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WO2016035415A1 - Cible de pulvérisation - Google Patents

Cible de pulvérisation Download PDF

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Publication number
WO2016035415A1
WO2016035415A1 PCT/JP2015/067226 JP2015067226W WO2016035415A1 WO 2016035415 A1 WO2016035415 A1 WO 2016035415A1 JP 2015067226 W JP2015067226 W JP 2015067226W WO 2016035415 A1 WO2016035415 A1 WO 2016035415A1
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Prior art keywords
powder
sputtering target
sputtering
oxide
particles
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Ceased
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PCT/JP2015/067226
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English (en)
Japanese (ja)
Inventor
荒川　篤俊
優斗 森下
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JX Nippon Mining and Metals Corp
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JX Nippon Mining and Metals Corp
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Priority to CN201580009968.3A priority Critical patent/CN106029943B/zh
Priority to JP2015548075A priority patent/JP5946974B1/ja
Priority to SG11201606737UA priority patent/SG11201606737UA/en
Publication of WO2016035415A1 publication Critical patent/WO2016035415A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • C22C5/00—Alloys based on noble metals
    • C22C5/04—Alloys based on a platinum group metal
    • 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
    • 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

Definitions

  • the present invention relates to a magnetic material sputtering target used to form a magnetic thin film of a magnetic recording medium, in particular, a granular film in a magnetic recording medium of a hard disk adopting a perpendicular magnetic recording method, and causes the generation of particles during sputtering.
  • the present invention relates to a non-magnetic material particle-dispersed magnetic material sputtering target containing Co or Fe as a main component, which can suppress abnormal discharge of the non-magnetic material.
  • a material based on Co or Fe which is a ferromagnetic metal, is used for a recording layer of a hard disk adopting a perpendicular magnetic recording system.
  • Co—Cr-based, Co—Pt, Co—Cr—Pt-based, and Fe—Pt-based alloys composed mainly of ferromagnetic metals and non-magnetic inorganic materials are often used. Yes.
  • the magnetic thin film of such magnetic recording media, such as a hard disk is often produced by sputtering a sputtering target containing the above material as a component because of high productivity.
  • a melting method or a powder metallurgy method can be considered as a method for producing a sputtering target for a magnetic recording medium. Which method is used depends on the required characteristics, but it cannot be unequivocally stated, but it is used for the recording layer of hard disks of the perpendicular magnetic recording system, an alloy mainly composed of a ferromagnetic metal and a non-magnetic inorganic substance.
  • Sputtering targets made of particles are generally produced by powder metallurgy. This is because the inorganic particles need to be uniformly dispersed in the alloy substrate, and thus it is difficult to produce by the melting method.
  • Patent Document 1 As a powder metallurgy method, for example, in Patent Document 1, mixed powder obtained by mixing Co powder, Cr powder, TiO 2 powder, and SiO 2 powder and Co spherical powder are mixed by a planetary motion mixer, and this mixing is performed. A method has been proposed in which powder is formed by hot pressing to obtain a sputtering target for a magnetic recording medium.
  • Patent Document 2 discloses a sputtering target for forming a magnetic recording medium thin film by mixing Co—Cr binary alloy powder, Pt powder, and SiO 2 powder and hot-pressing the obtained mixed powder. A method has been proposed.
  • Patent Document 3 proposes a sputtering target composed of a matrix phase of Co and Pt and a metal oxide phase having an average particle size of 0.05 ⁇ m or more and less than 7.0 ⁇ m, which suppresses the growth of crystal grains and has a low Proposals have been made to increase the film formation efficiency by obtaining a magnetic permeability and high density target. Further, in Patent Document 4, the average particle diameter of the particles formed by the oxide phase is set to 3 ⁇ m or less, and in Patent Document 5, silica particles or titania particles are sputtered in a cross section perpendicular to the main surface of the sputtering target.
  • the average particle diameter of the oxide particles present in the target is 1.5 ⁇ m or less
  • the maximum value of the distance between any two points on the outer periphery of the oxide particles is the maximum diameter
