TW201221674A - Crti-based alloy and sputtering target material, perpendicular magnetic recording medium, and processes for producing same - Google Patents

Crti-based alloy and sputtering target material, perpendicular magnetic recording medium, and processes for producing same Download PDF

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TW201221674A
TW201221674A TW100129208A TW100129208A TW201221674A TW 201221674 A TW201221674 A TW 201221674A TW 100129208 A TW100129208 A TW 100129208A TW 100129208 A TW100129208 A TW 100129208A TW 201221674 A TW201221674 A TW 201221674A
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crti
sputtering
cr2ti
target
based alloy
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TW100129208A
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Chinese (zh)
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TWI500791B (en
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Hiroyuki Hasegawa
Toshiyuki Sawada
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Sanyo Special Steel Co Ltd
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    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
    • G11B5/8404—Processes or apparatus specially adapted for manufacturing record carriers manufacturing base layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B22F3/15—Hot isostatic pressing
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/06—Alloys based on chromium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/62—Record carriers characterised by the selection of the material
    • G11B5/73—Base layers, i.e. all non-magnetic layers lying under a lowermost magnetic recording layer, e.g. including any non-magnetic layer in between a first magnetic recording layer and either an underlying substrate or a soft magnetic underlayer
    • G11B5/739—Magnetic recording media substrates
    • G11B5/73911—Inorganic substrates
    • G11B5/73917—Metallic substrates, i.e. elemental metal or metal alloy substrates
    • G11B5/73919—Aluminium or titanium elemental or alloy substrates
    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
    • G11B5/851—Coating a support with a magnetic layer by sputtering

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Vapour Deposition (AREA)
  • Powder Metallurgy (AREA)
  • Manufacturing Of Magnetic Record Carriers (AREA)
  • Magnetic Record Carriers (AREA)

Abstract

The present invention provides: a CrTi-based alloy or sputtering target material which comprises 35 to 65at% of Ti with the balance consisting of Cr and unavoidable impurities; and processes for producing the same. The CrTi-based alloy or sputtering target material has an intensity ratio of [I(Cr2Ti)/I(Cr)] of 0.50 or lower, wherein [I(Cr)] represents the X-ray diffraction intensity of Cr(110), and [I(Cr2Ti)] represents the X-ray diffraction intensity of Cr2Ti(311). According to the present invention, the content of compounds in a CrTi-based alloy or sputtering target material can be reduced, which makes it possible to suppress the generation of particles during sputtering and thus enhance the yield of sputtering film.

Description

