小時1中,在傳統鑄造製程之凝固 過程中’谷易有縮孔、成分偏析及組織粗大等缺點,故需 再以費時之熱軋步驟消除鑄錠之偏析,並細化組織。 ,因此、’有必要提供-創新且富有進步性之锦合金乾材之 製造方法,以解決上述問題。 【發明内容】 本發明提供-種鎳合金輕材之製造方法,包括以下步 驟:⑷提供鎳金屬及至少-第-合金元素;(b)進行一真 空溶煉步驟,以形成—合金溶液;⑷霧化該合金溶液,以 形成錄合金粉體;⑷進m步驟,以小於一設定BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a target, and more particularly to a method for producing a nickel alloy target. [Prior Art] Referring to Chinese Patent No. 200510104828.2 and No. 200610076274.4, which discloses a powder metallurgy manufacturing technique in which high-purity nickel (Ni) powder and tungsten (w) powder are first mixed by ball milling, and then loaded. In the graphite mold, 'discharge plasma sintering method is used at 8〇〇~12〇〇°C, the pressure is controlled at 30~80 MPa, and the temperature is maintained for 1 minute, and the powder is sintered and compacted to obtain the state_~ alloy. Although these patents can produce dense Ni-W alloys, they use traditional powder mixing methods to mix Ni powder and W powder, because the density of Ni is 8.9 g/cm3 'W density is 19.3 g/cm3, the density of the two More than double the difference, in the process of using ball milling powder, the 'density of W powder is easy to be separated from the density of Ni powder, resulting in uneven powder mixing, further affecting the composition uniformity of the alloy after sintering. In addition, the method of the above two patents adopts a conventional powder metallurgy process, and it is necessary to use Ni powder and W powder which are expensive (purity of 99.99%) and fine in size (particle size of about 3 to 6 μm), and thus prepared. The cost of Ni_w alloy is relatively high. Furthermore, in the above two patents, only the Ni powder and the arm powder are mixed by ball milling, and the Ni powder and the W powder are not alloyed during mixing. After sintering, the Ni powder and the W powder are dense due to the sintering reaction. However, it is not completely alloyed, and it is still apparent that Ni powder and W powder are separately present. In addition, in the conventional powder process, the required powder mixing time is about 8 to 24 hours longer than 138926.doc 201103999, and the powder is mixed in the crucible, which is easy to be compared with the high metal powder. Large, causing the powder (four) to be uneven, and affecting the composition of the sintered (four) material. Moreover, in the traditional smelting and knowing process, after the simmering soup is cast and cooled, it is still necessary to carry out hot rolling to refine the structure. It also takes several tens of hours. In the solidification process of the traditional casting process, There are disadvantages such as shrinkage cavities, composition segregation and coarse structure, so it is necessary to eliminate the segregation of the ingot and refine the structure by a time-consuming hot rolling step. Therefore, it is necessary to provide - an innovative and progressive method of manufacturing brocade alloy dry materials to solve the above problems. SUMMARY OF THE INVENTION The present invention provides a method for producing a nickel alloy light material, comprising the steps of: (4) providing a nickel metal and at least a - alloying element; (b) performing a vacuum melting step to form an alloy solution; (4) Atomizing the alloy solution to form a recorded alloy powder; (4) stepping into the m step to less than one setting

