WO2014175392A1 - Cible de pulvérisation pour film d'enregistrement magnétique, et matière carbonée brute destinée à être utilisée dans la production de celle-ci - Google Patents

Cible de pulvérisation pour film d'enregistrement magnétique, et matière carbonée brute destinée à être utilisée dans la production de celle-ci Download PDF

Info

Publication number
WO2014175392A1
WO2014175392A1 PCT/JP2014/061594 JP2014061594W WO2014175392A1 WO 2014175392 A1 WO2014175392 A1 WO 2014175392A1 JP 2014061594 W JP2014061594 W JP 2014061594W WO 2014175392 A1 WO2014175392 A1 WO 2014175392A1
Authority
WO
WIPO (PCT)
Prior art keywords
sputtering
powder
particles
sputtering target
target
Prior art date
Application number
PCT/JP2014/061594
Other languages
English (en)
Japanese (ja)
Inventor
真一 荻野
Original Assignee
Jx日鉱日石金属株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jx日鉱日石金属株式会社 filed Critical Jx日鉱日石金属株式会社
Priority to SG11201506097YA priority Critical patent/SG11201506097YA/en
Priority to JP2014530046A priority patent/JP5876155B2/ja
Priority to CN201480006305.1A priority patent/CN104955981B/zh
Publication of WO2014175392A1 publication Critical patent/WO2014175392A1/fr

Links

Images

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
    • G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
    • G11B5/851—Coating a support with a magnetic layer by sputtering
    • 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

