WO2010007980A1 - Alliages pour couches pelliculaires magnétiques molles dans des supports d’enregistrement magnétiques verticaux, matériaux de cibles de pulvérisation et leur procédé de fabrication - Google Patents
Alliages pour couches pelliculaires magnétiques molles dans des supports d’enregistrement magnétiques verticaux, matériaux de cibles de pulvérisation et leur procédé de fabrication Download PDFInfo
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- WO2010007980A1 WO2010007980A1 PCT/JP2009/062716 JP2009062716W WO2010007980A1 WO 2010007980 A1 WO2010007980 A1 WO 2010007980A1 JP 2009062716 W JP2009062716 W JP 2009062716W WO 2010007980 A1 WO2010007980 A1 WO 2010007980A1
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- sputtering target
- target material
- raw material
- soft magnetic
- powder
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- 239000013077 target material Substances 0.000 title claims abstract description 61
- 238000005477 sputtering target Methods 0.000 title claims abstract description 56
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 39
- 239000000956 alloy Substances 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000000203 mixture Substances 0.000 claims abstract description 54
- 229910052796 boron Inorganic materials 0.000 claims abstract description 13
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 13
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 12
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 11
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 11
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 68
- 239000002994 raw material Substances 0.000 claims description 43
- 238000000034 method Methods 0.000 claims description 29
- 238000000465 moulding Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 5
- 238000007711 solidification Methods 0.000 claims description 3
- 230000008023 solidification Effects 0.000 claims description 3
- -1 and in atomic ratio Substances 0.000 claims description 2
- 230000004907 flux Effects 0.000 abstract description 41
- 230000007797 corrosion Effects 0.000 abstract description 31
- 238000005260 corrosion Methods 0.000 abstract description 31
- 229910052759 nickel Inorganic materials 0.000 abstract description 16
- 229910052742 iron Inorganic materials 0.000 abstract description 9
- 238000001755 magnetron sputter deposition Methods 0.000 abstract description 4
- 229910001004 magnetic alloy Inorganic materials 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 15
- 239000000463 material Substances 0.000 description 15
- 238000011156 evaluation Methods 0.000 description 12
- 238000004544 sputter deposition Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000011812 mixed powder Substances 0.000 description 7
- 239000010409 thin film Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 230000005307 ferromagnetism Effects 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000010791 quenching Methods 0.000 description 4
- 230000000171 quenching effect Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000009689 gas atomisation Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 229910000531 Co alloy Inorganic materials 0.000 description 2
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229910001362 Ta alloys Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 101000993059 Homo sapiens Hereditary hemochromatosis protein Proteins 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001475 halogen functional group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
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- 238000003825 pressing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- 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
- G11B5/64—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent
- G11B5/65—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition
- G11B5/657—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition containing inorganic, non-oxide compound of Si, N, P, B, H or C, e.g. in metal alloy or compound
-
- 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
-
- 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
- C22C1/0433—Nickel- or cobalt-based alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/07—Alloys based on nickel or cobalt based on cobalt
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/04—Amorphous alloys with nickel or cobalt as the major constituent
-
- 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
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2202/00—Physical properties
- C22C2202/02—Magnetic
Definitions
- the present invention relates to a Co—Fe—Ni alloy used for forming a soft magnetic layer film in a perpendicular magnetic recording medium, a sputtering target material using the same, and a method for manufacturing the same.
- the perpendicular magnetic recording method is a method suitable for high recording density, in which the easy magnetization axis is oriented in the perpendicular direction with respect to the medium surface in the magnetic film of the perpendicular magnetic recording medium.
- a two-layer recording medium having a magnetic recording film layer and a soft magnetic film layer with improved recording sensitivity has been developed.
- a CoCrPt—SiO 2 alloy is used for the magnetic recording film layer.
- JP-A-2005-320627 contains Zr: 1 to 10 atomic%, Nb and / or Ta: 1 to 10 atomic%, and the balance is substantially Discloses a method for producing a Co alloy target material made of Co. After the alloy powder is prepared by rapid solidification of a molten Co alloy, the alloy powder having a powder particle size of 500 ⁇ m or less is pressure-sintered to obtain CoZrNb. / Ta alloy target material has been proposed. The soft magnetic film layer of this perpendicular magnetic recording medium is required to have high saturation magnetic flux density and high amorphousness.