粒度之鎳合金粉體’·及⑷成型及緻密化該鎳合金粉體,以 形成鎳合金乾材β 本發明錦合金乾材之製造方法不需使用價格較為昂貴之 Ni粉體及W粉體為原料、不需使用相當昂貴的電浆燒結 備進打N1、w粉體的燒結’並且不需經冷乾製程及在氣氛 保護下進行再結晶退火處理,即可快逮、大量製備製得錄 合金靶材,故製造方法簡單且可減少製造時間。再者,本 發明之製造方法所製得之鎳合錄材無成分偏析、具細緻 晶粗、晶粒分佈均勾且完全合金化,故具有較高之雜品 質0 138926M〇c -4- [S] 201103999 【實施方式】Particle size nickel alloy powder '· and (4) forming and densifying the nickel alloy powder to form a nickel alloy dry material β The method for producing the nylon alloy dry material of the present invention does not require the use of relatively expensive Ni powder and W powder For raw materials, without the use of relatively expensive plasma sintering, the sintering of N1 and w powders can be carried out and can be quickly prepared and prepared in large quantities without the need of a cold-drying process and recrystallization annealing under the protection of the atmosphere. The alloy target is recorded, so the manufacturing method is simple and the manufacturing time can be reduced. Furthermore, the nickel composite recording material produced by the manufacturing method of the invention has no component segregation, fine grain coarseness, fine grain distribution and complete alloying, so it has a high impurity quality 0 138926M〇c -4- [ S] 201103999 [Embodiment]

圖1顯示本發明鎳合金靶材之製造方法流程圖。首先, 參考步驟S11 ’提供錄金屬及至少一第一合金元素,該第 一合金元素係選自鉬(M〇)、鎢(W)、钽(Ta)、給(Hf)、釕 (Ru)、銖(Re)、锆(Zr)或鈮(Nb)。其中,該鎳金屬及該第 一合金元素可為塊狀或條狀,該第一合金元素亦可為片 狀' 粉體狀或屑狀。較佳地,該鎳金屬及該第一合金元素 之純度係大於99.9%,該第一合金元素之重量百分比係為 5%至20%。在本實施例中,該第一合金元素係為鎢合金元 素。 在其他應用中,除該鎳金屬及該第一合金元素外,亦可 另包括一第二合金元素。該第二合金元素係選自鐵(Fe)、 銅(Cu)或鋅(Zn),其中該第二合金元素之熔點低於該第一 合金元素之熔點。較佳地,該鎳金屬之重量百分比係大於 50。/❶’該第-合金元素之重量百分比係為㈣至纖,其餘 之重重百分比係為該第二合金元素含量。 、 另外,在步驟S11之前較佳係另包括以下步驟:利用郵 性溶液移除(例如:利用超音波震動方式)該鎳金屬及該驾 一合金元素表面之氧化物及污染物;移除(例如:利用南 音波震動方式)該錄金屬及該第一合金元素表面之酸性遂 液’及乾無該錄金屬及該第一合令冬 , 口金兀素。其令,該酸性淫 液之體積濃度係為95%以上,且係w 土缺2, 係以去離子水移除該鎳4 屬及該第一合金元素表面之酸性 吸注办液。較佳地,該酸性潭 液係選自鹽酸或硝酸。 138926.doc 201103999 參考步驟S12,進行一真空熔煉步驟,以使該鎳金屬及 該第一合金元素熔融形成一合金溶液。在本實施例中,其 係於真空感應熔煉爐或真空電弧熔煉爐中進行該真空熔煉 步驟,並利用一感應線圈所提供之磁場攪拌熔融之合金溶 液,使熔融合金溶液之成分均勻。較佳地,該真空熔煉之 度係為150(TC至1750。(:,該真空熔煉之之真空度係為 10 3托(torr)以上。 φ 參考步驟S13,霧化該合金溶液,以形成鎳合金粉體。 在本實施例中,其係利用高壓惰性氣體(例如:氬氣(Ar)或 氮氣(Ν2))以噴擊方式霧化該合金溶液。較佳地,該高壓惰 性氣體之壓力為1至5肘1>3,流速為5〇i1〇〇m/s。 其中,本發明之方法在步驟su之後另包括一冷卻步 驟以冷卻霧化後之該鎳合金粉體。舉例而言,本發明可 利用氬氣或氮氣喷擊方式或自然冷卻方式,冷卻霧化後之 該錄合金粉體。 # 參考步驟S14’進行一篩分步驟’以選取一設定粒度之 鎳°金粉體。其中’該設定粒度較佳係小於200微米 ⑽)。該筛分步驟可控制鎳合金粉體具有較小及較均句之 吏/寻錄5金粉體成型為錄合金耗材後,具有更細緻 之晶粒及更均句之晶粒分佈。 參考步驟S15 ’成型及緻密化該錄合金粉體,以形成錄 合金乾材,苴Φ ,^ /、Τ ’本發明鎳合金靶材可應用於磁記錄產 業光電產業或半導體產業之薄膜濺鍍製程。在步驟S15 中其係以熱壓製程或熱均壓製程進行該成型及緻密化步 138926.doc -6 · 201103999 驟。較佳地,成型及緻密化之溫度較佳係為赋至 1200 C,成型及緻密化之時間較佳係為〇5至3小時。 根據實際試驗結果,在本發明之製造方法中,自該鎳金 屬及該第-合金it素置人真空爐中至以惰性氣體喷擊該合 金溶液獲得均勻之鎳合金粉體,其只約需2〜 所製得鎳合金粉體之成分與乾材成分之設定含量:誤差在 〇.5原子百分比(at.%)之内。接著,僅需再經卜3小時之熱BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a flow chart showing a method of manufacturing a nickel alloy target of the present invention. First, referring to step S11', a metal is recorded and at least a first alloying element selected from the group consisting of molybdenum (M〇), tungsten (W), tantalum (Ta), (Hf), and ruthenium (Ru). , 铢 (Re), zirconium (Zr) or bismuth (Nb). Wherein, the nickel metal and the first alloying element may be in the form of a block or a strip, and the first alloying element may also be in the form of a sheet of powder or crumb. Preferably, the nickel metal and the first alloying element have a purity of more than 99.9%, and the first alloying element has a weight percentage of 5% to 20%. In this embodiment, the first alloying element is a tungsten alloy element. In other applications, in addition to the nickel metal and the first alloying element, a second alloying element may be included. The second