201221674 六、發明說明： 關聯申請案的相互參照 本申請案係以20 1 0年8月1 7日申請的日本發明專利 201 0-1 82M4號爲基礎，主張優先權，藉由參照其全體的 * 揭示內容而倂入本說明書中。 【發明所屬之技術領域】 〇 本發明關於CrTi系合金及濺鍍用靶材以及彼等的製造 方法，其係用於藉由濺鍍來形成薄膜，已抑制化合物的生 '成。又’本發明亦關於使用CrTi系合金及濺鍍用靶材所製 造的垂直磁記錄介質以及其製造方法。 【先前技術】 一般地，CrTi系靶係使用垂直磁記錄介質的基底膜， 藉由將純Cr粉末與純Ti粉末熱成形而得。該CrTi系靶含有 〇 許的脆的化合物相，濺鑛時脆的化合物相係造成粒子，粒 子對灘鍍膜附著而降低製品良率。因此，必須減少c r T i祀 中的化合物。 作爲減少如此的CrTi靶中之化合物用的對策，例如像 特公昭64-2659號公報（專利文獻i )中所揭示，藉由將熔 融金屬急速冷卻，而減少化合物。然而，CrTi系靶在以粉 末冶金法製作材料時有無法成爲熔融金屬的問題。 另方面，通吊爲粉末燒結體時’係以熔點的80%左 右之溫度成形》例如，CrTi系類似組成者，如特開2〇〇3_ 201221674 226 96 3號公報（專利文獻2)中所揭示’藉由熱壓而在 1200它以上的溫度成形。又’如特開2002_212607號公報（ 專利文獻3 )中所揭示，藉由頂鍛法在I 200 °C的溫度成形 。然而，此燒結溫度愈高，則化合物愈有增加的傾向。 此等專利文獻2及3，由於皆成形溫度高，靶中的化合 物係多地存在，故在濺鍍時產生許多的粒子’有降低濺鍍 膜的製品良率之問題。 先前技術文獻 專利文獻 專利文獻1 :特公昭64-265 9號公報 專利文獻2 :特開2003-226963號公報 專利文獻3 :特開2002-212607號公報 【發明內容】 本發明者們此番得到以下的知識：藉由減少濺鍍靶中 的化合物，可提供能減少在濺鍍膜所產生的粒子之CrTi系 合金及擺鍍用祀材。 因此’本發明之目的係在於減少CrTi系合金及濺鍍靶 材中的化合物，及藉此抑制濺鍍時的粒子發生，而提高濺 鍍膜的製品良率。 依照本發明的一個態樣，提供一種CrTi系合金，其係 含有35〜65原子％的丁丨，剩餘部分由Cr及無可避免的雜質 所構成之CrTi系合金， 前述CrTi系合金具有〇.5〇以下之ChTi ( 3 1 1 )的X射線 201221674 繞射強度〔I ( Cr2Ti )〕對Cr ( 1 1 0 )的X射線繞射強度 〔1 ( Cr )〕之強度比〔I ( Cr2Ti ) /1 ( Cr )〕。 依照本發明的另一態樣，提供一種CrTi系濺鍍用靶材 ’其係含有35〜65原子％的1^，剩餘部分由Cr及無可避免 的雜質所構成之濺鍍靶材， ' 前述濺鍍靶材具有0.50以下之Ci^Ti ( 311 )的X射線 繞射強度〔I ( Cr2Ti )〕對Cr ( 1 1〇 )的X射線繞射強度 〇 "(以）〕之強度比〔1( Cr2Ti) /1 ( Cr)〕。 依照本發明的再一態樣，提供一種垂直磁記錄介質， 、’其具有使用前述CrTi系濺鍍用靶材的濺鍍所形成之基底膜 〇 依照本發明的又一態樣，提供一種方法，其係前述 CrTi系合金或CrTi系濺鍍用靶材之製造方法，該方法包含 以下者所成： 準備具有造成前述合金的全體組成之原料粉末， 〇 將該原料粉末在8 0 0〜1丨〇 〇 熱成形。 依照本發明的還一態樣，提供一種方法，其係前述垂 記錄介質之製造方法，該方法包含以下者所成： 準備具有造成前述基底膜的全體組成之原料粉末， 將該原料粉末在8〇0〜1100°C熱成形而成爲CrTi系濺鍍 材， it 該CrTi系濺鍍靶材進行濺鍍，而形成前述基底膜 201221674 【實施方式】 〔實施發明的形態〕 以下，詳細說明本發明。本發明的CrTi系合金、CrTi 系濺鍍用靶材、及垂直磁記錄介質的基底膜，係含有35〜 65原子％的Ti，剩餘部分由Cr及無可避免的雜質所構成之 CrTi系合金，較佳爲由此等成分所實質組成（consisting essentially of)，更佳爲僅由此等成分所組成（consisting of) 〇CrTi系合金及靶材具有0.50以下之Cr2Ti(311)的X 射線繞射強度〔I ( Cr2Ti )〕對Cr ( 110 )的X射線繞射強 度〔I(Cr)〕之強度比〔l(Cr2Ti) /I(Cr)〕。 本發明的CrTi系合金、CrTi系濺鍍用靶材、及垂直磁 記錄介質之基底膜，係含有35〜65原子％的丁丨，較佳含有 40〜60原子％。Ti若未達35原子％或超過65原子％，則使用 合金作爲濺鍍靶材時，濺鍍後的膜係不成爲非晶形。 於本發明的CrTi系合金、CrTi系濺鍍用靶材、及垂直 磁記錄介質的基底膜中，Cr2Ti ( 3 1 1 )的X射線繞射強度 〔I ( Cr2Ti )〕對 Cr ( 1 1〇 )的 X射線繞射強度〔I ( Cr )〕 之強度比〔I ( Cr2Ti ) /1 ( Cr )〕爲0.50以下，較佳爲0.07 以下’更佳爲0.03以下。此強度比高於〇.5〇時，會產生許 多的粒子。 本發明的CrTi系合金及CrTi系濺鍍用靶材，係可藉由 將原料粉末在800〜11〇(rc熱成形，較佳在800〜1〇5〇。€熱 成形而製造。若未達8 〇 〇 〇c，則得不到充分的密度。另一 方面’若爲超過1〖00°C的溫度，則X射線繞射強度比値變 201221674 大，而且在濺鏟時產生許多粒子，粒子對濺鍍膜附著而降 低製品良率。熱成形溫度在頂鍛（upsetting)法中，上限 更佳爲1 000°C以下，在HIP法中更佳爲900°C以下。 依照本發明的較佳態樣，在熱成形後，將成形體自熱 成形溫度以144〜3 6000°C/hr的冷卻速度冷卻，可進一步增 _ 大化合物的生成抑制效果。即，因爲藉由以上述的冷卻速 度進行急速冷卻，可將高溫相的CrTi固溶體維持在低溫， 〇 抑制固溶體往化合物的變態。上述冷卻速度的下限之較佳 速度爲500°c/hr以上。 ' 本發明的垂直磁記錄介質係與上述同樣，可經由將原 料粉末在800〜1100 °C熱成形，較佳在800〜1050 °C，而成 爲CrTi系濺鑛靶材後，使用CrTi系濺鍍靶材進行濺鍍，形 成基底膜而製造。基底膜之形成以外的垂直磁記錄介質製 造步驟係可適宜採用以往慣用的步驟，沒有特別的限定。 依照本發明的較佳態樣，基於前述理由，較佳爲在熱成形 〇 後，於上述濺鍍之前，將靶材自成形溫度以144〜 36000 °C/hr的冷卻速度冷卻，當時上述冷卻速度之下限的 較佳速度爲500°C/hr以上。 實施例 以下，藉由實施例來具體說明本發明。 以表1中所示的Cr-Ti合金組成，摻合粒度爲25〇μιη以 下的純C r粉末與粒度爲1 5 0 μ m以下的純τ i粉末而混合。將 所得之混合粉塡充於由鋼材質所成的封入罐內，於到達真 -9- 201221674 空度lO^P a以上，脫氣真空封入。然後，當爲HIP (熱等向 加壓）時，在加熱溫度800〜1100 °C、成形壓力150MP a、 加熱保持時間1小時的條件下成形後，於表1所示的條件下 ，以到3 00°c爲止，藉由空氣冷卻（No.3、4、5、7、1 1、 12、13、15、16、19、21、22、23、25、29、30、3 1 3 3 )或水冷（Νο·8、9、17' 26、27及34)來控制冷卻速度 ，以製作成形體。另一方面，當爲頂锻法時，在加熱溫度 8 00〜1100它、成形壓力500河？3、加熱保持時間1小時的條 件下成形後，於表1所示的條件下，以到30(TC爲止，藉由 空氣冷卻或水冷來控制冷卻速度，以製作成形體。接著， 對所得之成形體施予機械加工，以製作靶。 對於所得之靶，進行化合物波峰比〔I ( Cr2T〇 /1 ( Cr )〕之測定。此測定係X射線源爲Cu-Κα線，以掃描速率 4°/min的條件之X射線繞射來進行。又，粒子的評價係使 用所得之IE，在直徑95mm、板厚1.75mm的銘基板上，藉 由DC磁控濺鍍，以0.9P a的Ar氣體壓力來成膜，藉由光學 表面分析器（Optical Surface Analyzer)來計算粒子數。 此等的結果係如表1中所示。 -10 - 201221674201221674 VI. INSTRUCTIONS: Cross-Reference of Related Application This application is based on Japanese Invention Patent No. 201 0-1 82M4 filed on August 17, 2010, claiming priority, by reference to its entirety. * Reveal the content and break into this manual. [Technical Field of the Invention] The present invention relates to a CrTi-based alloy, a target for sputtering, and a method for producing the same, which are used for forming a thin film by sputtering, and suppressing the formation of a compound. Further, the present invention relates to a perpendicular magnetic recording medium produced by using a CrTi-based alloy and a target for sputtering, and a method for producing the same. [Prior Art] Generally, a CrTi-based target system is obtained by using a base film of a perpendicular magnetic recording medium by thermoforming a pure Cr powder and a pure Ti powder. The CrTi-based target contains a brittle compound phase, and the brittle compound phase causes particles during sputtering, and the particles adhere to the beach coating to lower the yield of the product. Therefore, it is necessary to reduce the compound in c r T i祀. As a measure for reducing the amount of the compound in the CrTi target, for example, as disclosed in Japanese Patent Publication No. Sho 64-2659 (Patent Document i), the molten metal is rapidly cooled to reduce the compound. However, the CrTi-based target has a problem that it cannot be a molten metal when a material is produced by a powder metallurgy method. On the other hand, in the case of a powder sintered body, it is formed at a temperature of about 80% of the melting point. For example, a CrTi-based composition is used, for example, in Japanese Laid-Open Patent Publication No. 2-201221674 226 96 3 (Patent Document 2). It is revealed that it is formed at a temperature of 1200 or more by hot pressing. Further, as disclosed in JP-A-2002-212607 (Patent Document 3), it is formed by a top forging method at a temperature of I 200 °C. However, the higher the sintering temperature, the more the compound tends to increase. In these Patent Documents 2 and 3, since the molding temperature is high and the compound in the target is present in a large amount, a large number of particles are generated during sputtering, which has a problem of lowering the yield of the product of the sputtering film. CITATION LIST Patent Literature Patent Literature 1: JP-A-2002-212963 (Patent Document 3) JP-A-2002-212607 (Invention) The present inventors have The following knowledge: By reducing the compound in the sputtering target, it is possible to provide a CrTi-based alloy and a pendulum plate for reducing the particles generated in the sputtering film. Therefore, the object of the present invention is to reduce the compound in the CrTi-based alloy and the sputtering target, and thereby suppress the occurrence of particles during sputtering, thereby improving the product yield of the sputtering film. According to an aspect of the present invention, there is provided a CrTi-based alloy comprising 35 to 65 atom% of butadiene, the remainder being CrTi-based alloy composed of Cr and inevitable impurities, and the CrTi-based alloy has a crucible. The intensity ratio of the X-ray 201221674 diffraction intensity [I (Cr2Ti)] to the X-ray diffraction intensity [1 (Cr)] of Cr (1 1 