- Patent Document 2 Japanese Patent Application Laid-Open No. 2007-284741
- Fe A soft magnetic target material has been proposed in which the Co at ratio is 100: 0 to 20:80 and one or two of Al or Cr are contained in an amount of 0.2 to 5 at%.
- amorphous property means the ease of becoming amorphous when the alloy is rapidly solidified or formed by sputtering, and the corrosion resistance is a level that does not occur in a normal environment where electronic components are used. Say the weather resistance.
- the sputtering target material for forming the alloy also has a high saturation magnetic flux density, resulting in a magnetron.
- the PTF value is lowered, which affects the deposition rate during sputtering and the stability of the deposition process.
- the PTF value is a ratio of magnetic lines of force from the magnet arranged on the back surface of the sputtering target material leaking to the surface of the sputtering target material during magnetron sputtering, and is related to the sputtering efficiency and the yield of the formed thin film. It is an influencing factor.
- a Co—Fe—Ni alloy having a predetermined composition has a high saturation magnetic flux density, a high amorphous property, and a high corrosion resistance.
- the present inventors have used a predetermined mixed powder as a raw material powder of a sputtering target material for forming a film of this alloy, thereby producing a uniform internal quality of the same composition manufactured with a single composition raw material powder. It has been found that the PTF value can be significantly improved as compared with the sputtering target material having the above.
- the object of the present invention is to provide a soft magnetic alloy for perpendicular magnetic recording media excellent in saturation magnetic flux density, amorphousness and corrosion resistance, and efficiently used during magnetron sputtering while having this excellent alloy composition as a whole.
- An object of the present invention is to provide a sputtering target material having a high PTF value.
- Fe 10 to 45%, Ni: 1-25%, One or more of Zr, Hf, Nb, Ta, B: 5 to 10% in total amount of Zr + Hf + Nb + Ta + B / 2 (B is 0% or more and 7% or less), One or two of Al and Cr: 0 to 5% in the total amount of Al + Cr, and the balance Co and unavoidable impurities: 37% or more, and in atomic ratio, Fe / (Co + Fe + Ni): 0.10 to 0.50, and Ni / (Co + Fe + Ni): 0.01 to 0.25
- An alloy for a soft magnetic film layer in a perpendicular magnetic recording medium that satisfies the above is provided.
- a method for producing a sputtering target material for a soft magnetic film layer in a perpendicular magnetic recording medium (A) a step of preparing two or more kinds of raw material powders having different compositions so that their total composition constitutes the soft magnetic film layer alloy according to claim 1, wherein at least one of the raw material powders Different types of raw material powder Atomic% Ni: 20 to 34%, Co: 0-6% One or more of Zr, Hf, Nb, Ta, B: 3 to 12% in total amount of Zr + Hf + Nb + Ta + B / 2 (B is 0% or more and 7% or less), One or two of Al and Cr: Al + Cr: 0 to 5%, and the balance Fe and inevitable impurities, and in atomic ratio, Ni / (Fe + Ni): 0.27 to 0.35 Which satisfies
- a method comprising the steps of (b) mixing the two or more raw material powders to obtain a mixture, and (c
- a sputtering target material produced by the above method is provided.
- the alloy for soft magnetic film layer in the perpendicular magnetic recording medium according to the present invention is atomic%, Fe: 10 to 45%, Ni: 1 to 25%, Zr, Hf, Nb. , Ta, B, one or more: 5 to 10% in total amount of Zr + Hf + Nb + Ta + B / 2 (B is 0% or more and 7% or less), one or two types of Al, Cr: total amount of Al + Cr 0 to 5%, and the balance Co and unavoidable impurities: 37% or more, preferably only these constituent elements.
- the alloy satisfies Fe / (Co + Fe + Ni): 0.10 to 0.50 and Ni / (Co + Fe + Ni): 0.01 to 0.25 in atomic ratio.
- Fe / (Co + Fe + Ni) 0.10 to 0.50
- Ni / (Co + Fe + Ni) 0.01 to 0.25 in atomic ratio.