  • the inventors of the present invention have found that in a sputtering target containing an oxide phase as non-magnetic material particles, the oxide phase is formed in the form of a material having a high melting point. It has been found that by making it exist in the inside, the coarsening of the oxide phase can be prevented, an abnormal discharge due to a nonmagnetic material during sputtering does not occur, and a target with less generation of particles can be obtained.
  • a sputtering target containing an alloy containing Co or Fe as a main component and an oxide containing Mn and B and in the composition of the sputtering target, 9 at% ⁇ Mn + B + O ⁇ 56 at%, B ⁇ Mn (at %) And Mn + B ⁇ O (at%).
  • a sputtering target containing an alloy containing Co or Fe as a main component and Mn, B and X (where X is one or more elements selected from Co, Cr and Si), A sputtering target characterized in that the composition of the sputtering target satisfies the following conditions: 9 at% ⁇ Mn + B + X + O ⁇ 56 at%, B ⁇ Mn + X (at%), Mn + X + B ⁇ O (at%).
  • an oxide containing Mn and B or an oxide containing Mn, X and B is contained in an amount of 0.1 mol% or more and 15 mol% or less, respectively 1) or 2) The sputtering target as described.
  • the maximum value of the distance between any two points on the outer periphery of the oxide particles is the maximum diameter, and the distance between the two lines when the particles are sandwiched between two parallel lines
  • the ratio of the maximum diameter to the minimum diameter shows a numerical value larger than 0.5
  • oxide particles having a particle area of 6 ⁇ m 2 or more are within 1 mm 2 field of view.
  • the sputtering target according to any one of 1) to 3) above, which has an average of 1 or less.
  • One or more elements selected from Pt, Ru, Ag, and Pd are contained in an alloy component of the sputtering target in an amount of 1 mol% to 50 mol%, according to any one of 1) to 4) above Sputtering target.
  • the non-magnetic material particle dispersion type magnetic material sputtering target of the present invention thus adjusted does not cause abnormal discharge due to the non-magnetic material during sputtering, and a target with less generation of particles can be obtained. Thereby, it has the outstanding effect that the cost improvement effect by a yield improvement can be acquired.
  • FIG. 1 is a diagram (photograph) showing a cross-sectional structure of a sputtering target of Example 1.
  • FIG. It is a figure (photograph) which shows the sputtering target cross-sectional structure of the comparative example 1.
  • the sputtering target of the present invention has a structure in which oxide particles containing Mn and B are dispersed as a nonmagnetic material in an alloy mainly composed of Co or Fe, which is a ferromagnetic metal.
  • the alloy containing Co or Fe as a main component include ferromagnetic alloys such as a Co—Cr alloy, a Co—Pt alloy, a Co—Cr—Pt alloy, and an Fe—Pt alloy.
  • Oxide particles containing Mn and B contained as a nonmagnetic material have good wettability with an alloy containing Co or Fe as the main component, and are effective in improving the quality of the magnetic recording medium.
  • the present inventor can prevent the oxide agglomeration (coarse) in the sputtering target structure by forming the oxide containing B in the form of Mn—B—O and forming a material having a high melting point. It was possible to obtain the knowledge that the abnormal discharge caused by the aggregated portion of the oxide can be remarkably suppressed.
  • the sputtering target of the present invention is a sputtering target containing an alloy containing Co or Fe as a main component and an oxide containing Mn and B.
  • 9 at% ⁇ It is characterized by satisfying the conditions of Mn + B + O ⁇ 56 at%, B ⁇ Mn (at%), and Mn + B ⁇ O (at%).
  • the sputtering target if the total content of Mn, B, and O is less than 9 at%, the effect of good characteristics of the perpendicular magnetic recording medium due to the inclusion of Mn, B, and O cannot be obtained, and Mn, B, and O
  • the oxide phase itself composed of Mn—B—O becomes coarse.
  • B> Mn (at%) B is not limited to the form of Mn—B—O, but B—O is present, and the B oxide is dissolved during the sintering, so that the oxide particles (Phase) becomes coarse.
  • Mn + B> O (at%) the effect of good characteristics of the perpendicular magnetic recording medium cannot be obtained.
  • the melting point is higher than that of B 2 O 3 and the dissolution during sintering is suppressed. And abnormal discharge due to coarse particles during sputtering can be reduced.
  • the conditions of 9 at% ⁇ Mn + X + B + O ⁇ 56 at%, B ⁇ Mn + X (at%), and Mn + X + B ⁇ O (at%) are satisfied.
