TWI512113B - An alloy for a seed layer of a magnetic recording medium, and a sputtering target - Google Patents
An alloy for a seed layer of a magnetic recording medium, and a sputtering target Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
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- C22C38/008—Ferrous alloys, e.g. steel alloys containing tin
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
- C22C38/105—Ferrous alloys, e.g. steel alloys containing cobalt containing Co and Ni
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- 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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- 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
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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
- G11B5/62—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
- G11B5/7368—Non-polymeric layer under the lowermost magnetic recording layer
- G11B5/7379—Seed layer, e.g. at least one non-magnetic layer is specifically adapted as a seed or seeding layer
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
- H01F41/18—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates by cathode sputtering
- H01F41/183—Sputtering targets therefor
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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
- G11B5/851—Coating a support with a magnetic layer by sputtering
Description
本發明係主張基於2010年11月22日申請之日本國專利申請號2010-259713號及2011年4月21日申請之日本國專利申請號2011-94594號之優先權者，該等全體揭示內容藉由參考而併入本發明說明書。The present invention claims the priority of Japanese Patent Application No. 2010-259713, filed on Nov. 22, 2010, and Japanese Patent Application No. 2011-94594, filed on Apr. 21, 2011. The description of the invention is incorporated by reference.
本發明係有關作為垂直磁性記錄媒體中之種子層來使用之Ni-Fe-Co系磁性記錄媒體之種子層用合金及濺鍍靶材者。The present invention relates to a seed layer alloy and a sputtering target for a Ni-Fe-Co-based magnetic recording medium used as a seed layer in a perpendicular magnetic recording medium.
近幾年來，由於垂直磁性記錄之顯著進步、驅動器(drive)之大容量化，使磁性記錄媒體朝高記錄密度化進展。例如，藉由以往即已普及之面內磁性記錄媒體可進一步實現高記錄密度之垂直記錄方式已實用化。此處，所謂垂直磁性記錄方式意指易磁化軸相對於垂直磁性記錄媒體之磁性膜中之媒體面，於垂直方向定向之方式形成者，係適於高密度記錄之方法。In recent years, magnetic recording media have progressed toward high recording densities due to significant advances in perpendicular magnetic recording and a large capacity of a drive. For example, a vertical recording method in which a high recording density can be further realized by an in-plane magnetic recording medium which has been widely used in the past has been put into practical use. Here, the perpendicular magnetic recording method means a method in which the easy magnetization axis is formed in a vertical direction with respect to a medium surface in a magnetic film of a perpendicular magnetic recording medium, and is suitable for a method of high-density recording.
於垂直磁性記錄方式中，已開發具有記錄密度經提高之磁性記錄膜層與軟磁性膜層之記錄媒體，於此種媒體構造，已開發出於軟磁性層與磁性記錄層之間製膜有種子層或底層膜層之記錄媒體。垂直磁性記錄方式用之種子層提案有如例如日本特開2009-155722號公報(專利文獻1)所揭示般之Ni-W系合金。In the perpendicular magnetic recording method, a recording medium having a magnetic recording film layer and a soft magnetic film layer having an improved recording density has been developed. In such a media structure, a film between a soft magnetic layer and a magnetic recording layer has been developed. Recording medium of the seed layer or the underlying film layer. A Ni-W-based alloy as disclosed in Japanese Laid-Open Patent Publication No. 2009-155722 (Patent Document 1) is proposed.
該專利文獻1中記載之Ni-W系合金並未添加具有磁性之VIII族，而係添加非磁性元素之IVa族(Ti、Zr、Hf)、Va族(V、Nb、Ta)、VIa族(Cr、Mo、W)、VIIa族(Mn、Tc、Re)、IIIb族(B、Al、Ga、In、Tl)、IVb族(C、Si、Ge、Sn、Pb)，結果成為非磁性。此處種子層所要求之特性之一，如其名所示，係為了控制在種子層上形成之層之定向性，使記錄磁性資訊之磁性膜之易磁化軸相對於媒體面垂直地定向，故種子層本身具有單獨之fcc構造，而且與媒體面平行之面係定向於(111)面。且，為了提高記錄密度而有必要使磁性膜之結晶粒度儘可能小，因此期望比種子層之結晶粒度更小。The Ni-W alloy described in Patent Document 1 is not added with a magnetic Group VIII, but is added with a non-magnetic element of Group IVa (Ti, Zr, Hf), Group Va (V, Nb, Ta), and Group VIa. (Cr, Mo, W), Group VIIa (Mn, Tc, Re), Group IIIb (B, Al, Ga, In, Tl), Group IVb (C, Si, Ge, Sn, Pb), resulting in non-magnetic . Here, one of the characteristics required for the seed layer, as the name suggests, is to control the orientation of the layer formed on the seed layer so that the easy magnetization axis of the magnetic film recording the magnetic information is oriented perpendicularly to the media surface, The seed layer itself has a separate fcc configuration, and the face parallel to the media face is oriented at the (111) face. Further, in order to increase the recording density, it is necessary to make the crystal grain size of the magnetic film as small as possible, and therefore it is desirable to have a smaller crystal grain size than the seed layer.