- Fe is an element having ferromagnetism together with Co and Ni. On the other hand, it is an element that degrades the corrosion resistance compared to Co and Ni. However, when the Fe content is less than 10%, the saturation magnetic flux density is small, and when it exceeds 45%, the corrosion resistance deteriorates. Therefore, the Fe content in the alloy is 10 to 45%, preferably 20 to 40%.
- Ni is an element having ferromagnetism together with Co and Fe, but has a lower saturation magnetic flux density than Co and Fe.
- the corrosion resistance is much higher than Fe and slightly better than Co.
- the Ni content in the alloy is 1 to 25%, preferably 10 to 22%.
- Zr, Hf, Nb, Ta, and B are elements that have an eutectic phase diagram with respect to Co and Fe and form an amorphous phase.
- the concentration of these elements in the eutectic composition is 8 to 13% excluding B, and B is less than 20%. This is almost similar to Ni. Therefore, the total amount of Zr, Hf, Nb, Ta, and B / 2 can be handled. However, if Zr + Hf + Nb + Ta + B / 2 is less than 5%, the amorphous property is not sufficient, and if it exceeds 10%, the amorphous property is saturated and the saturation magnetic flux density is lowered.
- the total amount of Zr + Hf + Nb + Ta + B / 2 in the alloy is 5 to 10%, preferably 7.0 to 9.5. Moreover, since corrosion resistance will deteriorate when B exceeds 7%, B content in an alloy shall be 7% or less.
- both Al and Cr are elements that improve corrosion resistance, they are added in a total amount of Al + Cr of 5% or less. However, if the total amount exceeds 5%, the saturation magnetic flux density decreases greatly, so the upper limit was made 5%.
- Fe is an element having ferromagnetism together with Co and Ni. On the other hand, it is an element that degrades the corrosion resistance compared to Co and Ni.
- the atomic ratio of Fe / (Co + Fe + Ni) is set to 0.10 to 0.50%, preferably 0.23 to 0.43%.
- Ni is an element having ferromagnetism together with Co and Fe, but has a lower saturation magnetic flux density than Co and Fe.
- the corrosion resistance is much higher than Fe and slightly better than Co.
- the atomic ratio of Ni / (Co + Fe + Ni) is set to 0.01 to 0.25, preferably 0.11 to 0.17.
- the remaining Co is required to be 37% or more, and if it is less than 37%, the corrosion resistance is deteriorated.
- the manufacturing method of the sputtering target material for the soft magnetic film layer in the perpendicular magnetic recording medium according to the present invention comprises (a) two or more kinds of raw material powders having different compositions, the total composition of which is A step of preparing the alloy for the film layer, (b) a step of mixing the two or more kinds of raw material powders to obtain a mixture, and (c) a step of solidifying and forming the mixture to form a sputtering target material. Comprising.
- the soft magnetic film layer alloy is an excellent alloy having high saturation magnetic flux density, high amorphousness, and high corrosion resistance.
- the PTF value will be low, so the film formation speed will be low, and film formation will be reduced. The stability of will also be low.
- the raw material powder of at least one composition is atomic%, Ni: 20 to 34%, Co: 0 to 6%, Zr, Hf, Nb. , Ta, B or more: 3 to 12% in total amount of Zr + Hf + Nb + Ta + B / 2 (B is 0% or more and 7% or less), Al or Cr: 1 or 2 types: Al + Cr: 0 to 5% and the balance Fe and unavoidable impurities and satisfy the atomic ratio of Ni / (Fe + Ni): 0.27 to 0.35. By doing so, the saturation magnetic flux density can be made extremely low.
- An alloy powder in which Ni and Ni / (Fe + Ni) fall within the above range has a very low saturation magnetic flux density.
- this alloy powder as at least a part of the raw material powder and solidifying and forming a sputtering target material, Compared with a uniform sputtering target material having the same composition, the PTF value can be remarkably improved.
- Ni and Ni / (Fe + Ni) are out of the above range, the saturation magnetic flux density of the alloy powder becomes high, and the effect of improving the PTF value is reduced. Therefore, Ni is set to 20 to 34% and Ni / (Fe + Ni) is set to 0.27 to 0.35.