  • the total content of Mn, X, B, and O is less than 9 at% in the composition of the sputtering target, the effect of good characteristics of the perpendicular magnetic recording medium due to the inclusion of Mn, X, B, and O cannot be obtained.
  • the total content of Mn, X, B, and O exceeds 56 at%, the oxide phase composed of Mn—X—B—O becomes coarse.
  • B is not limited to the form of Mn—X—B—O, but B—O is present, and the B oxide is dissolved out during the sintering. The product particles (phase) become coarse. Further, when Mn + X + B> O (at%), the effect of good characteristics of the perpendicular magnetic recording medium cannot be obtained.
  • the present invention also covers the scope of the present invention in the case of a composition in which B is expressed as a simple substance instead of an oxide.
  • B is not added as an oxide, but a reaction of 2B + 3CoO ⁇ B 2 O 3 + 3Co occurs during sintering.
  • a B oxide is formed, and the B oxide is melted during sintering and an enlarged structure is observed.
  • Co-40Pt—B 2 O 3 -2MnO—CoO (mol%) is considered, and the composition of the Mn oxide, X oxide (corresponding to CoO) and B oxide in the sputtering target is set as described above. It is necessary to adjust to meet.
  • the composition of the sputtering target after oxidation is included in the scope of the present invention as long as the composition is within the range defined in the present invention.
  • the content of the above-described oxide containing Mn and B or the oxide containing Mn, X and B is preferably 0.1 mol% or more and 15 mol% or less in the composition of the sputtering target. If the amount is less than 0.1 mol%, the inclusion effect is hardly observed, and if it exceeds 15 mol%, the content is too large to obtain the desired effect.
  • the Si oxide content is preferably 10 mol% or less, and more preferably 6 mol% or less.
  • the maximum value of the distance between any two points on the outer periphery of the oxide particle is set as the maximum diameter on the target surface or the cross-sectional structure, and the particle is sandwiched between two parallel straight lines.
  • the minimum value of the distance between two straight lines is the minimum diameter
  • the ratio of the maximum diameter to the minimum diameter is a value larger than 0.5
  • the oxide particle having a particle area of 6 ⁇ m 2 or more is 1 mm 2. It is characterized by an average of less than 1 in the field of view.
  • all the oxide particles in the sputtering target of the present invention do not show a numerical value in which the ratio of the maximum diameter to the minimum diameter is larger than 0.5.
  • the increase in the number of particles is greatly affected. If the shape of the oxide particles is long and continuous, it is difficult to cause grain breakage and discharge abnormalities, but the diameter of the oxide particles is close to a circle or square (that is, the ratio of the maximum diameter to the minimum diameter is 0.5). If it shows a larger numerical value), the increase in the number of particles has a great influence.
  • the observation of the structure of the sputtering target is performed at any five locations by polishing the target surface and using an electron microscope (viewing field: 1 mm 2 ). The microscopic image is displayed on a PC screen, image analysis processing (binarization processing) is performed, the outline of the oxide particles (black portions) is clarified, and the number of oxide particles of a predetermined size is counted. The average number is obtained.
  • a Co alloy such as a Co—Cr alloy, a Co—Pt alloy, a Co—Cr—Pt alloy, or an Fe alloy such as an Fe—Pt alloy is effective.
  • one or more elements selected from Pt, Ru, Ag, and Pd are contained in an alloy component of the sputtering target in an amount of 1 mol% to 50 mol%. These are elements added as necessary, and the added amount is an effective amount for exerting the effect of addition.
  • the sputtering target of the present invention can be produced by a powder metallurgy method.
  • a metal raw material powder such as Co, Fe, and Pt
  • a non-magnetic material raw material powder such as MnO
  • an additive metal powder such as Ag
  • the particle size of the raw material it is desirable to use metal powder having an average particle diameter of 10 ⁇ m or less and non-magnetic material powder of 5 ⁇ m or less.
  • the non-magnetic material raw powder is more likely to be as spherical as possible to achieve the microstructure of the present invention.
  • the particle size of the powder can be measured with a laser diffraction particle size distribution meter.
  • an oxide raw material having a low melting point such as B oxide does not melt during sintering and the oxide phase is not coarsened.
  • the oxides having a high melting point (MnBO 3 , Mn 3 B 2 O 6 or the like) is prepared in advance and used as a raw material powder.