另一方面，近幾年來，作為改善硬碟驅動器之磁性記錄特性之一方法，已對使種子層具有磁性之方法進行探討。然而，如上述，於專利文獻1中記載之種子層用合金為非磁性，尚無法稱為適合作為具有磁性之種子層用合金。因此要求開發出具備如上述之作為種子層用合金所要求之特性同時具有磁性之種子層用合金。又，至於軟磁性層與種子層之較大差異，於軟磁性層要求有用以減低雜訊之非晶型，但種子層則要求有控制在種子層上形成之層之定向的作用，而要求具有與非晶質的非晶型相反的高結晶性。On the other hand, in recent years, as a method of improving the magnetic recording characteristics of a hard disk drive, a method of making the seed layer magnetic is discussed. However, as described above, the alloy for seed layer described in Patent Document 1 is non-magnetic, and it cannot be said as an alloy suitable for a seed layer having magnetic properties. Therefore, it has been demanded to develop an alloy for a seed layer having the properties required for the alloy for a seed layer as described above and having magnetic properties. Moreover, as for the large difference between the soft magnetic layer and the seed layer, an amorphous type which is useful for reducing noise is required in the soft magnetic layer, but the seed layer requires the effect of controlling the orientation of the layer formed on the seed layer, and requires It has high crystallinity opposite to amorphous amorphous type.
本發明人等如今發現藉由添加具有磁性之VIII族元素的Fe或Co而使種子層具有磁性，且藉由降低(111)面方向之矯頑磁力(coercivity)可提高磁導率。The present inventors have now found that the seed layer is made magnetic by adding Fe or Co having a magnetic Group VIII element, and the magnetic permeability can be improved by lowering the coercivity in the (111) plane direction.
因此，本發明之目的係提供使在軟磁性底層膜(SUL)之上之Ni系中間層具有磁性，且可提高磁導率之磁性記錄媒體之種子層用合金及使用其之濺鍍靶材。Accordingly, an object of the present invention is to provide an alloy for a seed layer of a magnetic recording medium which has magnetic properties on a Ni-based intermediate layer over a soft magnetic underlayer film (SUL) and which can improve magnetic permeability, and a sputtering target using the same .
依據本發明之一樣態，係提供一種合金，其係磁性記錄媒體之種子層用合金，其中含有自W、Mo、Ta、Cr、V及Nb所成之組群選出之一種或兩種以上之M1元素佔前述合金之2~20 at%，自Al、Ga、In、Si、Ge、Sn、Zr、Ti、Hf、B、Cu、P、C及Ru所成之組群選出之一種或兩種以上之M2元素佔前述合金之0~10 at%，其餘為Ni、Fe及Co，以相對於Ni+Fe+Co之總量之at%計，為Ni：Fe：Co=98~20：0~50：0~60及Fe+Co≧1.5之比例。According to the same aspect of the present invention, there is provided an alloy which is an alloy for a seed layer of a magnetic recording medium, which comprises one or more selected from the group consisting of W, Mo, Ta, Cr, V and Nb. The M1 element accounts for 2 to 20 at% of the foregoing alloy, and one or two selected from the group consisting of Al, Ga, In, Si, Ge, Sn, Zr, Ti, Hf, B, Cu, P, C, and Ru The above M2 elements account for 0~10 at% of the above alloy, and the rest are Ni, Fe and Co, and are Ni:Fe:Co=98~20 with respect to at% of the total amount of Ni+Fe+Co: 0~50: 0~60 and the ratio of Fe+Co≧1.5.
依據本發明另一樣態係提供一種合金，其係磁性記錄媒體之種子層用合金，其中含有自W、Mo、Ta、Cr、V及Nb所成之組群選出之一種或兩種以上之M1元素佔前述合金之2~20 at%，自Al、Ga、In、Si、Ge、Sn、Zr、Ti、Hf、B、Cu、P、C及Ru所成之組群選出之一種或兩種以上之M2元素佔前述合金之0~10 at%，其餘為Ni、Fe及Co，以相對於Ni+Fe+Co之總量之at%計，為Ni：Fe：Co=98~20：2~50：0~60之比例。According to another aspect of the present invention, there is provided an alloy which is an alloy for a seed layer of a magnetic recording medium, which comprises one or more selected from the group consisting of W, Mo, Ta, Cr, V and Nb. The element accounts for 2 to 20 at% of the foregoing alloy, and one or two selected from the group consisting of Al, Ga, In, Si, Ge, Sn, Zr, Ti, Hf, B, Cu, P, C, and Ru The above M2 element accounts for 0~10 at% of the above alloy, and the rest are Ni, Fe and Co, and is Ni:Fe:Co=98~20:2 with respect to at% of the total amount of Ni+Fe+Co. ~50:0~60 ratio.