- the powder having Ni: 20 to 34%, Ni / (Fe + Ni): 0.27 to 0.35, Co: 0 to 6%, Zr + Hf + Nb + Ta + B / 2: 3 to 12% is the balance Fe
- the composition of the raw material powder (hereinafter referred to as the remaining composition) becomes Co-rich. Therefore, the remaining Fe raw material powder (low corrosion resistance) and Co-rich raw material powder (high corrosion resistance) are mixed and solidified to form a kind of local battery between the two powders. It becomes easy to do.
- Al + Cr is added to the remaining Fe powder having at least Ni: 20 to 34%, Ni / (Fe + Ni): 0.27 to 0.35, Co: 0 to 6%, Zr + Hf + Nb + Ta + B / 2: 3 to 12%.
- Ni 20 to 34%
- Ni / (Fe + Ni) 0.27 to 0.35
- Co 0 to 6%
- Zr + Hf + Nb + Ta + B / 2 3 to 12%.
- Solidification molding is preferably performed by an upset method in which molding is performed in a few seconds in the hot state, thereby suppressing the diffusion of elements in the raw material powder and maintaining the original low saturation magnetic flux density after the molding. .
- the mixed powder is solidified and formed for several hours with heat as in the HIP method or the hot press method, atomic diffusion occurs between different types of powder, and a diffusion layer having elements of both powder compositions is generated.
- the generated diffusion layer has a high saturation magnetic flux density, which hinders a sufficient PTF improvement effect.
- a preferable temperature in the upset method is 900 to 1250 ° C., more preferably 930 to 1070 ° C., and a preferable pressure is 400 to 1400 MPa, more preferably 500 to 900 MPa.
- the pressing time is not limited, but 1 to 10 seconds is preferable.
- a soft magnetic film layer in a perpendicular magnetic recording medium can be formed on a glass substrate or the like by sputtering a sputtering target material having the same component as that component.
- the thin film formed by sputtering is rapidly cooled.
- the quenching thin strip produced with the single roll type liquid quenching apparatus is used as a test material of an Example and a comparative example. This is a simple evaluation of the influence of the components on various properties of a thin film formed by quenching by sputtering in a simple manner using a liquid quenching ribbon.
- Example 1 30 g of raw materials weighed to the component composition shown in Table 1 were arc-melted in a reduced pressure Ar using a water-cooled copper mold of about ⁇ 10 ⁇ 40 mm to obtain a rapidly cooled ribbon base material.
- the conditions for preparing the quenched ribbon are the single roll method, set in this molten base material in a ⁇ 15 mm quartz tube, the diameter of the hot water nozzle is 1 mm, the atmospheric pressure is 61 kPa, the spray differential pressure is 69 kPa, and the copper roll ( ⁇ 300 mm) is rotated.
- Hot water was discharged at several 3000 rpm with a gap of 0.3 mm between the copper roll and the hot water nozzle. The hot water temperature was set immediately after each molten base material was melted. The following items were evaluated using the thus prepared quenched ribbon as a test material.
- Evaluation 1 Saturation magnetic flux density The saturation magnetic flux density of the quenched ribbon was measured with an applied magnetic field of 15 kOe using a VSM apparatus (vibrating sample magnetometer). The weight of the test material at that time was 15 mg.
- Evaluation 2 amorphous Usually, when measuring the X-ray diffraction pattern of an amorphous material, showed no diffraction peaks, the amorphous characteristic halo pattern. In addition, when it is not completely amorphous, a diffraction peak is seen, but the peak height is lower than that of the crystalline material, and a broad peak with a large half-value width (half height of the diffraction peak) Become. This half-value width correlates with the amorphous nature of the material, and the higher the amorphous nature, the more the diffraction peak becomes broader and the half-value width becomes larger. Therefore, the amorphous property of the quenched ribbon was evaluated by the following method.
- the test material was attached to a glass plate with a double-sided tape, and a diffraction pattern was obtained with an X-ray diffractometer. At this time, the test material was affixed on the glass plate so that the measurement surface was a copper roll contact surface of a quenched ribbon.
- the X-ray source was Cu—K ⁇ ray, and measurement was performed at a scan speed of 4 ° / min. The width of the half height of the main peak of this diffraction pattern was image-analyzed to find the half width, which was evaluated as amorphous. *
- Evaluation 3 Corrosion resistance
- the sample material was attached to a glass plate with a double-sided tape, and a salt spray test of 5% NaCl-35 ° C-16h was conducted.
- Each evaluation result is shown in Table 2.