  • MnBO 3 powder for example, mixing a Mn 2 O 3 powder and B 2 O 3 powder, synthetic, can be used after pulverizing. However, the MnBO 3 powder may become Mn-rich, B-rich, and oxygen-rich MnBO 3 powder rather than the stoichiometric ratio.
  • Mn and B composition of the produced MnBO 3 powder for each mixed, synthesized, and pulverized lot, and determine the weighed value so as to obtain a predetermined target composition.
  • the Mn 3 B 2 O 6 powder for example, can be used mixed with MnO powder and B 2 O 3 powder, synthetic, those pulverized.
  • the Mn 3 B 2 O 6 powder may be Mn-rich, B-rich, and oxygen-rich Mn 3 B 2 O 6 powders rather than the stoichiometric ratio, as with the MnBO 3 powder, it was prepared.
  • Mn and B composition of the Mn 3 B 2 O 6 powder it is preferable to analyze the Mn and B composition of the Mn 3 B 2 O 6 powder for each lot that has been mixed, synthesized, and pulverized, and to determine the weighed value so as to obtain a predetermined target composition. At that time, it is preferable to use a small amount of CoO powder, Mn powder, CoB powder or the like for adjustment to obtain a desired composition. Next, these metal powders, non-magnetic material raw material powders, and the like are weighed so as to have a desired composition, and mixed by pulverization using a known method such as a ball mill. In order to shorten the mixing time and increase the productivity, it is preferable to use a high energy ball mill.
  • the mixed powder obtained as described above is sintered using a hot press or a hot isostatic press. Although it depends on the component composition of the target, by setting the mixing conditions and sintering conditions for the above raw materials, the density is sufficiently high and the conditions for non-magnetic material particles to be finely dispersed in the metal phase are found. If the manufacturing conditions are fixed, a sintered body target in which such non-magnetic material particles are always dispersed can be obtained.
  • Example 1 As the metal raw material powder, Co powder with an average particle diameter of 4 ⁇ m, Pt powder with an average particle diameter of 3 ⁇ m, as a nonmagnetic material powder, Cr 2 O 3 powder with an average particle diameter of 1 ⁇ m, MnBO 3 powder with an average particle diameter of 1.2 ⁇ m, A SiO 2 powder having an average particle size of 0.7 ⁇ m and a CoO powder having an average particle size of 2 ⁇ m were prepared.
  • MnBO 3 powder was used previously Mn 2 O 3 powder, B 2 O 3 powder mixed, synthetic, those pulverized. Then, 1500 g of these powders were weighed at the following composition ratio.
  • the composition of the oxide component is as follows: Mn: 3.2 at%, X as Co: 1.6 at%, Cr: 3.2 at% and Si: 0.8 at%, B: 3.2 at%, O: 16 .1 at%.
  • the weighed powder was enclosed in a ball mill pot with a capacity of 10 liters together with a tungsten alloy ball as a grinding medium, and rotated and mixed for 120 hours.
  • the mixed powder thus obtained was filled in a carbon mold and hot-pressed in a vacuum atmosphere at a temperature of 980 ° C., a holding time of 2 hours, and a pressure of 30 MPa to obtain a sintered body. Further, this was cut with a lathe to obtain a disk-shaped sputtering target having a diameter of 180 mm and a thickness of 4 mm.
  • the ratio of the maximum diameter to the minimum diameter is larger than 0.5 within a 1 mm 2 visual field, and the particle area is 6 ⁇ m.
  • the average number of the two or more oxide particles was 0.5.
  • a microscopic image is displayed on a PC screen, and image analysis processing (binarization processing) is performed. These were calculated after clarifying the outline of (black part).
  • this target was attached to a DC magnetron sputtering apparatus, and sputtering was performed.
  • the sputtering conditions were a sputtering power of 1.2 kW, an Ar gas pressure of 1.5 Pa, and after performing 2 kWhr pre-sputtering, sputtering was performed on a 4-inch diameter silicon substrate with a target film thickness of 1000 nm.
  • the number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles on the silicon substrate was seven. Even when sputtering is not performed, the number of particles on the silicon substrate may be counted as 4 to 6 when measured with a particle counter. Therefore, it can be said that the number of particles in this example is at an extremely low level. .
  • the composition of this oxide component is Mn: 2.3 at%
  • X is Cr: 1.6 at%
  • Si 0.8 at%
  • B 7.8 at%
  • O 17.8 at%.
  • the weighed powder was enclosed in a ball mill pot with a capacity of 10 liters together with a tungsten alloy ball as a grinding medium, and rotated and mixed for 120 hours.
  • the mixed powder thus obtained was filled in a carbon mold, and in the same manner as in Example 1, sintered in a vacuum atmosphere by hot pressing at a temperature of 980 ° C., a holding time of 2 hours, and a pressure of 30 MPa. Got. Further, this was cut with a lathe to obtain a disk-shaped sputtering target having a diameter of 180 mm and a thickness of 4 mm.