依據本發明另一樣態係提供一種濺鍍靶材，其係以上述合金構成。According to another aspect of the present invention, there is provided a sputtering target which is composed of the above alloy.
依據本發明另一樣態係提供一種磁性記錄媒體，其係具備以上述合金構成之種子層。According to another aspect of the present invention, a magnetic recording medium comprising a seed layer made of the above alloy is provided.
以下具體說明本發明。只要無特別明示，則本說明書中之「%」意指at%。The invention is specifically described below. Unless otherwise stated, "%" in this specification means at%.
本發明之磁性記錄媒體之種子層用合金含有(comprising)自W、Mo、Ta、Cr、V及Nb所成之組群選出之一種或兩種以上之M1元素佔合金之2~20 at%，自Al、Ga、In、Si、Ge、Sn、Zr、Ti、Hf、B、Cu、P、C及Ru所成之組群選出之一種或兩種以上之M2元素佔合金之0~10 at%，其餘為Ni、Fe及Co之至少兩種，較好實質上由該等元素及不可避免雜質組成(consisting essentially of)，更好為由該等元素及不可避免雜質組成(consisting of)。但，Ni、Fe及Co之各量相對於Ni+Fe+Co之總量之at%計，為(i)Ni：Fe：Co=98~20：0~50：0~60及Fe+Co≧1.5之比例，或(ii)Ni：Fe：Co=98~20：2~50：0~60之比例。The seed layer of the magnetic recording medium of the present invention is made of an alloy containing one or more kinds of M1 elements selected from the group consisting of W, Mo, Ta, Cr, V and Nb, which accounts for 2 to 20 at% of the alloy. One or more kinds of M2 elements selected from the group consisting of Al, Ga, In, Si, Ge, Sn, Zr, Ti, Hf, B, Cu, P, C, and Ru account for 0 to 10 of the alloy. At%, the balance being at least two of Ni, Fe and Co, preferably consisting essentially of the elements and the unavoidable impurities, more preferably consisting of the elements and the unavoidable impurities (consisting of) . However, the respective amounts of Ni, Fe, and Co are (i) Ni:Fe:Co=98~20:0~50:0-60 and Fe+Co with respect to at% of the total amount of Ni+Fe+Co. The ratio of ≧1.5, or (ii) the ratio of Ni:Fe:Co=98~20:2~50:0~60.
本發明之合金中，Ni、Fe及Co之比例以Ni：Fe：Co=α：β：γ表示時，Ni之原子比α為98(更嚴格為98.5)~20，較好為98(更嚴格為98.5)~60。α超過98.5時，β+γ成為未達1.5而使矯頑磁力變高，α未達20時，與上述同樣矯頑磁力亦變高。In the alloy of the present invention, when the ratio of Ni, Fe and Co is represented by Ni:Fe:Co=α:β:γ, the atomic ratio α of Ni is 98 (more stringently 98.5) to 20, preferably 98 (more). Strictly 98.5)~60. When α exceeds 98.5, β+γ becomes less than 1.5 and the coercive force becomes high. When α is less than 20, the coercive force is also increased as described above.
Fe為降低矯頑磁力之元素，且亦為改善膜定向性之元素，於設為Ni：Fe：Co=α：β：γ時，Fe之原子比β為0~50，較好為2~50%，更好為10~40。β超過50時，矯頑磁力變高。Fe is an element which lowers the coercive force and is also an element which improves the film orientation. When Ni:Fe:Co=α:β:γ, the atomic ratio of Fe is 0 to 50, preferably 2~. 50%, better 10~40. When β exceeds 50, the coercive force becomes high.
Co為減低(111)方向之矯頑磁力之元素，於設為Ni：Fe：Co=α：β：γ時，Co之原子比γ為0~60，較好為40以下。γ超過60時，矯頑磁力變高。Co is an element which reduces the coercive force in the (111) direction. When Ni:Fe:Co=α:β:γ, the atomic ratio γ of Co is 0 to 60, preferably 40 or less. When γ exceeds 60, the coercive force becomes high.