- Comparative Example No. No. 12 has a low content of Fe as a component composition and a low value of Fe / (Co + Fe + Ni), so that the saturation magnetic flux density is low.
- Comparative Example No. No. 13 has a high Fe content as a component composition, a high value of Fe / (Co + Fe + Ni), and a small amount of Co, so that the corrosion resistance is inferior.
- Comparative Example No. No. 14 has a low Ni content as a component composition and a low value of Ni / (Co + Fe + Ni), so that the corrosion resistance is inferior.
- Comparative Example No. No. 15 has a high Ni content as a component composition and a high value of Ni / (Co + Fe + Ni), so that the saturation magnetic flux density is low.
- Comparative Example No. 16 has a small half width because the content of Zr + Hf + Nb + Ta + B / 2 is low. That is, the amorphous property is low. Comparative Example No. Since No. 17 has a high content of Zr + Hf + Nb + Ta + B / 2, the saturation magnetic flux density is low. Comparative Example No. Since No. 18 has high B content as a component composition, its corrosion resistance is inferior. Comparative Example No. Since No. 19 has a high Al + Cr content, the saturation magnetic flux density is low.
- Example 2 Next, examples relating to the influence of the raw material powder on the PTF value of the sputtering target material will be described.
- an alloy powder used as a raw material was prepared by a gas atomizing method, and a saturation magnetic flux density was measured to examine a raw material powder composition having a low saturation magnetic flux density. The results are shown in Table 3.
- these raw material powders and the raw material powder of the remaining composition shown in Table 4 are mixed so as to have the composition of the target material of Table 5, and the PTF value of the sputtering target material prepared by solidification molding and machining is measured. The influence of the raw material powder composition on the PTF value was examined. The results are shown in Table 5. At the same time, the corrosion resistance of the sputtering target material was evaluated.
- the raw material powder and the sputtering target material were prepared as follows.
- raw material powders having respective compositions shown in Tables 3 and 4 were prepared by a gas atomization method.
- the gas atomization method was performed under the conditions that the gas type was Ar, the nozzle diameter was 6 mm, and the gas pressure was 5 MPa. Thereafter, No. 1 shown in Table 3 was obtained.
- the powders 1 to 11 and the alloy powder having the corresponding residual composition shown in Table 4 were mixed at the residual composition powder mixing ratio shown in Table 4.
- the raw material powders were mixed by stirring in a V-type mixer.
- the vacuum-enclosed mixed powder was molded by the upset method.
- the upset method was performed under the conditions of a heating temperature of 950 ° C., a pressure of 540 MPa, and a processing time of 5 seconds.
- the upset method is a method in which a billet filled with raw material powder, deaerated, and sealed in a metal outer can is heated to a predetermined temperature, charged into a container, and pressure-formed by a punch.
- the molding pressure can be increased, and the molding can be performed by pressurizing for a short time.
- Evaluation 1 Saturation magnetic flux density The saturation magnetic flux density of the raw material powder was measured with an applied magnetic field of 15 kOe with a VSM apparatus (vibrating sample magnetometer). The weight of the test material at that time was 200 mg.
- Evaluation 2 PTF value
- the PTF value of the sputtering target material was measured according to ASTM F1761-00.
- a sputtering target material having the same composition was solidified and formed from a single component powder under the same conditions, and the PTF value was measured. In that case, it evaluated by the difference of the PTF which deducted the PTF value (unit:%) of the sputtering target material by a single powder from the PTF (unit:%) of the sputtering target material by mixed powder.
- Evaluation 3 Corrosion resistance As a corrosion resistance evaluation of the sputtering target material, as a salt spray test using the sputtering target material, the appearance of the sputtering target material after spraying a NaCl: 5 mass% solution for 24 hours based on JIS Z 2371 is visually observed. The presence or absence of fire was confirmed.
- the evaluation criteria were as follows. ⁇ : No occurrence ⁇ : Occurred on part of sputtering target material ⁇ : Generated on the entire surface of the sputtering target material
- Table 5 shows the components (at.%) Of the sputtering target material, the raw material powder, the difference in PTF value (%), and the corrosion resistance.
- B to D, F, and J are examples of the present invention, and A, E, G to I, and K are comparative examples.