0) below ChTi ( 3 1 1 ) [I ( Cr2Ti ) /1 (Cr)]. According to another aspect of the present invention, there is provided a CrTi-based sputtering target which contains 35 to 65 atom% of a sputtering target which is composed of Cr and inevitable impurities, ' The sputtering target has an intensity ratio of an X-ray diffraction intensity [I(Cr2Ti)] of Cr(1 1〇) to a Cr (1 1〇) X-ray diffraction intensity 〇" [1(Cr2Ti) /1 (Cr)]. According to still another aspect of the present invention, there is provided a perpendicular magnetic recording medium having a base film formed by sputtering using the aforementioned CrTi-based sputtering target. According to still another aspect of the present invention, a method is provided. The method for producing the CrTi-based alloy or the CrTi-based sputtering target, the method comprising the steps of: preparing a raw material powder having a total composition of the alloy, and preparing the raw material powder at 8000 to 1 Hot forming. According to still another aspect of the present invention, there is provided a method of producing the above-described perpendicular recording medium, which comprises the steps of: preparing a raw material powder having a total composition of the base film, the raw material powder being 8 〇 0 to 1100 ° C is hot-formed to form a CrTi-based sputtering material, and the CrTi-based sputtering target is sputtered to form the base film 201221674. [Embodiment] [Embodiment of the Invention] Hereinafter, the present invention will be described in detail. . The CrTi-based alloy, the CrTi-based sputtering target, and the base film of the perpendicular magnetic recording medium of the present invention contain a CrTi-based alloy containing 35 to 65 at% of Ti and the balance being Cr and inevitable impurities. Preferably, the composition is substantially the same as the composition, and more preferably consists of only the composition of the composition of the CrTi-based alloy and the target having an X-ray around Cr2Ti (311) of 0.50 or less. The intensity ratio [I(Cr2Ti) / I(Cr)] of the X-ray diffraction intensity [I(Cr)] of the incident intensity [I (Cr2Ti)] to Cr (110). The CrTi-based alloy, the CrTi-based sputtering target, and the base film of the perpendicular magnetic recording medium of the present invention contain 35 to 65 atom% of butadiene, preferably 40 to 60% by atom. When Ti is less than 35 atom% or exceeds 65 atom%, when an alloy is used as a sputtering target, the film after sputtering does not become amorphous. In the CrTi-based alloy, the CrTi-based sputtering target, and the base film of the perpendicular magnetic recording medium of the present invention, the X-ray diffraction intensity [I (Cr2Ti)] of Cr2Ti (3 1 1 ) is Cr (1 1 〇). The intensity ratio [I (Cr2Ti ) /1 ( Cr )] of the X-ray diffraction intensity [I (Cr)] is 0.50 or less, preferably 0.07 or less, more preferably 0.03 or less. When the intensity ratio is higher than 〇.5〇, many particles are produced. The CrTi-based alloy and the CrTi-based sputtering target of the present invention can be produced by thermoforming a raw material powder at 800 to 11 Torr (rc thermoformed, preferably 800 to 1 Torr. If it is 8 〇〇〇c, it will not get sufficient density. On the other hand, if it is more than 1 00 °C, the X-ray diffraction intensity is larger