alloying element is selected from the group consisting of iron (Fe), copper (Cu) or zinc (Zn), wherein the melting point of the second alloying element is lower than the melting point of the first alloying element. Preferably, the weight percentage of the nickel metal is greater than 50. The weight percentage of the first alloying element is (iv) to the fiber, and the remaining weight percentage is the second alloying element content. In addition, before step S11, the method further comprises the steps of: removing (for example, using ultrasonic vibration) the oxides and pollutants on the surface of the nickel metal and the alloy element; For example, using the Southern Sonic vibration method, the recorded metal and the acidic sputum on the surface of the first alloying element and the dry metal and the first combined order winter, the oral scorpion. Therefore, the volume concentration of the acidic morbidity liquid is 95% or more, and the soil is deficient in 2, and the nickel genus and the acidic absorbing liquid on the surface of the first alloying element are removed by deionized water. Preferably, the acid pool is selected from the group consisting of hydrochloric acid or nitric acid. 138926.doc 201103999 Referring to step S12, a vacuum melting step is performed to melt the nickel metal and the first alloying element to form an alloy solution. In the present embodiment, the vacuum melting step is carried out in a vacuum induction melting furnace or a vacuum arc melting furnace, and the molten alloy solution is stirred by a magnetic field provided by an induction coil to make the composition of the molten alloy solution uniform. Preferably, the degree of vacuum melting is 150 (TC to 1750. (:, the vacuum degree of the vacuum melting is 10 3 torr or more. φ. Referring to step S13, the alloy solution is atomized to form Nickel alloy powder. In the present embodiment, the alloy solution is atomized by a high pressure inert gas (for example, argon (Ar) or nitrogen (?2)). Preferably, the high pressure inert gas The pressure is 1 to 5 cubits 1 > 3, and the flow rate is 5 〇 i1 〇〇 m / s. wherein the method of the present invention further comprises a cooling step after the step su to cool the atomized nickel alloy powder. In the present invention, the atomized alloy powder can be cooled by argon gas or nitrogen gas spraying or natural cooling. # Refer to step S14' for a screening step to select a nickel particle size of a set size. Wherein 'the set particle size is preferably less than 200 micrometers (10)). The screening step can control the nickel alloy powder to have a smaller and more uniform sentence / search 5 gold powder formed into a recorded alloy consumable, Finer grain size and more uniform grain distribution. Refer to step S15 '成成Type and densification of the alloy powder to form a dry alloy of the alloy, 苴Φ, ^ /, Τ 'The nickel alloy target of the invention can be applied to the film sputtering process of the photoelectric industry or the semiconductor industry in the magnetic recording industry. In S15, the forming and densification step 138926.doc -6 · 201103999 is carried out by a hot pressing process or a hot pressing process. Preferably, the molding and densification temperature is preferably 1200 C, molding and The densification time is preferably 〇5 to 3 hours. According to the actual test results, in the manufacturing method of the present invention, the nickel metal and the first alloy alloy are placed in a vacuum furnace to spray with an inert gas. The alloy solution obtains a uniform nickel alloy powder, which requires only about 2% of the composition of the obtained nickel alloy powder and the dry material composition: the error is within 原子.5 atomic percent (at.%). Just need another 3 hours of heat