本發明之合金，含有合金全體之2~20 at%，較好5~15at%之自W、Mo、Ta、Cr、V及Nb所成之組群選出之一種或兩種以上之M1元素。該M1元素為具有高熔點之bcc系金屬，藉由以本發明規定之成分範圍添加於fcc的合金系中，其機制雖尚不明確，但係可改善種子層所要求之對(111)面之定向性且使結晶粒微細化之元素。因此，M1元素量未達2%時其效果不充分，且超過20%時，化合物會析出或非晶型化。由於作為種子層用合金要求為fcc單相，故該M1元素量之範圍設為上述。The alloy of the present invention contains 2 to 20 at%, preferably 5 to 15 at% of the total of one or more M1 elements selected from the group consisting of W, Mo, Ta, Cr, V and Nb. The M1 element is a bcc-based metal having a high melting point, and is added to the fcc alloy system by the range of the components specified in the present invention. Although the mechanism is not clear, the desired (111) surface of the seed layer can be improved. An element that is oriented and refines crystal grains. Therefore, when the amount of the M1 element is less than 2%, the effect is insufficient, and when it exceeds 20%, the compound is precipitated or amorphous. Since the alloy for the seed layer is required to be fcc single phase, the range of the amount of the M1 element is set as described above.
其中尤以W及Mo提高(111)面之定向效果較高，故較好添加W及Mo之一種或兩種，亦可添加Cr、Ta、V及Nb之任一種或兩種以上。其理由係由於藉由Ni與高熔點bcc金屬之組合，Mo或W之熔點比Cr高而有利之故。且，Ta、V或Nb之添加，相比於W及Mo，亦具有提高非晶型性之作用，對種子層所要求之fcc相形成不利。Cr以較期望之超過5%添加時，就定向性方面為有利。In particular, W and Mo have a higher orientation effect on the (111) plane. Therefore, one or two of W and Mo are preferably added, and any one or two or more of Cr, Ta, V, and Nb may be added. The reason for this is that the combination of Ni and a high melting point bcc metal makes it advantageous for the melting point of Mo or W to be higher than Cr. Further, the addition of Ta, V or Nb has an effect of improving the amorphous form as compared with W and Mo, and is disadvantageous for the formation of the fcc phase required for the seed layer. When Cr is added more than 5% as desired, it is advantageous in terms of orientation.
本發明之合金，係含有合金之0~10at%，較好1~10at%，更好5%之自Al、Ga、In、Si、Ge、Sn、Zr、Ti、Hf、B、Cu、P、C及Ru所成之組群選出之一種或兩種以上之M2元素作為任意元素。該M2元素為使(111)面定向之元素，且為使結晶粒微細化之元素。然而，M2元素量超過10%時會產生化合物、或會非晶型化。又，M1+M2之合計量較好為25at%以下，進而更好為20at%以下。The alloy of the present invention contains 0 to 10 at%, preferably 1 to 10 at%, more preferably 5% of the alloy from Al, Ga, In, Si, Ge, Sn, Zr, Ti, Hf, B, Cu, P. One or two or more M2 elements selected from the group formed by C and Ru are used as arbitrary elements. The M2 element is an element that orients the (111) plane, and is an element that refines crystal grains. However, when the amount of the M2 element exceeds 10%, a compound may be produced or may be amorphous. Further, the total amount of M1 + M2 is preferably 25 at% or less, and more preferably 20 at% or less.
以下利用實施例對本發明具體說明。The invention will be specifically described below by way of examples.
通常，垂直磁性記錄媒體中之種子層係以與其成分相同成分之濺鍍靶材進行濺鍍，在玻璃基板上成膜而得。此處使利用濺鍍而成膜之薄膜急速冷卻。本發明之供試材料係使用以單輥式急冷裝置製作之急冷薄帶。其係簡易地藉由液體急冷薄帶而評價實際上由濺鍍而急冷且成膜之薄膜中因成分對諸特性之影響者。Generally, a seed layer in a perpendicular magnetic recording medium is sputtered with a sputtering target having the same composition as that of the composition, and is formed by film formation on a glass substrate. Here, the film formed by sputtering is rapidly cooled. The test material of the present invention uses a quenched ribbon produced by a single roll quenching device. It is easy to evaluate the influence of the composition on the characteristics of the film which is actually quenched by sputtering and is formed into a film by the liquid quenching ribbon.