than the enthalpy change 201221674, and many particles are generated when the shovel is spattered. The particles adhere to the sputtering film to lower the yield of the product. The hot forming temperature is preferably more than 1 000 ° C in the upsetting method, and more preferably 900 ° C or less in the HIP method. In a preferred embodiment, after the hot forming, the formed body is cooled from the hot forming temperature at a cooling rate of 144 to 3 6000 ° C / hr, thereby further increasing the formation inhibition effect of the large compound. The cooling rate is rapidly cooled to maintain the CrTi solid solution in the high temperature phase at a low temperature, and the solid solution is inhibited from being metamorphosed to the compound. The preferred lower limit of the cooling rate is 500 ° C / hr or more. The perpendicular magnetic recording medium is the same as described above, and the raw material powder can be passed. After hot forming at 800 to 1100 ° C, preferably 800 to 1050 ° C, a CrTi-based sputtering target is sputtered using a CrTi-based sputtering target to form a base film, and the base film is formed. The manufacturing process of the perpendicular magnetic recording medium can be suitably carried out by conventionally used steps, and is not particularly limited. According to the preferred embodiment of the present invention, preferably, after the hot forming of the crucible, before the sputtering, The target is cooled from a forming temperature of 144 to 36,000 ° C / hr, and a preferred speed of the lower limit of the cooling rate is 500 ° C / hr or more. EXAMPLES Hereinafter, the present invention will be specifically described by way of examples. The composition of the Cr-Ti alloy shown in Table 1 was blended with a pure Cr powder having a particle size of 25 μm or less and a pure τ i powder having a particle size of 150 μm or less. The obtained mixed powder was charged. In the sealed tank made of steel material, after reaching the true -9-201221674 vacancy lO^P a or more, the degassing vacuum is sealed. Then, when it is HIP (hot isostatic pressing), the heating temperature is 800~ 1100 °C, forming pressure 150MP a, heating retention time 1 After molding under the conditions of the time, under the conditions shown in Table 1, air cooling was performed up to 300 ° C (No. 3, 4, 5, 7, 1 1, 12, 13, 15, 16 19, 21, 22, 23, 25, 29, 30, 3 1 3 3 ) or water-cooled (Νο·8, 9, 17' 26, 27 and 34) to control the cooling rate to produce a shaped body. When it is the top forging method, it is heated at a temperature of 00~1100, and the forming pressure is 500? 3. After molding under the conditions of heating and holding time for 1 hour, under the conditions shown in Table 1, the cooling rate was controlled by air cooling or water cooling until 30 (TC), and then the molded body was produced. The molded body is subjected to mechanical processing to prepare a target. For the obtained target, a compound peak ratio [I (Cr2T〇/1 (Cr)] is measured. The X-ray source is a Cu-Κα line at a scan rate of 4 The X/ray diffraction of the condition of °/min was carried out. Further, the evaluation of the particles was carried out by using a IE obtained on a plate having a diameter of 95 mm and a plate thickness of 1.75 mm by DC magnetron sputtering at 0.9 Pa. Ar gas pressure was used to form a film, and the number of particles was calculated by an optical surface analyzer. The results are shown in Table 1. -10 - 201221674