壓或熱均壓即可獲得敏密之鎳合絲材。因此,本發明: 製造方法不僅能快速、大量製備含高熔點元素之鎳合金靶 材,且鎳合金靶材之成分及組織,皆優於以傳統粉末冶金 及熔煉製程製備之合金靶材。 唯並不意謂本發明 兹以下列實例予以詳細說明本發明 僅侷限於此等實例所揭示之内容。 實例1 : 本實例係以Ni-8w(at.%)靶材之原料粉末的製作為 例’其中Ni-8W(at.〇/0)表示犯與|之原子百分比為92: 8。 首先,按照Ni-8W(at.%)合金比例準備鎳塊及鶴#,接著 進行鎳塊及鎢片之表面處理步驟,將鎳塊及鎢片置於體積 濃度95%以上的鹽酸溶液中,以超音波震動方式去除表面 氧化物及油污,再將鎳塊及鎢片置於去離子水中,以超音 波震動方式去除殘留在表面的鹽酸溶液後,再予以烘乾。 接著,將酸洗過後之錄塊及鶴片放入真空感應炫煉爐 之掛鋼中並抽成真空,待真空度達到HTW以上後開始升 溫至1500t ’當堆銷中之鎳塊及鶴片完全炫化後,持溫$ 138926.doc 201103999 分鐘,確m溶點之㈣能充分熔解,並在—感應線圈所 提供之磁場攪拌下使熔融金屬湯液成分均勻。 接著,將熔融Ni-8W金屬湯液自真空感應熔煉爐之坩 禍中倒出,並利用流量控制在3 MPa、流速控制在5〇 _ 之Ar軋’喷擊熔融州_8霄金屬湯液使其霧化成鎳合金粉 體。A dense nickel wire can be obtained by pressure or hot pressure equalization. Therefore, the present invention: The manufacturing method not only enables rapid and large-scale preparation of a nickel alloy target containing a high melting point element, but also has a composition and structure of a nickel alloy target superior to those of an alloy target prepared by a conventional powder metallurgy and smelting process. The invention is not intended to be limited by the following examples, but the invention is limited only by the examples. Example 1: This example is based on the preparation of a raw material powder of a Ni-8w (at.%) target, wherein Ni-8W (at.〇/0) represents an atomic percentage of 92:8. First, the nickel block and the crane # are prepared according to the Ni-8W (at.%) alloy ratio, and then the surface treatment steps of the nickel block and the tungsten piece are performed, and the nickel block and the tungsten piece are placed in a hydrochloric acid solution having a volume concentration of 95% or more. The surface oxide and oil stain are removed by ultrasonic vibration, and the nickel block and the tungsten piece are placed in deionized water, and the hydrochloric acid solution remaining on the surface is removed by ultrasonic vibration, and then dried. Then, the acid-washed recording block and the crane piece are placed in the steel of the vacuum induction smelting furnace and vacuumed. After the vacuum reaches HHT, the temperature is raised to 1500t. 'When the nickel block and the crane piece are piled up After the complete simplification, hold the temperature of 138926.doc 201103999 minutes, the m melting point (4) can be fully melted, and the molten metal soup is evenly distributed under the magnetic field stirring provided by the induction coil. Next, the molten Ni-8W metal soup liquid was poured out from the vacuum induction melting furnace, and the flow rate was controlled at 3 MPa, and the flow rate was controlled at 5 〇 _ Ar rolling 'spraying molten state _8 霄 metal soup liquid It is atomized into a nickel alloy powder.

接著,於一腔體中利用乂氣繼續喷擊加速冷卻霧化後之 鎳口金叙胃’待鎳合金粉體冷卻後,再進篩分步驟。在本 實施例中’篩分步驟係可利用篩分機將粒度大於150㈣以 上之鎳合金粉體篩分移除 ^ 筲下粒度小於1 5 0 μηι之鎳合金 粉體。 、5荨錦σ金粉體之晶粒粒徑約1 〇 μηι,並且根據 能量散佈光譜儀(EDS)之實際分析結果得知,本發明製作 之鎳《金㈣元全合金化’成分為請⑷%)。另外, 由X光繞射刀析結果得知,本發明所製備之鎳合金粉體只 出見Νι之FCC之繞射峰’並未出之之繞射峰,此 代表Νι及W&全合金化,目㈣b 最後’以不錄鋼 小時後,可製得晶 金乾材。 封罐後進行熱均壓製程,於900°C持溫2 粒粒度為5〜50 μηι且完全合金化之鎳合 圖2顯示以本發 之顯微組織結構圖 圖2中可清楚得知 且該專晶粒之分佈 8月製造方法所製得之Ni-8W鎳合金靶材 其中右下角之比例尺標為20 μηι,由 ’該錦合金靶材不僅具有細緻之晶粒, 亦非常均勻。 138926.doc 201103999 實例2 : 本實例係以Ni-17Fe-8W(at·%)靶材之原料粉末的製作為 例。首先’按照Ni-17Fe-8W(at.