  • the ratio of the maximum diameter to the minimum diameter is larger than 0.5 in a 1 mm 2 visual field, and the particle area is 6 ⁇ m 2.
  • the average number of the above oxide particles was 3.0. In calculating the maximum diameter, the minimum diameter, and the particle area of the oxide particles, the calculation was performed in the same manner as in Example 1.
  • this target was attached to a DC magnetron sputtering apparatus, and sputtering was performed.
  • the sputtering conditions were a sputtering power of 1.2 kW, an Ar gas pressure of 1.5 Pa, and after performing 2 kWhr pre-sputtering, sputtering was performed on a 4-inch diameter silicon substrate with a target film thickness of 1000 nm.
  • the number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles on the silicon substrate was 35.
  • Example 2 As a metal raw material powder, Co powder with an average particle diameter of 4 ⁇ m, Pt powder with an average particle diameter of 3 ⁇ m, Ru powder with an average particle diameter of 5 ⁇ m, Mn powder with an average particle diameter of 4 ⁇ m, and CrBO 3 with an average particle diameter of 1 ⁇ m as a nonmagnetic material powder. A powder, MnBO 3 powder having an average particle diameter of 1.2 ⁇ m, and TiO 2 powder having an average particle diameter of 1 ⁇ m were prepared. For MnBO 3 powder, pre-mixing the Mn 2 O 3 powder and B 2 O 3 powder, synthesized, it was used after grinding. The same was used for CrBO 3 powder.
  • the composition of the oxide component is Mn: 2.3 at%, X is Cr: 4.5 at%, B: 6.0 at%, O: 19.6 at%. Note that Ti is omitted.
  • the weighed powder was enclosed in a ball mill pot with a capacity of 10 liters together with a tungsten alloy ball as a grinding medium, and rotated and mixed for 120 hours.
  • the mixed powder thus obtained was filled in a carbon mold, and in the same manner as in Example 1, sintered in a vacuum atmosphere by hot pressing at a temperature of 980 ° C., a holding time of 2 hours, and a pressure of 30 MPa. Got. Further, this was cut with a lathe to obtain a disk-shaped sputtering target having a diameter of 180 mm and a thickness of 4 mm.
  • the ratio of the maximum diameter to the minimum diameter is larger than 0.5 in a 1 mm 2 visual field, and the particle area is 6 ⁇ m 2.
  • the average number of the above oxide particles was 0.8. In calculating the maximum diameter, the minimum diameter, and the particle area of the oxide particles, the calculation was performed in the same manner as in Example 1.
  • this target was attached to a DC magnetron sputtering apparatus, and sputtering was performed.
  • the sputtering conditions were a sputtering power of 1.2 kW, an Ar gas pressure of 1.5 Pa, and after performing 2 kWhr pre-sputtering, sputtering was performed on a 4-inch diameter silicon substrate with a target film thickness of 1000 nm.
  • the number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles on the silicon substrate was nine.
  • Example 3 As the metal raw material powder, Fe powder having an average particle diameter of 4 ⁇ m, Pt powder having an average particle diameter of 3 ⁇ m, Ag powder having an average particle diameter of 5 ⁇ m, and MnBO 3 powder having an average particle diameter of 1.2 ⁇ m, an average particle diameter of 0 A 7 ⁇ m SiO 2 powder was prepared.
  • MnBO 3 powder was used previously Mn 2 O 3 powder, B 2 O 3 powder mixed, synthetic, those pulverized. Then, 1500 g of these powders were weighed at the following composition ratio.
  • the composition of the oxide component is Mn: 1.7 at%
  • X is Si: 5.8 at%
  • B 1.7 at%
  • O 15.8 at%.
  • the weighed powder was enclosed in a ball mill pot with a capacity of 10 liters together with a tungsten alloy ball as a grinding medium, and rotated and mixed for 120 hours.
  • the mixed powder thus obtained was filled in a carbon mold, and in the same manner as in Example 1, sintered in a vacuum atmosphere by hot pressing at a temperature of 980 ° C., a holding time of 2 hours, and a pressure of 30 MPa. Got. Further, this was cut with a lathe to obtain a disk-shaped sputtering target having a diameter of 180 mm and a thickness of 4 mm.
  • the ratio of the maximum diameter to the minimum diameter is larger than 0.5 in a 1 mm 2 visual field, and the particle area is 6 ⁇ m 2.
  • the average number of the above oxide particles was 1.0. In calculating the maximum diameter, the minimum diameter, and the particle area of the oxide particles, the calculation was performed in the same manner as in Example 1.
  • this target was attached to a DC magnetron sputtering apparatus, and sputtering was performed.