- Comparative Examples A, E, and G are the raw material powder Nos. Used. Since the saturation magnetic flux density of 1, 5, and 7 is high, the effect of improving the PTF is small.
- sputtering was performed using the sputtering target material of Comparative Examples H and I at an Ar pressure of 0.5 Pa and a DC power of 500 W, many irregularities were generated on the surface of the sputtering target material, and the formed thin film had many particles, Compared with the thin film using the same composition sputtering target material shape
- the powder of No. 11 has Al + Cr of 6 at%, and No. 11 used for the production of the sputtering target material of Example J of the present invention. Compared to 10 powder, Cr is only 1 at% higher. As a result, the evaluation of the corrosion resistance of both the sputtering target materials of Invention Example J and Comparative Example K is ⁇ , and it can be seen that the effect of improving the corrosion resistance of the sputtering target material by adding Al + Cr is saturated.
- a sputtering target material having a composition of B, C, and D is designated as No. 2+ Residual composition 2, No. 3 + residual composition 3, no.
- the mixed powder of 4 + residual composition 4 was used and HIP treatment molding was performed at 950 ° C., 147 MPa, and 2 hours, the difference from the PTF of the sputtering target material produced from each single raw material powder was 8, 11, and It was 9%. From this, it can be seen that the PTF improvement effect is higher in the case of molding by the upset method than in the case of molding by the HIP method.
- the alloy powder in which Ni / (Fe + Ni) falls within the range of 0.27 to 0.35 has a very low saturation magnetic flux density, and this alloy powder is used as at least a part of the raw material powder to be solidified and molded. It can be seen that by obtaining a sputtering target material, the PTF value could be remarkably improved as compared with a uniform sputtering target material having the same composition.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Vapour Deposition (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
L’invention concerne des alliages magnétiques mous pour des supports d’enregistrement magnétiques verticaux avec une densité de flux magnétique de saturation, une non-cristallinité et une résistance à la corrosion supérieures, et des matériaux de cibles de pulvérisation qui, tout en étant sensiblement composés des alliages supérieurs, présentent des valeurs PTF élevées qui peuvent être utilisées efficacement pendant la pulvérisation de magnétrons. Les alliages comprennent, en % atomique, du Fe dans une proportion de 10-45 % ; du Ni dans une proportion de 1-25 %, un ou plusieurs éléments sélectionnés parmi Zr, Hf, Nb, Ta, et B dans une proportion totale de 5-10 % pour Zr+Hf+Nb+Ta+B/2 (à condition que B soit supérieur à 0 % et inférieur à 7 %), de l’Al ou du Cr ou les deux dans une proportion totale de 0-5 % pour Al+Cr, et du Co résiduel et les impuretés inévitables dans une proportion totale de 37 % ou plus. Par les rapports atomiques, ces alliages satisfont Fe/(Co+Fe+Ni): 0,10-0,50 et Ni/(Co+Fe+Ni): 0,01-0,25.
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CN200980135768.7A CN102149836B (zh) | 2008-07-14 | 2009-07-14 | 用于在垂直磁记录介质中的软磁膜层的溅射靶材及其制备方法 |
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JP2008182645A JP5605787B2 (ja) | 2008-07-14 | 2008-07-14 | 垂直磁気記録媒体における軟磁性膜層用合金を成膜するためのスパッタリングターゲット材とその製造方法 |
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JP (1) | JP5605787B2 (fr) |