No 成形方法 組成 (at%) 成形溫度 (•C/h r ) 冷卻速度 CC/hr) X射線繞射強度 [(Cr2Ti)/I(Cr)] 粒子數 判 定 備 1 頂鍛 Cr-35Ti 800 144 0.0232 10 〇 2 頂鍛 Cr*45Ti 1000 144 0.0249 7 〇 3 頂鍛 Cr-45Ti 1000 300 0.0186 5 〇 4 頂鍛 Cr-45Ti 1000 500 0.0171 2 〇 5 頂鍛 Cr-45Ti 1000 1500 0.0146 1 〇 6 頂鍛 Cr-45Ti 1050 2500 0.149 15 〇 7 頂鍛 Cr*35Ti 1050 144 0.138 14 〇 8 頂鍛 Cr-35Ti 1050 36000 0.132 12 〇 9 頂鍛 Cr-65Ti 800 3G000 0.0250 8 〇 10 頂鍛 Cr-50Ti 1000 144 0.0274 6 〇 11 頂鍛 Cr-50Ti 1000 300 0.0262 4 〇 12 頂鍛 Cr-50Ti 1000 500 0.0255 0 〇 13 頂锻 Cr-50Ti 1000 1500 0.0249 0 〇 牛 Μ 頂鍛 Cr- 50Ti 1050 2500 0.365 14 〇 15 頂锻 Cr-65Ti 1050 144 0.413 11 〇 16 頂鍛 Cr-50Ti 1100 300 0.450 15 〇 17 頂鍛 Cr-C5Ti 1050 36000 0.404 10 〇 18 HIP Cr-35Ti 800 144 0.0530 14 〇 明 19 HIP Cr-45Ti 900 500 0.0292 6 〇 20 HIP Cr-45Ti 1000 144 0.0636 14 〇 21 HIP Cr-45Ti 1000 500 0.0541 10 〇 例 22 HIP Cr-45Ti 1000 1500 0.0397 9 〇 23 HIP Cr-45Ti 1000 2500 0.0353 7 〇 24 HIP Cr-45Ti 1050 300 0.198 15 〇 25 HIP Cr-35Ti 1050 144 0.172 14 〇 26 HIP Cr-35Ti 1050 36000 0.132 13 〇 27 HIP Cr-65Ti 800 36000 0.0591 12 〇 28 HIP Cr-50Ti 1000 144 0.0689 11 〇 29 HIP Cr-50Ti 1000 500 0.0633 10 〇 3D HIP Cr-50Ti 1000 J500 0.0533 9 〇 31 HIP Cr-50Ti 1000 2500 0.0489 8 〇 32 HIP Cr-50Ti 1050 300 0.399 11 〇 33 HIP Cr-65Ti 1050 144 0.450 14 〇 34 Η I P Cr-65Ti 1050 36000 0.438 13 〇 35 HIP Cr-&0Ti 1100 500 0.500 14 〇 36 頂鍛 Cr-35Ti 700 80 — - — 37 頂鍛 Cr-35Ti 1200 80 1.29 29 X 38 頂鍛 Cr-65Ti 700 80 —— — - 39 頂鍛 Cr-65Ti 1200 80 1.48 24 X 比 40 HIP Cr-35Ti 700 80 — - - 較 41 HIP Cr-35Ti 1200 80 1.30 28 X 42 HIP Cr-65Ti 700 500 —— 一 一 例 43 HI P Cr-65Ti 1000 80 1.58 26 X 44 HIP Cr-30Ti 1000 500 — - - 45 HIP Cr-70Ti 1050 600 — — - 註)畫底線者係本發明條件外 如表1所示，No. 1〜35係本發明例，No. 36〜45係比 較例。 表1中所示的比較例No · 3 6、3 8及4 0，由於成形溫度 低，冷卻速度慢，所得之粉末成形體的密度低，而不評價 。比較例N 〇 · 3 7、3 9及4 1，由於皆成形溫度高，而且冷卻 -11 - 201221674 速度慢，故χ射線繞射強度之値大，且粒子數大。比較例 No. 42，由於成形溫度低所得之粉末成形體的密度低， 而不評價。比較例N 〇. 4 3，由於成形後的冷卻速度慢，故 X射線繞射強度比的値大，而且粒子數大。 比較例No. 44，由於Ti含量低，濺鍍後的膜係不成爲 非晶形，而不評價。比較例N 〇 . 4 5，由於T i含量高，與比 較例No .44同樣地，濺鏟後的膜係不成爲非晶形，而不評 價。相對於此，可知本發明例的No. 1〜35，由於皆滿足 本發明條件，而可將X射線繞射強度抑制在0.5以下，而且 粒子數小。 如以上，藉由將本發明的原料粉末在800〜1100 °C的 溫度範圍熱成形，而且按照所欲在該熱成形後自成形溫度 以144〜36〇00°C/hr的冷卻速度來急速冷卻，可製造化合物 生成量少之CrTi系合金及CrTi系靶，可謀求濺鍍膜的製品 良率之提高。 -12-No Forming method composition (at%) Forming temperature (•C/hr) Cooling rate CC/hr) X-ray diffraction intensity [(Cr2Ti)/I(Cr)] Particle number determination 1 Top forging Cr-35Ti 800 144 0.0232 10 〇2 Top forging Cr*45Ti 1000 144 0.0249 7 〇3 Top forging Cr-45Ti 1000 300 0.0186 5 〇4 Top forging Cr-45Ti 1000 500 0.0171 2 〇5 Top forging Cr-45Ti 1000 1500 0.0146 1 〇6 Top forging Cr -45Ti 1050 2500 0.149 15 〇7 Top forging Cr*35Ti 1050 144 0.138 14 〇8 Top forging Cr-35Ti 1050 36000 0.132 12 〇9 Top forging Cr-65Ti 800 3G000 0.0250 8 〇10 Top forging Cr-50Ti 1000 144 0.0274 6 〇11 Top forging Cr-50Ti 1000 300 0.0262 4 〇12 Top forging Cr-50Ti 1000 500 0.0255 0 〇13 Top forging Cr-50Ti 1000 1500 0.0249 0 yak 顶 Top forging Cr- 50Ti 1050 2500 0.365 14 〇15 Top forging Cr -65Ti 1050 144 0.413 11 〇16 Top forging Cr-50Ti 1100 300 0.450 15 〇17 Top forging Cr-C5Ti 1050 36000 0.404 10 〇18 HIP Cr-35Ti 800 144 0.0530 14 19明 19 HIP Cr-45Ti 900 500 0.0292 6 〇 20 HIP Cr-45Ti 1000 144 0.0636 14 〇21 HIP Cr-45Ti 