%)合金比例準備鎳塊、鐵 塊及鶴粉,接著進行鎳塊及鐵塊之表面處理步驟,將錄塊 及鐵塊置於體積濃度95%以上的鹽酸溶液中,以超音波震 動方式去除表面氧化物及油污,再將鎳塊及鐵塊置於去離 子水中’以超音波震動方式去除殘留在表面的鹽酸溶液 後,再予°以烘乾。 接著’將酸洗過後之鎳塊及鐵塊以及鎢粉放入真空感應 熔煉爐之坩鍋中並抽成真空,待真空度達到1〇-\〇〇1以上後 開始升溫至170(TC,當坩鍋中之鎳塊、鐵塊及鎢粉完全熔 化後,於1700°C持溫5分鐘,確保高炫點之鎢粉能充分溶 解,並在一感應線圈所提供之磁場攪拌下使熔融金屬湯液 成分均勻。 接著,將熔融Ni-17Fe-8W金屬湯液自真空感應熔煉爐之 坩堝中倒出,並利用Ar氣喷擊熔融Ni_17Fe_8W金屬湯液使 其霧化成鎳合金粉體。 接著,將霧化之鎳合金粉體於腔體靜置4小時,讓鎳合 金粉體自然冷卻。待鎳合金粉體冷卻後,再進行筛分步 驟。在本實施例中,篩分步驟係可利用篩分機將粒度大於 200 μιη以上之鎳合金粉體篩分移除,留下粒度小於2〇〇 μιη 之錄合金粉體’並真空封裝保存。 其中,該等鎳合金粉體之晶粒粒徑約1〇 μιη,並且根據 能量散佈光譜儀(EDS)之實際分析結果得知,本發明製作 138926.doc 201103999 之鎳合金粉體完全合金化,成分為Nii6 8Fe7 9w (at·%) 0 最後,進行熱壓製程,於l00(rc持溫2小時後,即可製 得晶粒細緻且完全合金化之録合金乾材。 圖3顯示以本發明製造方法所製得之州」7Fe_8w鎳合金 靶材之顯微組織結構圖,其中右下角之比例尺標為2〇 由圖3巾可清楚得知,_合錄料僅具有細緻之 晶粒’且該等晶粒之分佈亦非常均勻。 本發明鎳合金靶材之製造方法不需使用價格較為昂貴之 Νι粉體及W粉體為原料、不需使用相當昂責的電漿燒結設 備進打Ni、W粉體的燒結,並且不需經冷軋製程及在氣氛 保護下進行再結晶退火處理,即可快速、大量製備製得鎳 合金靶材,故製造方法簡單且可減少製造時間。再者,本 發明之製造方法所製得之鎳合金靶材無成分偏析、具細緻 晶粒、晶粒分佈均勻且完全合金化,故具有較高之濺鍍品 質。 上述實施例僅為說明本發明之原理及其功效,並非限制 本發明。因此習於此技術之人士對上述實施例進行修改及 變化仍不脫本發明之精神。本發明之權利範圍應如後述之 申請專利範圍所列。 【圖式簡單說明】 圖1顯示本發明鎳合金靶材之製造方法流程圖; 圖2顯示以本發明製造方法所製得之Ni_8W鎳合金靶材 之顯微組織結構圖;及 138926.doc •10· 201103999 圖3顯示以本發明製造方法所製得之Ni-17Fe-8W鎳合金 靶材之顯微組織結構圖。Then, the helium gas is continuously sprayed in a cavity to accelerate the cooling and atomization of the nickel port. The nickel alloy powder is cooled, and then the sieve step is performed. In the present embodiment, the 'sieving step' is performed by sieving a nickel alloy powder having a particle size of more than 150 (four) or more by a sieving machine to remove a nickel alloy powder having a particle size of less than 150 μm. The grain size of the 5 荨 σ 金 gold powder is about 1 〇μηι, and according to the actual analysis results of the energy dispersive spectrometer (EDS), the nickel "gold (four) element fully alloyed" component produced by the present invention is requested (4). %). In addition, it is known from the results of X-ray diffraction knife that the nickel alloy powder prepared by the present invention only sees the diffraction peak of the FCC diffraction peak of Νι, which represents the Νι and W& all alloys. (4) b Finally, after the hour of no steel recording, the crystal gold dry material can be obtained. After the canning, the heat is uniformly pressed, and the temperature is maintained at 900 ° C. The particle size is 5 to 50 μηι and the fully alloyed nickel is shown in Fig. 2. The microstructure of the present invention is clearly shown in Fig. 2 The special grain is distributed in the Ni-8W nickel alloy target produced by the August manufacturing method, wherein the scale in the lower right corner is 20 μηι, which is not only fine grained but also very uniform. 138926.doc 201103999 Example 2: This example is an example of the production of a raw material powder of a Ni-17Fe-8W (at·%) target. First, prepare nickel blocks, iron blocks and crane powder according to the ratio of Ni-17Fe-8W (at.%) alloy, then carry out the surface treatment steps of nickel blocks and iron blocks, and place the recording blocks and iron blocks at a volume concentration of 95% or more. In the hydrochloric acid solution, the surface oxide and oil stain are removed by ultrasonic vibration, and then the nickel block and the iron block are placed in deionized water. After removing the hydrochloric acid solution remaining on the surface by ultrasonic vibration, the film is dried. . Then, the nickel block and the iron block and the tungsten powder after pickling are placed in a crucible of a vacuum induction melting furnace and evacuated, and the temperature is raised to 170 (TC, after the