依表1之成分秤量之原料30g於直徑10mm、長度40mm程度之水冷銅鑄模具中減壓，於Ar中進行電弧溶解，作為急冷薄帶之溶解母材。急冷薄帶之製作條件為以單輥方式於直徑15mm之石英罐中，設定該溶解母材，熔體金屬出料噴嘴直徑設為1mm，環境氣壓61kPa，噴霧差壓69kPa，銅輥(直徑300mm)之旋轉數3000rpm，銅輥與熔體金屬出料噴嘴之間距為0.3mm進行熔體金屬出料。出料溫度設為恰使各溶解母材熔融落下之後。將如此製作之急冷薄帶作為供試材，評價下述項目。30 g of the raw material weighed according to the composition of Table 1 was decompressed in a water-cooled copper casting mold having a diameter of 10 mm and a length of 40 mm, and was subjected to arc dissolution in Ar to serve as a dissolved base material for the quenched ribbon. The production conditions of the quenched ribbon were set in a single roll on a quartz tank having a diameter of 15 mm, and the dissolved base material was set. The diameter of the melt metal discharge nozzle was set to 1 mm, the ambient pressure was 61 kPa, the spray differential pressure was 69 kPa, and the copper roll (diameter 300 mm). The rotation number was 3000 rpm, and the melt metal discharge was performed at a distance of 0.3 mm between the copper roll and the melt metal discharge nozzle. The discharge temperature was set just after the molten base material was melted and dropped. The quenched ribbon thus produced was used as a test material, and the following items were evaluated.
關於振動試料型之矯頑磁力計，以雙面膠帶將急冷帶張貼於試料台上，以初期施加磁場144kA/m測定急冷薄帶之矯頑磁力。矯頑磁力為300A/m以下記為○，超過300A/m、500A/m以下記為△，超過500A/m者記為×。Regarding the coercive force meter of the vibration sample type, the quenching tape was attached to the sample stage with a double-sided tape, and the coercive force of the quenched ribbon was measured by an initial application magnetic field of 144 kA/m. When the coercive force is 300 A/m or less, it is represented by ○, and when it exceeds 300 A/m and 500 A/m or less, it is represented by Δ, and when it exceeds 500 A/m, it is represented by ×.
於VSM裝置(振動試料型磁力計)中以施加磁場1200 kA/m，測定急冷薄帶之飽和磁通密度。供試材之重量為15mg左右，於0.2T以上評價為○，未達0.2T評價為×。The saturation magnetic flux density of the quenched ribbon was measured in a VSM apparatus (vibration sample type magnetometer) by applying a magnetic field of 1200 kA/m. The weight of the test material was about 15 mg, and it was evaluated as ○ at 0.2 T or more, and was evaluated as × at less than 0.2 T.
利用濺鍍成膜之種子層為fcc構造。種子層藉由急冷而使(200)定向。通常若隨機定向，則(111)面與(200)面之X射線繞射強度係I(200)高於I(111)。因此，以下述方法評價急冷薄帶之(111)面之定向性。The seed layer formed by sputtering is an fcc structure. The seed layer is oriented (200) by quenching. Generally, if randomly oriented, the X-ray diffraction intensity I (200) of the (111) plane and the (200) plane is higher than I (111). Therefore, the directivity of the (111) plane of the quenched ribbon was evaluated by the following method.
以雙面膠帶於玻璃板上貼附供試材，以X射線繞射裝置獲得繞射圖型。此時，以使測定面成為急冷薄帶之銅輥接觸面之方式貼附供試材。以Cu-α線為X射線源、掃描速度4°/分鐘進行測定。於該折射圖型之(111)面繞射之X射線強度I(111)與(200)面之X射線強度I(200)之強度比I(111)/I(200)為未達0.7者記為×，0.7以上者記為○。且產生化合物者、非晶型化者記為×。A test piece was attached to the glass plate with a double-sided tape, and a diffraction pattern was obtained by an X-ray diffraction device. At this time, the test piece was attached so that the measurement surface became the contact surface of the copper roll of the quenched ribbon. The Cu-α line was used as an X-ray source and the scanning speed was 4°/min. The intensity ratio I(111)/I(200) of the X-ray intensity I(111) and the (200) plane X-ray intensity I(200) of the (111) plane of the refractive pattern is less than 0.7. It is written as ×, and 0.7 or more is recorded as ○. The person who produced the compound and the amorphous type were recorded as ×.
於急冷薄帶之剖面微組織像之輥方向，依據JIS G0551「鋼‧結晶粒度之顯微鏡試驗方法」測定急冷薄帶之結晶粒徑。P/Lt為1.0以上記為○，0.5以上、未達1.0記為△，未達0.5記為×。The crystal grain size of the quenched ribbon was measured in accordance with JIS G0551 "Microscope test method for steel and crystal grain size" in the direction of the roll of the microstructure of the quenched ribbon. When P/Lt is 1.0 or more, it is represented by ○, 0.5 or more, and less than 1.0 is Δ, and less than 0.5 is ×.
[表1][Table 1]
[表2][Table 2]
[表3][table 3]
[表4][Table 4]
[表5][table 5]
[表6][Table 6]
[表7][Table 7]
[表8][Table 8]
如表1~8所示，No.1~95、125~188為本發明例，No.96~124及189~193為比較例，No.194為參考例。As shown in Tables 1 to 8, No. 1 to 95 and 125 to 188 are examples of the invention, Nos. 96 to 124 and 189 to 193 are comparative examples, and No. 194 is a reference example.