Definitions

  • the present invention relates to a sputtering target used for manufacturing a magnetic thin film in a heat-assisted magnetic recording medium and a carbon raw material used for manufacturing the sputtering target.
  • a material based on Co, Fe, or Ni which is a ferromagnetic metal, is used as a material for a magnetic thin film in a magnetic recording medium.
  • a Co—Cr-based or Co—Cr—Pt-based ferromagnetic alloy containing Co as a main component has been used.
  • hard magnetic thin films employing perpendicular magnetic recording that have been put into practical use in recent years often use a composite material composed of Co—Cr—Pt-based ferromagnetic alloy mainly composed of Co and non-magnetic inorganic particles. It has been.
  • the said magnetic thin film is high in productivity, it is often produced by sputtering the sputtering target which uses the said material as a component with a DC magnetron sputtering apparatus.
  • the recording density of hard disks is rapidly increasing year by year, and it is considered that the future will reach 1 Tbit / in 2 from the current surface density of 600 Gbit / in 2 .
  • the size of the recording bit becomes less than 10 nm.
  • superparamagnetization due to thermal fluctuation is expected to be a problem.
  • a material such as a material in which Pt is added to a Co—Cr base alloy to increase the magnetocrystalline anisotropy is not sufficient. This is because magnetic particles that behave stably as ferromagnetism with a size of 10 nm or less need to have higher crystal magnetic anisotropy.
  • FePt phase having an L1 0 structure is attracting attention as a material for an ultra-high density recording medium.
  • the FePt phase is expected to be a material suitable for application as a magnetic recording medium because it has high crystal magnetic anisotropy and excellent corrosion resistance and oxidation resistance.
  • it is necessary to develop a technique that aligns and disperses ordered FePt magnetic particles with as high a density as possible in a magnetically isolated state. It has been.
  • a granular structure magnetic thin film of FePt magnetic particles are isolated by a non-magnetic material such oxides or carbon having an L1 0 structure, as for a magnetic recording medium of the next generation hard disk employing a thermally assisted magnetic recording method ,Proposed.
  • This granular structure magnetic thin film has a structure in which magnetic particles are magnetically insulated by interposition of a nonmagnetic substance.
  • a granular magnetic thin film having an Fe—Pt phase is formed using an Fe—Pt sintered sputtering target.
  • Patent Document 1 a technique related to a ferromagnetic sputtering target using a metal oxide has been disclosed.
  • Patent Documents 2 and 3 describe that a sputtering target for forming a magnetic recording medium film has a structure in which C is interposed in a metal matrix.
  • the graphite powder or carbon black powder used as the C raw material powder is degassed by heat-treating in advance in a vacuum.
  • a sputtering target containing a non-magnetic material in an alloy with a sputtering apparatus When attempting to sputter a sputtering target containing a non-magnetic material in an alloy with a sputtering apparatus, there is a problem that abnormal discharge occurs from the non-magnetic material as a starting point during sputtering and particles (dust attached to the substrate) are generated.
  • a sputtering target in which a nonmagnetic material is usually contained in an alloy is produced by a powder sintering method.
  • C when C is contained in Fe—Pt, C is a difficult-to-sinter material. There was a case where a ready dropout occurred.
  • the present invention provides an Fe—Pt-based sputtering target in which C particles are dispersed and a carbon raw material used in the production thereof, which enable the production of a magnetic thin film of a thermally assisted magnetic recording medium without using an expensive simultaneous sputtering apparatus. Furthermore, it is an object to provide a sputtering target in which the amount of particles generated during sputtering is reduced.
  • the present invention 1) A sintered sputtering target made of an alloy having a composition of Pt of 5 to 60 mol% and the balance of Fe and a nonmagnetic material dispersed in the alloy, and at least C of 5 to 60 mol% as the nonmagnetic material An average particle area of C particles in a cross section perpendicular to the sputtering surface of the target is 50 ⁇ m 2 or more, 2) The sputtering target according to 1) above, wherein the average value of the peripheral length of the C particles in a cross section perpendicular to the sputtering surface of the target is 35 ⁇ m or more, 3) One or more elements selected from B, Mg, Al, Si, Ti, Cr, Zr, Nb, Ta, Mn, Ag, Cu, Zn, W, Zr, Y as additive components to the nonmagnetic material The sputtering target according to 1) or 2) above, which contains 20 mol% or less of an oxide or nitride of 4) The sputter
  • the Fe—Pt sputtering target in which C particles are dispersed according to the present invention enables the production of a magnetic thin film of a thermally assisted magnetic recording medium without using an expensive simultaneous sputtering apparatus, and suppresses abnormal discharge during sputtering. Therefore, it has an excellent effect that generation of particles can be suppressed.
  • the present invention is a sintered sputtering target comprising an alloy having a composition of Pt of 5 to 60 mol% and the balance of Fe, and a nonmagnetic material dispersed in the alloy, wherein at least C is 5 to 5 as the nonmagnetic material.
  • the average particle area of C (carbon) particles in a cross section perpendicular to the sputtering surface of the sputtering target is 50 ⁇ m 2 or more.
  • the content of C is preferably 5 mol% or more and 60 mol% or less in the composition of the sputtering target.
  • the content of the C particles in the target composition is less than 5 mol%, good magnetic properties may not be obtained.
  • the content exceeds 60 mol%, it becomes difficult to disperse the C particles in the sintered body. In some cases, C particles are aggregated to generate more particles.
  • the Pt content is preferably 5 mol% or more and 60 mol% or less in the Fe—Pt alloy composition. If the content of Pt in the Fe—Pt alloy is less than 5 mol%, good magnetic properties may not be obtained, and if it exceeds 60 mol%, similarly good magnetic properties may not be obtained. is there.
  • the average particle area of the carbon (C) particles is 50 ⁇ m 2 or more in a cross section perpendicular to the sputtering surface of the sputtering target. Carbon particles that do not satisfy this requirement, that is, aggregates of carbon particles, cause abnormal discharge during sputtering and increase the amount of particles generated.
  • the average particle area of the carbon (C) particles is preferably 200 ⁇ m 2 or less. This is because too large carbon particles have the effect of hindering the movement of electrons in the sintered body and can cause abnormal discharge.
  • the average particle area of the carbon particles (C) in the horizontal section with respect to the sputtering surface of the target is preferably 220 ⁇ m 2 or less.
  • the average value of the peripheral lengths of the carbon particles in a cross section perpendicular to the sputtering surface of the target is 35 ⁇ m or more.
  • a sputtering target including an aggregate of carbon particles is not preferable because it significantly reduces the sputtering performance and deteriorates the quality and productivity of the film.