vacuum reaches 1 〇-\〇〇1 or more. When the nickel block, iron block and tungsten powder in the crucible are completely melted, hold the temperature at 1700 ° C for 5 minutes to ensure that the high-taste tungsten powder is fully dissolved and melted under the magnetic field provided by the induction coil. The metal soup solution is uniformly distributed. Next, the molten Ni-17Fe-8W metal soup liquid is poured out from the crucible of the vacuum induction melting furnace, and the Ni_17Fe_8W metal soup liquid is sprayed by Ar gas to be atomized into a nickel alloy powder. The atomized nickel alloy powder is allowed to stand in the cavity for 4 hours, and the nickel alloy powder is naturally cooled. After the nickel alloy powder is cooled, the sieving step is further performed. In this embodiment, the sieving step can be performed. The nickel alloy powder having a particle size of more than 200 μm is sieved and removed by using a sieving machine, and the alloy powder having a particle size of less than 2 〇〇μηη is left and stored in a vacuum package. The crystal grains of the nickel alloy powder are contained therein. The diameter is about 1〇μηη, and the spectrum is scattered according to energy. According to the actual analysis results of the instrument (EDS), the nickel alloy powder of the invention produced by 138926.doc 201103999 is completely alloyed, and the composition is Nii6 8Fe7 9w (at·%) 0. Finally, the hot pressing process is performed at l00 (rc) After 2 hours of temperature, the fine-grained and fully alloyed alloy dry material can be obtained. Figure 3 shows the microstructure of the 7Fe_8w nickel alloy target produced by the manufacturing method of the present invention, wherein right The scale of the lower corner is marked as 2〇. It can be clearly seen from the towel of Fig. 3. The composite material has only fine crystal grains 'and the distribution of the crystal grains is very uniform. The method for manufacturing the nickel alloy target of the invention does not need to be used. The expensive powder of Νι powder and W powder is used as raw material, and the sintering of Ni and W powders is not required without using a considerable plasma sintering equipment, and recrystallization is carried out without cold rolling and under the protection of the atmosphere. Annealing treatment can produce nickel alloy target quickly and in large quantities, so the manufacturing method is simple and the manufacturing time can be reduced. Furthermore, the nickel alloy target obtained by the manufacturing method of the invention has no component segregation and fine crystal grains. , the grain distribution is uniform and complete It is alloyed and therefore has a high sputter quality. The above embodiments are merely illustrative of the principles and effects of the present invention, and are not intended to limit the present invention. Therefore, those skilled in the art have made modifications and changes to the above embodiments. The scope of the invention should be as described in the following claims. BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flow chart showing a method for producing a nickel alloy target of the present invention; FIG. 2 is a view showing the manufacturing method of the present invention. The microstructure of the Ni_8W nickel alloy target obtained; and 138926.doc •10·201103999 Fig. 3 shows the microstructure of the Ni-17Fe-8W nickel alloy target prepared by the manufacturing method of the present invention.