又，表1~8所之之成分組成中記載之例如由於No.1係W為2at%，故(Ni2Fe)為100%-2%而係98at%，將該98%設為1時，Ni為(100-2)，Fe為2之比例。且由於不含Co，故其比例相當於0。同樣地，若為No.50，由於W與In計7at%，故(Ni50Fe)係100%-7%而為93at%，將該93at%設為1時，Ni為100-50，Fe為50之比，亦即Ni與Fe以at比計為相同比例，因此，意指平均各為93%的一半之各46.5%者。Further, as described in the component compositions of Tables 1 to 8, for example, since No. 1 is W at 2 at%, (Ni2Fe) is 100% to 2% and is 98 at%, and when 98% is set to 1, Ni is Ni. For (100-2), Fe is a ratio of 2. And since it does not contain Co, its ratio is equivalent to zero. Similarly, in the case of No. 50, since W and In are 7 at%, (Ni50Fe) is 100%-7% and is 93 at%, and when 93 at% is 1, Ni is 100-50, and Fe is 50. The ratio, that is, Ni and Fe are in the same ratio at the ratio of at, and therefore means an average of 46.5% of each of 93%.
比較例No.96由於僅為Ni，故矯頑磁力高，定向性及結晶粒徑均差。比較例No.97由於不含M元素，故定向性及結晶粒徑均差。比較例No.98由於Fe含量高，故矯頑磁力高。比較例No.99由於W含量低且Al含量高，故矯頑磁力稍變高且定向性差。比較例No.100由於W含量高，故矯頑磁力難以測定，且飽和磁通密度及定向性差。In Comparative Example No. 96, since it was only Ni, the coercive force was high, and the orientation and crystal grain size were inferior. In Comparative Example No. 97, since the M element was not contained, the orientation and the crystal grain size were inferior. In Comparative Example No. 98, since the Fe content was high, the coercive force was high. In Comparative Example No. 99, since the W content was low and the Al content was high, the coercive force was slightly increased and the orientation was poor. In Comparative Example No. 100, since the W content was high, the coercive force was difficult to measure, and the saturation magnetic flux density and the directivity were poor.
比較例No.101、102由於W含量低且Zr及B之含量高，故定向性差。比較例No.103由於Ni含量低，Fe含量高，故矯頑磁力變高。比較例No.104由於Ni含量低，Fe含量高，故矯頑磁力變高。比較例No.105由於Cr含量低故矯頑磁力高，定向性及結晶粒徑均差。比較例No.106由於Cr含量高，故所有特性均差。比較例No.107由於Mo含量低，故矯頑磁力高，定向性及結晶粒徑均差。In Comparative Examples Nos. 101 and 102, since the W content was low and the contents of Zr and B were high, the orientation was poor. In Comparative Example No. 103, since the Ni content was low and the Fe content was high, the coercive force was high. In Comparative Example No. 104, since the Ni content was low and the Fe content was high, the coercive force was high. In Comparative Example No. 105, since the Cr content was low, the coercive force was high, and both the orientation and the crystal grain size were inferior. In Comparative Example No. 106, since the Cr content was high, all the characteristics were inferior. In Comparative Example No. 107, since the Mo content was low, the coercive force was high, and the orientation and crystal grain size were inferior.
比較例No.108由於Mo含量高，故所有特性均差。比較例No.109由於Ta含量低，故矯頑磁力高，定向性及結晶粒徑均差。比較例No.110由於Ta含量高，故所有特性均差。比較例No.111由於V含量低，故矯頑磁力高，定向性及結晶粒徑均差。比較例No.112由於V含量高，故所有特性均差。比較例No.113由於Nb含量低，故矯頑磁力高，定向性及結晶粒徑均差。In Comparative Example No. 108, since the Mo content was high, all the characteristics were inferior. In Comparative Example No. 109, since the Ta content was low, the coercive force was high, and the orientation and crystal grain size were inferior. In Comparative Example No. 110, since the Ta content was high, all the characteristics were inferior. In Comparative Example No. 111, since the V content was low, the coercive force was high, and the orientation and crystal grain size were inferior. In Comparative Example No. 112, since the V content was high, all the characteristics were inferior. In Comparative Example No. 113, since the Nb content was low, the coercive force was high, and the orientation and crystal grain size were inferior.