  • the sputtering conditions were a sputtering power of 1.2 kW, an Ar gas pressure of 1.5 Pa, and after performing 2 kWhr pre-sputtering, sputtering was performed on a 4-inch diameter silicon substrate with a target film thickness of 1000 nm.
  • the number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles on the silicon substrate was 11.
  • Example 4 As the metal raw material powder, Co powder with an average particle size of 4 ⁇ m, Pt powder with an average particle size of 3 ⁇ m, Pd powder with an average particle size of 5 ⁇ m, and MnBO 3 powder with an average particle size of 1.2 ⁇ m, an average particle size of 2 ⁇ m as a nonmagnetic material powder Co 3 O 4 powder was prepared.
  • MnBO 3 powder previously, Mn 2 O 3 powder, the B 2 O 3 powder mixed, synthesized, was used after grinding. Then, 1500 g of these powders were weighed at the following composition ratio.
  • the composition of the oxide component is Mn: 1.6 at%
  • X is Co: 7.1 at%
  • B 1.6 at%
  • O 14.3 at%.
  • the weighed powder was enclosed in a ball mill pot with a capacity of 10 liters together with a tungsten alloy ball as a grinding medium, and rotated and mixed for 120 hours.
  • the mixed powder thus obtained was filled in a carbon mold, and in the same manner as in Example 1, sintered in a vacuum atmosphere by hot pressing at a temperature of 980 ° C., a holding time of 2 hours, and a pressure of 30 MPa. Got. Further, this was cut with a lathe to obtain a disk-shaped sputtering target having a diameter of 180 mm and a thickness of 4 mm.
  • the ratio of the maximum diameter to the minimum diameter is larger than 0.5 in a 1 mm 2 visual field, and the particle area is 6 ⁇ m 2.
  • the average number of the above oxide particles was 1.0. In calculating the maximum diameter, the minimum diameter, and the particle area of the oxide particles, the calculation was performed in the same manner as in Example 1.
  • this target was attached to a DC magnetron sputtering apparatus, and sputtering was performed.
  • the sputtering conditions were a sputtering power of 1.2 kW, an Ar gas pressure of 1.5 Pa, and after performing 2 kWhr pre-sputtering, sputtering was performed on a 4-inch diameter silicon substrate with a target film thickness of 1000 nm.
  • the number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles on the silicon substrate was eight.
  • Example 5 As the metal raw material powder, Co powder with an average particle diameter of 4 ⁇ m, Pt powder with an average particle diameter of 3 ⁇ m, as nonmagnetic material powder, Mn 3 B 2 O 6 powder with an average particle diameter of 2.4 ⁇ m, SiO 2 powder with an average particle diameter of 2 ⁇ m A CoO powder having an average particle diameter of 2 ⁇ m was prepared. The Mn 3 B 2 O 6 powder was used previously MnO powder, B 2 O 3 powder mixed, synthetic, those pulverized. Then, 1500 g of these powders were weighed at the following composition ratio.
  • the composition of this oxide component is Mn: 2.6 at%, X is Co: 3.5 at%, B: 1.7 at%, Si: 1.7 at%, O: 12.2 at%.
  • the weighed powder was enclosed in a ball mill pot with a capacity of 10 liters together with a tungsten alloy ball as a grinding medium, and rotated and mixed for 120 hours.
  • the mixed powder thus obtained was filled in a carbon mold, and in the same manner as in Example 1, sintered in a vacuum atmosphere by hot pressing at a temperature of 980 ° C., a holding time of 2 hours, and a pressure of 30 MPa. Got. Further, this was cut with a lathe to obtain a disk-shaped sputtering target having a diameter of 180 mm and a thickness of 4 mm.
  • the ratio of the maximum diameter to the minimum diameter is larger than 0.5 in a 1 mm 2 visual field, and the particle area is 6 ⁇ m 2.
  • the average number of the above oxide particles was 0.8. In calculating the maximum diameter, the minimum diameter, and the particle area of the oxide particles, the calculation was performed in the same manner as in Example 1.
  • this target was attached to a DC magnetron sputtering apparatus, and sputtering was performed.
  • the sputtering conditions were a sputtering power of 1.2 kW, an Ar gas pressure of 1.5 Pa, and after performing 2 kWhr pre-sputtering, sputtering was performed on a 4-inch diameter silicon substrate with a target film thickness of 1000 nm.
  • the number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles on the silicon substrate was seven.
  • the present invention can suppress abnormal discharge due to a nonmagnetic material during sputtering by suppressing aggregation (coarseness) of the oxide phase.
  • the magnetic thin film of a magnetic recording medium particularly a hard disk, has an excellent effect of reducing the generation of particles during sputtering caused by abnormal discharge and obtaining a cost improvement effect by improving yield. It is useful as a ferromagnetic material sputtering target used for forming a drive recording layer.