138926.doc -11 -138926.doc -11 -

Claims (1)

201103999 七、申請專利範圍: 一種鎳合金乾材之製造方法,包括以下步驟: (a) 提供鎳金屬及至少一第—合金元素; (b) 進行一真空熔煉步驟,以形成一合金溶液; (c) 霧化該合金溶液,以形成鎳合金粉體; (d) 進行一筛分步驟,以選取小於一設定粒度之鎳合金 粉體;及201103999 VII. Patent application scope: A method for manufacturing a nickel alloy dry material, comprising the steps of: (a) providing nickel metal and at least one first alloying element; (b) performing a vacuum melting step to form an alloy solution; c) atomizing the alloy solution to form a nickel alloy powder; (d) performing a sieving step to select a nickel alloy powder having a smaller than a set particle size; (e) 成型及緻密化該鎳合金粉體,以形成鎳合金靶材。 如"月求項1之製造方法,其中在步驟(a)中係選用片狀、 粉體狀或屑狀之第一合金元素。 如請求項1之製造方法,其中在步驟(幻中該第一合金元 素係選自鉬(Mo)、鎢(W) '钽(Ta)、姶(Hf)、釕(Ru)、銖 (Re)、鍅(Zr)或鈮(Nb)。 4·如凊求項丨之製造方法,其中在步驟(3)之前另包括以下 步驟: (al)利用酸性溶液移除該鎳金屬及該第一合金元素表面 之氧化物及污染物; (a2)移除該鎳金屬及該第一合金元素表面之酸性溶液; 及 (a3)乾燥該鎳金屬及該第一合金元素。 5·如請求項4之製造方法,其中在步驟(al)中,該酸性溶液 之體積濃度係為95°/❶以上。 6.如請求項4之製造方法,其中在步驟(al)中,該酸性溶液 係選自鹽酸或硝酸。 138926.doc 201103999 7. 如請求項4之製造方法 移除該鎳金屬及該第一 8. 如請求項3之製造方法 分比係為5%至20%。 ’其中在步驟(a2)中係以去離子水 合金元素表面之酸性溶液。 ,其中該第一合金元素之重量百 9.如請求項8之製造方法, 金元素。 其中該第一合金元素係為鎢合 10.如請求項3之製造方法,其(e) Forming and densifying the nickel alloy powder to form a nickel alloy target. The manufacturing method of the above-mentioned item 1, wherein the first alloying element in the form of a sheet, a powder or a crumb is used in the step (a). The manufacturing method of claim 1, wherein in the step (the first alloying element is selected from the group consisting of molybdenum (Mo), tungsten (W) '钽 (Ta), 姶 (Hf), 钌 (Ru), 铢 (Re) , 鍅 (Zr) or 铌 (Nb). The manufacturing method of the 丨 丨 , , , , , , , , , 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 An oxide and a contaminant on the surface of the alloying element; (a2) removing the nickel metal and an acidic solution on the surface of the first alloying element; and (a3) drying the nickel metal and the first alloying element. The manufacturing method, wherein, in the step (al), the volume concentration of the acidic solution is 95°/❶ or more. 6. The method of claim 4, wherein in the step (al), the acidic solution is selected from the group consisting of Hydrochloric acid or nitric acid. 138926.doc 201103999 7. The method of claim 4 removes the nickel metal and the first 8. The manufacturing method according to claim 3 is 5% to 20%. A2) is an acidic solution on the surface of the deionized water alloying element. The weight of the first alloying element is 100. The production method 8, the alloying elements. Wherein the first alloy is a tungsten-based element 10. The method for manufacturing the bonded requested item 3, which is 中在步驟(a)中另提供一第二 之熔點低於該第一合金元素 合金元素,該第二合金元素 之熔點。 11·如請求項10之製造方法,立 ㈣、銅(CU)或鋅叫 第—合h素係選自袭 A如請求物之製造方法,其巾_ 大於50%,該第一合金元 罝百刀比4 2〇%,盆餘之…、 量百分比係為% 如請求们之製造方法,第:5金…量。 熔煉爐或真空電弧熔煉爐中進 工感力 14·Γ求項1之製造方法,其中在步驟:中;1。 溫度係為1500°c至175〇t^ 具二熔煉4 15. 如請求们之製造方法,其中在 之真空度係為1〇·3托(torr)以上。 ,真空熔煉4 16. 如請求们之製造方法,其中 性氣體以噴擊方式霧化該合金溶液。()中係利用高㈣ I7·如請求項之製造方法,其 或氮氣(N2)。 f氣體係為氩氣(Ar 138926.doc 201103999 a如請求項16之製造方法,其中在步驟 以壓力為⑴MPa、流速為5 ^性氣體係 溶液。 至100 m/s嗔擊霧化該合金 19. 如請求項丨之製造方法,其 料聰 ^ ?在步驟⑷之後另包括-冷 部步驟,以冷卻霧化後之該鎳合金粉體。 20. 如請求項19之製造方法, ... 二 中在該冷部步驟中利用氬氣 乳以喷擊方式冷卻霧化後之該錄合金粉體。 21_如請求項19之製造方法, Μ方m 步财利用自然 冷部方式冷卻霧化後之該鎳合金粉體。 22. 如請求項1之製造方 金粉體+ ”中在步驟⑷中所篩分之鎳合 ’之該设定粒徑係小於200微米(μηι)。 23. 如請求項1之製造方 亦赦仏r 其中在步驟(e)中係以熱壓製程 或二均壓製程進行該成型及緻密化步驟。 24. =求項!之製造方法,其中在步驟⑷中成 度係為嗔至贼,成型及緻密化之時間係 馬U.5至3小時。 月长項1之製造方法,其係應用於磁記 產業或半導體產業之薄膜缝製程。 光電 138926.docFurther, in the step (a), a second melting point is lower than the first alloying element alloying element, and the melting point of the second alloying element. 