比較例No.114由於Nb含量高，故所有特性均差。比較例No.115由於Ca含量高，故定向性及結晶粒徑差。比較例No.116由於In含量高，故定向性及結晶粒徑差。比較例No.117由於Si含量高，故定向性及結晶粒徑差。比較例No.118由於Ge含量高，故定向性及結晶粒徑差。比較例No.119由於Ti含量高，故定向性及結晶粒徑差。In Comparative Example No. 114, since the Nb content was high, all the characteristics were inferior. In Comparative Example No. 115, since the Ca content was high, the orientation and crystal grain size were inferior. In Comparative Example No. 116, since the In content was high, the orientation and crystal grain size were inferior. In Comparative Example No. 117, since the Si content was high, the orientation and the crystal grain size were inferior. In Comparative Example No. 118, since the Ge content was high, the orientation and crystal grain size were inferior. In Comparative Example No. 119, since the Ti content was high, the orientation and crystal grain size were inferior.
比較例No.120由於Hf含量高，故定向性及結晶粒徑差。比較例No.121由於Cu含量高，故定向性及結晶粒徑差。比較例No.122由於P含量高，故定向性及結晶粒徑差。比較例No.123由於C含量高，故定向性及結晶粒徑差。比較例No.124由於Ru含量高，故定向性及結晶粒徑差。In Comparative Example No. 120, since the Hf content was high, the orientation and crystal grain size were inferior. In Comparative Example No. 121, since the Cu content was high, the orientation and the crystal grain size were inferior. In Comparative Example No. 122, since the P content was high, the orientation and the crystal grain size were inferior. In Comparative Example No. 123, since the C content was high, the orientation and the crystal grain size were inferior. In Comparative Example No. 124, since the Ru content was high, the orientation and crystal grain size were inferior.
表8之比較例No.189由於Fe+Co之含量低，故矯頑磁力差。比較例No.190由於Fe+Co之含量低，故矯頑磁力差。No.191由於Fe+Co之含量低，故矯頑磁力差。No.192由於Fe+Co之含量低，故矯頑磁力差。No.193由於Fe+Co之含量低，故矯頑磁力差。No.194雖在本發明條件內，但由於Cr添加量為4.9並未超過5，故特性稍差。因此作為參考例。In Comparative Example No. 189 of Table 8, since the content of Fe + Co was low, the coercive force was poor. In Comparative Example No. 190, since the content of Fe + Co was low, the coercive force was poor. No. 191 has a low coercive force due to a low content of Fe + Co. No. 192 has a low coercive force due to a low content of Fe + Co. No. 193 has a low coercive force due to a low content of Fe + Co. Although No. 194 was within the conditions of the present invention, since the amount of addition of Cr was 4.9 and did not exceed 5, the characteristics were slightly inferior. Therefore, as a reference example.
如以上所述，於Ni-Fe-Co-M合金中，藉由限制於一定含量，藉由限制在該區域，發現具有磁性、且(111)方向之磁導率變高，藉由對Ni系種子層賦予磁性而可發揮使磁頭與軟磁性底層膜之距離縮短之優異效果。As described above, in the Ni-Fe-Co-M alloy, by being restricted to a certain content, it is found to have magnetic properties by being restricted in the region, and the magnetic permeability in the (111) direction becomes high by using Ni The seed layer imparts magnetic properties and exhibits an excellent effect of shortening the distance between the magnetic head and the soft magnetic underlayer film.
接著，顯示濺鍍靶材之製造方法之例。將經秤量表1之本發明例No.2、No.10、No.14、No.18、No.25及表2之No.35、No.38、No.43、表3之No.51、No.70、表4之No.79、No.85、No.89、No.95、表5之No.102、No.117、No.118、No.122、表6之No.128、No.135、No.144、表7之No.159、No.170、No.176、表8之No.188、比較例No.190、比較例No.193所示之成分組成者之溶解原料，在減壓Ar氣體環境之耐火物坩堝內經感應加熱熔解後，自坩鍋下部之直徑8mm之噴嘴出料，利用Ar氣體霧化。以該氣體霧化粉末作為原料粉末，填充於碳鋼製之直徑250mm、長度100mm之膠囊內，進行真空脫氣密封。Next, an example of a method of manufacturing a sputtering target will be described. Inventive Example No. 2, No. 10, No. 14, No. 18, No. 25, and Table No. 35, No. 38, No. 43, and No. 51 of Table 3 of the weighing scale 1. No. 70, No. 79 of Table 4, No. 85, No. 89, No. 95, No. 102 of Table 5, No. 117, No. 118, No. 122, No. 128 of Table 6, Dissolved raw materials of components of No. 135, No. 144, No. 159, No. 170, No. 176 of Table 7, No. 188 of Table 8, No. 190 of Comparative Example No. 190, and Comparative Example No. 193 After being melted by induction heating in a refractory crucible of a decompressed Ar gas atmosphere, the nozzle was discharged from a nozzle having a diameter of 8 mm at the lower portion of the crucible, and was atomized by Ar gas. The gas atomized powder was used as a raw material powder, and it was filled in a capsule made of carbon steel and having a diameter of 250 mm and a length of 100 mm, and vacuum degassing and sealing was performed.