1000 500 0.0541 10 Example 22 HIP Cr-45Ti 1000 1500 0.0397 9 〇23 HIP Cr-45Ti 1000 2500 0.0353 7 HIP24 HIP Cr-45Ti 1050 300 0.198 15 〇25 HIP Cr-35Ti 1050 144 0.172 14 〇26 HIP Cr-35Ti 1050 36000 0.132 13 〇27 HIP Cr-65Ti 800 36000 0.0591 12 〇28 HIP Cr-50Ti 1000 144 0.0689 11 〇29 HIP Cr-50Ti 1000 500 0.0633 10 〇3D HIP Cr-50Ti 1000 J500 0.0533 9 〇31 HIP Cr-50Ti 1000 2500 0.0489 8 〇32 HIP Cr-50Ti 1050 300 0.399 11 〇33 HIP Cr-65Ti 1050 144 0.450 14 〇34 Η IP Cr-65Ti 1050 36000 0.438 13 〇35 HIP Cr-&0Ti 1100 500 0.500 14 〇36 Top forging Cr -35Ti 700 80 — - — 37 Upset forging Cr-35Ti 1200 80 1.29 29 X 38 Upset forging Cr-65Ti 700 80 — — - 39 Upset forging Cr-65Ti 1200 80 1.48 24 X to 40 HIP Cr-35Ti 700 80 — - - Compared to 41 HIP Cr-35Ti 1200 80 1.30 28 X 42 HIP Cr-65Ti 700 500 - A case of 43 HI P Cr-65Ti 1000 80 1.58 26 X 44 HIP Cr-30Ti 1000 500 — - - 45 HIP Cr- 70Ti 1050 600 — — — Note) The bottom line is the conditions of the present invention as shown in Table 1. Example, No. 1~35 according to the present invention is based, No. 36~45 system than comparative example. In Comparative Examples No. 3, 3, and 40 shown in Table 1, since the molding temperature was low, the cooling rate was slow, and the density of the obtained powder molded body was low, which was not evaluated. In the comparative examples N 〇 · 3 7, 3 9 and 4 1, since the forming temperature is high and the cooling -11 - 201221674 is slow, the diffraction intensity of the x-ray is large and the number of particles is large. Comparative Example No. 42, the density of the powder molded body obtained by the low molding temperature was low, and was not evaluated. In Comparative Example N 〇. 4 3, since the cooling rate after molding is slow, the X-ray diffraction intensity ratio is large and the number of particles is large. In Comparative Example No. 44, since the Ti content was low, the film system after sputtering did not become amorphous, and was not evaluated. Comparative Example N 〇 . 4 5 . Since the content of Ti was high, similarly to Comparative Example No. 44, the film system after the shovel was not made amorphous, and was not evaluated. On the other hand, it is understood that No. 1 to 35 of the present invention can satisfy the conditions of the present invention, and can suppress the X-ray diffraction intensity to 0.5 or less and the number of particles is small. As described above, the raw material powder of the present invention is thermoformed at a temperature ranging from 800 to 1100 ° C, and is rapidly cooled at a cooling rate of 144 to 36 〇 00 ° C / hr at the self-forming temperature after the hot forming. By cooling, a CrTi-based alloy and a CrTi-based target having a small amount of compound formation can be produced, and the product yield of the sputtered film can be improved. -12-

Claims (1)

201221674 七、申請專利範圍： 1.—種CrTi系合金，其係含有35〜65原子％的Ti，剩 餘部分由Cr及無可避免的雜質所構成之CrTi系合金， 前述CrTi系合金具有0.50以下之Cr2Ti ( 3 1 1 )的X射線 繞射強度〔I ( Cr2Ti )〕對Cr ( 1 10 )的X射線繞射強度 ' 〔1 ( c〇 〕之強度比〔I ( Cr2Ti) /1 ( Cr)〕。 2 ·如申請專利範圍第1項之C rT i系合金，其係僅由3 5 Ο 〜65原子％的Ti、剩餘部分的Cr及無可避免的雜質所構成 〇 • ' 3·—種CrTi系濺鍍用靶材，其係含有35〜65原子％的 Ti ’剩餘部分由Cr及無可避免的雜質所構成之濺鍍靶材， 前述濺鍍靶材具有0.50以下之Cr2Ti ( 311 )的X射線 繞射強度〔I ( Cr2Ti )〕對Cr ( 1 10 )的X射線繞射強度 〔1 ( Cr)〕之強度比〔I ( Cr2Ti ) /1 ( Cr )〕。 4.如申請專利範圍第3項之CrTi系濺鍍用靶材，其係 ϋ 丨堇® 35〜65原子％的Ti、剩餘部分的Cr及無可避免的雜質 所構成。 , 5 · 一種垂直磁記錄介質，其具有使用如申請專利範 ® ϋ 3或4項之CrTi系濺鍍用靶材的濺鍍所形成之基底膜。 6·—種方法，其係如申請專利範圍第1〜4項中任一 € β CfTi系合金或CrTi系濺鍍用靶材之製造方法，該方法 包含以下者所成： $備具有造成前述合金的全體組成之原料粉末， 將該原料粉末在8 00〜1 100t熱成形。 -13- 201221674 7·如申請專利範圍第6項之方法，其更包含在前述熱 成形後’將成形體自成形溫度以l44〜36〇〇(rc/hr的冷卻速 度冷卻。 8 · 種方法’其係如申請專利範圍第5項之垂直磁記 錄介質之製造方法’該方法包含以下者所成： 準備具有造成前述基底膜的全體組成之原料粉末， 將該原料粉末在800〜1100。(：熱成形而成爲CrTi系濺鍍 祀材， 使用該CrTi系濺鍍靶材進行濺鍍，而形成前述基底膜 〇 9.如申請專利範圍第8項之方法，其更包含在前述 熱成形後，於前述濺鍍之前，將前述靶材自成形溫度以 144〜36000 °C/hr的冷卻速度冷卻。 -14- 201221674 四、指定代表圖： (一） 本案指定代表圖為：無。 (二） 本代表圖之元件符號簡單說明：無 201221674 五、本案若有化學式時，請揭示最能顯示發明特徵的化學 式：無201221674 VII. Patent application scope: 1. A CrTi-based alloy containing 35 to 65 atom% of Ti, the balance being CrTi-based alloy composed of Cr and inevitable impurities, and the CrTi-based alloy having 0.50 or less The intensity ratio of the X-ray diffraction intensity [I ( Cr2Ti )] of Cr2Ti ( 3 1 1 ) to the X-ray diffraction intensity of the Cr ( 1 10 ) [1 (c〇) [I ( Cr2Ti) /1 ( Cr )] 2 · The C rT i alloy as in the first paragraph of the patent application is composed of only 3 5 〜 to 65 atom% of Ti, the remainder of Cr and inevitable impurities 〇 • ' 3· a CrTi-based sputtering target which contains 35 to 65 atom% of a sputtering target composed of Cr and an inevitable impurity, and the sputtering target has a Cr2Ti of 0.50 or less ( 311) intensity ratio of X-ray diffraction intensity [I (Cr2Ti)] to Cr (1 10 ) X-ray diffraction intensity [1 (Cr)] [I (Cr2Ti) /1 (Cr)]. The target for CrTi sputtering according to item 3 of the patent application is composed of ϋ 丨堇 35 35 to 65 atom% of Ti, the remaining part of Cr, and inevitable impurities. 5) A perpendicular magnetic recording medium having a base film formed by sputtering using a CrTi-based sputtering target as disclosed in Patent Application No. 3 or 4. 6. A method, such as application A method for producing a target for a β CfTi-based alloy or a CrTi-based sputtering according to any one of the first to fourth aspects of the patent, wherein the method comprises the following steps: preparing a raw material powder having a total composition of the alloy; The raw material powder is thermoformed at 00 to 1100 ton. -13- 201221674 7. The method of claim 6, which further comprises: after the aforementioned thermoforming, the shaped body is formed at a temperature of 14 to 36 〇〇 (rc) The cooling rate of /hr is cooled. 8 · A method of manufacturing a perpendicular magnetic recording medium according to claim 5 of the patent application's method comprises the following steps: preparing a raw material powder having the entire composition of the base film The raw material powder is 800 to 1100. (The film is formed into a CrTi-based sputtering material by thermoforming, and the CrTi-based sputtering target is used for sputtering to form the base film 〇9. Method of Further, after the hot forming, the target is cooled from the forming temperature by a cooling rate of 144 to 36000 ° C / hr before the sputtering. -14- 201221674 IV. Designated representative figure: (1) Representative of the case Pictured: None. (2) Simple description of the symbol of the representative figure: None 201221674 V. If there is a chemical formula in this case, please disclose the chemical formula that best shows the characteristics of the invention: none
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