11. The manufacturing method of claim 10, the vertical (four), copper (CU) or zinc is called the first-in-one system selected from the method of manufacturing the request material, the towel _ is greater than 50%, the first alloy element 罝The ratio of the hundred knives to 4 2 〇%, the rest of the basin..., the percentage of the percentage is %, such as the manufacturing method of the requester, the number: 5 gold. Inductive force in a smelting furnace or a vacuum arc melting furnace 14. The manufacturing method of the item 1 is in the step: 1. The temperature is 1500 ° C to 175 〇 t ^ with two smelting 4 15. The manufacturing method of the requester, wherein the degree of vacuum is 1 〇 3 torr (torr) or more. , Vacuum Melting 4 16. As a manufacturing method of the requester, the neutral gas atomizes the alloy solution by spraying. () The middle system utilizes high (four) I7. The manufacturing method of the request item, or nitrogen (N2). The f gas system is argon gas (Ar 138926.doc 201103999 a. The manufacturing method of claim 16, wherein the pressure is (1) MPa in the step, and the flow rate is 5 ^ gas system solution. The atomization of the alloy is up to 100 m/s. The method of manufacturing the item of claim ,, after the step (4), further comprises a cold portion step to cool the atomized nickel alloy powder. 20. The method of claim 19, ... In the cold part step, the atomized milk is used to cool the atomized alloy powder by means of argon gas. 21_ The manufacturing method of claim 19, the m-square m-step cooling and atomization by the natural cold part method Then, the nickel alloy powder is 22. The set particle diameter of the nickel alloy sifted in the step (4) in the production of the gold powder + ” of claim 1 is less than 200 μm (μηι). The manufacturing method of claim 1 is also wherein the step of forming and densifying is carried out in step (e) by a hot press or a two-pass process. 24. = the manufacturing method of the item, wherein in step (4) The degree of success is from 嗔 to thief, and the time of forming and densification is U. 5 to 3 hours. The manufacturing method of the long term 1 is applied to the film sewing process of the magnetic recording industry or the semiconductor industry. Optoelectronics 138926.doc
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Cited By (6)

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TWI558819B (en) * 2016-01-22 2016-11-21 光洋應用材料科技股份有限公司 Nickel alloy sputtering target and nickel alloy layer
TWI622661B (en) * 2013-12-20 2018-05-01 攀時歐洲公司 W-Ni sputtering target and its preparation method and use
TWI659119B (en) * 2017-08-30 2019-05-11 光洋應用材料科技股份有限公司 Nickel-rhenium alloy sputtering target and method of preparing the same
CN110938757A (en) * 2018-12-27 2020-03-31 河南城建学院 A kind of preparation method of ultra-high-strength textured nickel-based alloy base tape
CN113290427A (en) * 2021-05-24 2021-08-24 宁波江丰电子材料股份有限公司 Treatment method of high-purity nickel evaporation material
TWI803774B (en) * 2019-09-19 2023-06-01 日商日立金屬股份有限公司 target

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Publication number Priority date Publication date Assignee Title
TWI622661B (en) * 2013-12-20 2018-05-01 攀時歐洲公司 W-Ni sputtering target and its preparation method and use
US11746409B2 (en) 2013-12-20 2023-09-05 Plansee Se Process for producing and using a W—Ni sputtering target
TWI558819B (en) * 2016-01-22 2016-11-21 光洋應用材料科技股份有限公司 Nickel alloy sputtering target and nickel alloy layer
TWI659119B (en) * 2017-08-30 2019-05-11 光洋應用材料科技股份有限公司 Nickel-rhenium alloy sputtering target and method of preparing the same
CN110938757A (en) * 2018-12-27 2020-03-31 河南城建学院 A kind of preparation method of ultra-high-strength textured nickel-based alloy base tape
CN110938757B (en) * 2018-12-27 2021-05-07 河南城建学院 A kind of preparation method of ultra-high-strength textured nickel-based alloy base tape
TWI803774B (en) * 2019-09-19 2023-06-01 日商日立金屬股份有限公司 target
CN113290427A (en) * 2021-05-24 2021-08-24 宁波江丰电子材料股份有限公司 Treatment method of high-purity nickel evaporation material

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