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  • Thin Magnetic Films (AREA)

Abstract

L'invention concerne une cible de pulvérisation contenant : un alliage comprenant du Co ou du Fe comme composant principal; et un oxyde comprenant du Mn et du B. La cible de pulvérisation est caractérisée en ce qu'elle a la composition, qui satisfait les conditions de 9% at. ≦ Mn + B + O ≦ 56% at., B ≦ Mn (% at.), et Mn + B ≦ O (% at.) Cette cible de pulvérisation est capable de supprimer une décharge anormale qui est provoquée par un matériau non magnétique et entraîne la formation de particules pendant la pulvérisation.
PCT/JP2015/067226 2014-09-04 2015-06-16 Cible de pulvérisation Ceased WO2016035415A1 (fr)

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CN201580009968.3A CN106029943B (zh) 2014-09-04 2015-06-16 溅射靶
JP2015548075A JP5946974B1 (ja) 2014-09-04 2015-06-16 スパッタリングターゲット
SG11201606737UA SG11201606737UA (en) 2014-09-04 2015-06-16 Sputtering target

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018123500A1 (fr) * 2016-12-28 2018-07-05 Ｊｘ金属株式会社 Cible de pulvérisation de matériau magnétique et procédé de production de ladite cible
CN108884557A (zh) * 2016-03-31 2018-11-23 捷客斯金属株式会社 强磁性材料溅射靶
WO2020066114A1 (fr) * 2018-09-25 2020-04-02 Ｊｘ金属株式会社 Cible de pulvérisation et poudre pour produire une cible de pulvérisation
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JP7625109B1 (ja) 2024-03-29 2025-01-31 Ｊｘ金属株式会社 磁性材ターゲット及び磁性材ターゲット組立品
JP7625110B1 (ja) 2024-03-29 2025-01-31 Ｊｘ金属株式会社 磁性材ターゲット及び磁性材ターゲット組立品
JP7625111B1 (ja) 2024-03-29 2025-01-31 Ｊｘ金属株式会社 磁性材ターゲット及び磁性材ターゲット組立品
JP7625112B1 (ja) 2024-03-29 2025-01-31 Ｊｘ金属株式会社 磁性材ターゲット及び磁性材ターゲット組立品