CN (1) | CN102149836B (fr) |
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Cited By (3)
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JP4885333B1 (ja) * | 2010-09-03 | 2012-02-29 | Jx日鉱日石金属株式会社 | 強磁性材スパッタリングターゲット |
WO2012057087A1 (fr) * | 2010-10-26 | 2012-05-03 | 山陽特殊製鋼株式会社 | Alliage magnétique doux pour enregistrement magnétique, matériau de cible de pulvérisation et support d'enregistrement magnétique |
WO2013047328A1 (fr) * | 2011-09-28 | 2013-04-04 | 山陽特殊製鋼株式会社 | Alliage utilisé dans une couche de film mince à aimantation temporaire sur un support d'enregistrement magnétique perpendiculaire, matière cible de pulvérisation cathodique et support d'enregistrement magnétique perpendiculaire ayant une couche de film mince à aimantation temporaire |
Families Citing this family (8)
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JP5403418B2 (ja) * | 2008-09-22 | 2014-01-29 | 日立金属株式会社 | Co−Fe−Ni系合金スパッタリングターゲット材の製造方法 |
JP5917045B2 (ja) * | 2011-08-17 | 2016-05-11 | 山陽特殊製鋼株式会社 | 垂直磁気記録媒体における軟磁性薄膜層用合金およびスパッタリングターゲット材 |
JP5778052B2 (ja) * | 2012-02-03 | 2015-09-16 | 山陽特殊製鋼株式会社 | 磁気記録媒体に用いる低飽和磁束密度を有する軟磁性膜層用合金およびスパッタリングターゲット材 |
WO2013183546A1 (fr) * | 2012-06-06 | 2013-12-12 | 日立金属株式会社 | Matériau de cible de pulvérisation en alliage à base de fe-co, et son procédé de production |
JP6161991B2 (ja) * | 2013-08-15 | 2017-07-12 | 山陽特殊製鋼株式会社 | Fe−Co系合金スパッタリングターゲット材 |
JP6405261B2 (ja) * | 2014-05-01 | 2018-10-17 | 山陽特殊製鋼株式会社 | 磁気記録用軟磁性合金及びスパッタリングターゲット材並びに磁気記録媒体 |
TWI602940B (zh) * | 2014-06-11 | 2017-10-21 | 光洋應用材料科技股份有限公司 | 軟磁性合金濺鍍靶材及軟磁性合金材料 |
CN113787189A (zh) * | 2021-11-16 | 2021-12-14 | 西安欧中材料科技有限公司 | 一种增材制造用模具钢球形粉末及其循环利用方法 |
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- 2009-07-14 CN CN200980135768.7A patent/CN102149836B/zh not_active Expired - Fee Related
- 2009-07-14 WO PCT/JP2009/062716 patent/WO2010007980A1/fr active Application Filing
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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JP4885333B1 (ja) * | 2010-09-03 | 2012-02-29 | Jx日鉱日石金属株式会社 | 強磁性材スパッタリングターゲット |
WO2012029331A1 (fr) * | 2010-09-03 | 2012-03-08 | Jx日鉱日石金属株式会社 | Cible de pulvérisation cathodique en matériau ferromagnétique |
CN103038388A (zh) * | 2010-09-03 | 2013-04-10 | 吉坤日矿日石金属株式会社 | 强磁性材料溅射靶 |
WO2012057087A1 (fr) * | 2010-10-26 | 2012-05-03 | 山陽特殊製鋼株式会社 | Alliage magnétique doux pour enregistrement magnétique, matériau de cible de pulvérisation et support d'enregistrement magnétique |
JP2012108997A (ja) * | 2010-10-26 | 2012-06-07 | Sanyo Special Steel Co Ltd | 磁気記録用軟磁性合金およびスパッタリングターゲット材並びに磁気記録媒体 |
CN103221568A (zh) * | 2010-10-26 | 2013-07-24 | 山阳特殊制钢株式会社 | 磁记录用软磁性合金、溅射靶材及磁记录介质 |
CN103221568B (zh) * | 2010-10-26 | 2016-03-23 | 山阳特殊制钢株式会社 | 磁记录用软磁性合金、溅射靶材及磁记录介质 |
WO2013047328A1 (fr) * | 2011-09-28 | 2013-04-04 | 山陽特殊製鋼株式会社 | Alliage utilisé dans une couche de film mince à aimantation temporaire sur un support d'enregistrement magnétique perpendiculaire, matière cible de pulvérisation cathodique et support d'enregistrement magnétique perpendiculaire ayant une couche de film mince à aimantation temporaire |
JP2013072114A (ja) * | 2011-09-28 | 2013-04-22 | Sanyo Special Steel Co Ltd | 垂直磁気記録媒体における軟磁性薄膜層用合金およびスパッタリングターゲット材並びに軟磁性薄膜層を有する垂直磁気記録媒体。 |
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CN102149836B (zh) | 2014-03-19 |
JP2010018869A (ja) | 2010-01-28 |
JP5605787B2 (ja) | 2014-10-15 |
MY159546A (en) | 2017-01-13 |
CN102149836A (zh) | 2011-08-10 |
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