上述粉末填充彈，於表1之No.2、No.10、No.14、No.18、No.25、表3之No.51、No.70係以成形溫度1000℃、成形壓力147MPa、成形時間1小時之條件進行HIP成形，於表2之No.35、No.38、No.43、表4之No.79、No.85、No.89、No.95係以成形溫度1100℃、成形壓力147MPa、成形時間3小時之條件進行HIP成形，於表5之No.102、No.117、No.118、No.122、表6之No.128、No.135、No.144、表7之No.159、No.170、No.176、表8之No.188、比較例No.190、比較例No.193係以成形溫度950℃、成形壓力147MPa、成形時間5小時之條件進行HIP成形。該HIP體藉由金屬線切割、旋盤加工、平面研磨，而加工成直徑180mm、厚度7mm之圓盤狀，作為濺鍍靶材。The powder-filled bombs described in No. 2, No. 10, No. 14, No. 18, No. 25, Table No. 51, and No. 70 of Table 1 have a molding temperature of 1000 ° C and a molding pressure of 147 MPa. HIP molding was carried out under the conditions of a molding time of 1 hour, and No. 35, No. 38, No. 43 of Table 2, No. 79, No. 85, No. 89, and No. 95 of Table 4 were formed at a molding temperature of 1100 ° C. HIP molding was carried out under the conditions of a molding pressure of 147 MPa and a molding time of 3 hours, and No. 102, No. 117, No. 118, No. 122, Table 6, No. 128, No. 135, No. 144 of Table 6, No. 159, No. 170, No. 176, Table No. 188, Comparative Example No. 190, and Comparative Example No. 193 of Table 7 were prepared at a molding temperature of 950 ° C, a molding pressure of 147 MPa, and a molding time of 5 hours. Perform HIP forming. The HIP body was processed into a disk shape having a diameter of 180 mm and a thickness of 7 mm by wire cutting, rotary disk processing, or surface polishing, and used as a sputtering target.
使用關於該等27種類之成分組成之濺鍍靶材，在玻璃基板上使濺鍍膜成膜。X射線繞射峰中於本發明例No.2、No.10、No.14、No.18、No.25、No.35、No.38、No.43、No.51、No.70、No.79、No.85、No.89、No.95、No.128、No.135、No.144、No.159、No.170、No.176、No.186均見到良好定向性，而比較例No.102、No.117、No.118、No.122並未見到良好定向性。A sputtered film was formed on the glass substrate by using a sputtering target having a composition of these 27 types. The X-ray diffraction peaks are in the present invention examples No. 2, No. 10, No. 14, No. 18, No. 25, No. 35, No. 38, No. 43, No. 51, No. 70, No. 79, No. 85, No. 89, No. 95, No. 128, No. 135, No. 144, No. 159, No. 170, No. 176, No. 186 all saw good orientation. Comparative Examples No. 102, No. 117, No. 118, and No. 122 did not show good directivity.
又，與急冷薄帶同樣地進行磁特性之測定後，本發明例No.2、No.10、No.14、No.18、No.25、No.35、No.38、No.43、No.51、No.70、No.79、No.85、No.89、No.95、No.128、No.135、No.144、No.159、No.170、No.176、No.186均見到良好之磁特性，而比較例No.189、比較例No.190、比較例No.193並未見到良好磁特性。關於X射線繞射圖型，亦與急冷薄帶進行同樣測定後，與急冷薄帶之評價結果同樣評價為○、△、×。總結以上所述，確認了急冷薄帶之評價結果與使用濺鍍靶材而成膜之濺鍍膜評價為相同之傾向。Further, after measuring the magnetic properties in the same manner as the quenched ribbon, the present invention examples No. 2, No. 10, No. 14, No. 18, No. 25, No. 35, No. 38, No. 43, No. 51, No. 70, No. 79, No. 85, No. 89, No. 95, No. 128, No. 135, No. 144, No. 159, No. 170, No. 176, No. Good magnetic properties were observed in all of 186, and good magnetic properties were not observed in Comparative Example No. 189, Comparative Example No. 190, and Comparative Example No. 193. The X-ray diffraction pattern was also measured in the same manner as in the quenched ribbon, and evaluated as ○, Δ, and × in the same manner as the evaluation results of the quenched ribbon. In summary, it was confirmed that the evaluation result of the quenched ribbon was evaluated to be the same as that of the sputtering film formed by using the sputtering target.
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| CN104651788B (en) * | 2013-11-21 | 2017-03-15 | 安泰科技股份有限公司 | Ni Fe W alloys targets and its manufacture method |
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| US9685184B1 (en) * | 2014-09-25 | 2017-06-20 | WD Media, LLC | NiFeX-based seed layer for magnetic recording media |
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