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* Cited by examiner, † Cited by third party
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63276728A (ja) * 1987-05-08 1988-11-15 Hitachi Ltd 光磁気記録媒体
JPH07232926A (ja) * 1993-12-27 1995-09-05 Alps Electric Co Ltd 微細結晶粒フェライト及びその製造方法
JP2012169021A (ja) * 2011-02-16 2012-09-06 Sanyo Special Steel Co Ltd 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ならびに磁気記録媒体
WO2013024845A1 (fr) * 2011-08-17 2013-02-21 山陽特殊製鋼株式会社 Alliage pour une couche de film mince magnétique et tendre sur un support d'enregistrement magnétique perpendiculaire et matériau de cible de pulvérisation

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050277002A1 (en) * 2004-06-15 2005-12-15 Heraeus, Inc. Enhanced sputter target alloy compositions
CN102482765B (zh) * 2010-07-20 2014-03-26 吉坤日矿日石金属株式会社 粉粒产生少的强磁性材料溅射靶

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63276728A (ja) * 1987-05-08 1988-11-15 Hitachi Ltd 光磁気記録媒体
JPH07232926A (ja) * 1993-12-27 1995-09-05 Alps Electric Co Ltd 微細結晶粒フェライト及びその製造方法
JP2012169021A (ja) * 2011-02-16 2012-09-06 Sanyo Special Steel Co Ltd 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ならびに磁気記録媒体
WO2013024845A1 (fr) * 2011-08-17 2013-02-21 山陽特殊製鋼株式会社 Alliage pour une couche de film mince magnétique et tendre sur un support d'enregistrement magnétique perpendiculaire et matériau de cible de pulvérisation

Cited By (17)

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WO2018123500A1 (fr) * 2016-12-28 2018-07-05 Ｊｘ金属株式会社 Cible de pulvérisation de matériau magnétique et procédé de production de ladite cible
JPWO2018123500A1 (ja) * 2016-12-28 2019-03-28 Ｊｘ金属株式会社 磁性材スパッタリングターゲット及びその製造方法
WO2020066114A1 (fr) * 2018-09-25 2020-04-02 Ｊｘ金属株式会社 Cible de pulvérisation et poudre pour produire une cible de pulvérisation
CN112739846A (zh) * 2018-09-25 2021-04-30 Ｊｘ金属株式会社 溅射靶以及用于制造溅射靶的粉体
JPWO2020066114A1 (ja) * 2018-09-25 2021-10-21 Ｊｘ金属株式会社 スパッタリングターゲット及びスパッタリングターゲットの製造方法
JP7072664B2 (ja) 2018-09-25 2022-05-20 Ｊｘ金属株式会社 スパッタリングターゲット及びスパッタリングターゲットの製造方法
JP7625109B1 (ja) 2024-03-29 2025-01-31 Ｊｘ金属株式会社 磁性材ターゲット及び磁性材ターゲット組立品
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JP2025154879A (ja) * 2024-03-29 2025-10-10 Ｊｘ金属株式会社 磁性材ターゲット及び磁性材ターゲット組立品
JP2025154895A (ja) * 2024-03-29 2025-10-10 Ｊｘ金属株式会社 磁性材ターゲット及び磁性材ターゲット組立品
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JP2025154891A (ja) * 2024-03-29 2025-10-10 Ｊｘ金属株式会社 磁性材ターゲット及び磁性材ターゲット組立品
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JPWO2016035415A1 (ja) 2017-04-27
MY179241A (en) 2020-11-02
JP5946974B1 (ja) 2016-07-06
CN106029943A (zh) 2016-10-12
CN106029943B (zh) 2018-08-31

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