  • the average value of the peripheral length of the carbon particles is preferably 100 ⁇ m or less. This is because too large carbon particles have the effect of hindering the movement of electrons in the sintered body and can cause abnormal discharge.
  • the average value of the circumference of the carbon particles in the horizontal section with respect to the sputtering surface of the target is 55 ⁇ m or less.
  • the average particle area is determined by observing three arbitrary points on the polished surface (vertical cross section with respect to the sputter surface and horizontal cross section with respect to the sputter surface) of the end material from which the sputtering target has been cut. Is derived as an average value of values obtained by dividing the area by the number. Further, in the present invention, the average perimeter length is derived as an average value of values obtained by observing three arbitrary positions on the polished surface and dividing by the perimeter length of the observed C particles. For observation of the tissue, a laser microscope (VK-9710, manufactured by Keyence Corporation) was used. In order to distinguish C particles from the photographed tissue photograph from other phases, binary data was obtained using VK Analyzer (image analysis application). Was applied.
  • the binarization threshold the value set in the automatic mode of VK Analyzer is used as it is, and isolated points of 1 pixel or less are removed as noise. Furthermore, the binarized image was analyzed by the particle analysis function of VK Analyzer, and the above average particle area and average perimeter length were derived. It should be understood that an apparatus other than a laser microscope can be used for tissue observation, and such a case is also included in the present invention.
  • the sputtering target of the present invention is selected from B, Mg, Al, Si, Ti, Cr, Zr, Nb, Ta, Mn, Ag, Cu, Zn, W, Zr, and Y as an additive component to the nonmagnetic material. 20 mol% or less of oxides or nitrides of more than one element can be contained. This is because the oxide or nitride has a structure that insulates the magnetic interaction between the magnetic particles together with C, and good magnetic properties can be obtained in the magnetic thin film. In addition, from the viewpoint of suppressing the generation of particles during sputtering, it is desirable that the oxide be finely dispersed in the alloy as in the case of C.
  • the lower limit of the addition amount is preferably 0.1 mol%. This is because if it is less than the lower limit, it is difficult to obtain the effect of addition.
  • the sputtering target of the present invention contains 0.1 to 20 mol% of one or more metal elements selected from Au, Ag, Cu, B, Mn, Rh, Ir, and Ta as an additive component to the alloy. it can. This is because good magnetic properties can be obtained in the magnetic thin film.
  • the lower limit of the addition amount is preferably 0.1 mol%. This is because if it is less than the lower limit, it is difficult to obtain the effect of addition.
  • the upper limit of the addition amount is preferably 20 mol%. This is because if this upper limit is exceeded, good magnetic properties cannot be obtained.
  • a carbon raw material powder having a particle diameter of 5 ⁇ m or less and a fine powder content of 1% or less is preferably used.
  • the carbon powder having a small particle diameter has a high surface energy and thus easily forms an aggregate.
  • the particles in the aggregate are also difficult to bond. For this reason, when such aggregates are present in the sputtering target, abnormal discharge is generated from the starting point, and there is a problem that a large number of particles adhere to the magnetic thin film. Therefore, by removing the carbon powder having a small particle diameter at the raw material stage, formation of aggregates can be suppressed and sputtering abnormalities can be prevented.
  • the sputtering target of the present invention is produced by a powder sintering method.
  • each raw material powder Fe powder, Pt powder, C powder, powder of additive components as required
  • C powder it is desirable to use those powders having a particle size of 0.5 ⁇ m or more and 50 ⁇ m or less. If the particle size of the raw material powder is too small, there is a problem that the raw material powder is likely to aggregate. On the other hand, when the particle size of the raw material powder is large, it is difficult to finely disperse the C particles in the alloy.
  • Fe—Pt alloy powder may be used as the raw material powder.
  • the alloy powder containing Pt is effective for reducing the impurity gas component of the raw material powder, although it depends on its composition.
  • the C powder it is preferable to use a fine powder having a particle size of 5 ⁇ m or less and a content of 1% or less. More preferably, the content rate of the powder having a particle size of 10 ⁇ m or less is set to 10% or less. Since the C powder having a small particle size is particularly likely to form an aggregate, the formation of the aggregate due to the C particles in the target tissue is suppressed by separating and removing such a small C powder from the raw material powder in advance. be able to. This is an important point of the present invention.
  • the particle size distribution of the C powder used as a raw material and the average particle area of the carbon particles in the target, in the present invention, by making the particle size range of the C powder, in the cross section perpendicular to the sputtering surface of the sputtering target
  • the average particle area of the carbon particles can be 50 ⁇ m 2 or more.
  • the present invention only needs to be able to remove C powder having a small particle size so as to form an aggregate, and it is naturally understood that the present invention is included even when a means other than the airflow classification method is used. Should.
  • the above-mentioned powder is weighed so as to have a desired composition, and the raw material powder excluding the C powder is mixed for pulverization using a known method such as a ball mill. After adding the C powder previously weighed to the mixed powder thus obtained, classification is performed to separate and remove the powder having a small particle size.
  • the mixed powder is molded and sintered with a hot press. In addition to hot pressing, a plasma discharge sintering method or a hot isostatic pressing method can also be used. The temperature during sintering depends on the composition of the sputtering target, but in many cases, the temperature ranges from 800 to 1400 ° C.
  • isotropic hot pressing is performed on the sintered body taken out from the hot press.
  • Isotropic hot pressing is effective in improving the density of the sintered body.
  • the holding temperature during the isotropic hot pressing is in the temperature range of 800 to 1400 ° C., although it depends on the composition of the sintered body.
  • the applied pressure is set to 100 MPa or more.
  • the average particle area of the carbon particles in the section orthogonal to the sputtering surface of the target is not less 50 [mu] m 2 or more and, Fe-Pt-based sputtering target average particle area of the carbon particles in the horizontal section for sputter surface is 220 .mu.m 2 or less Can be produced. And the sputtering target of this invention produced in this way is useful for film-forming of the magnetic thin film of a thermally assisted magnetic recording medium.
  • Example 1 As a raw material powder, a C-powder (exfoliated graphite) having the particle size distribution shown in Table 1 was prepared by separating Fe-Pt alloy powder having an average particle size of 100 ⁇ m and small-diameter particles by airflow classification. The median diameter, particle size distribution, etc. shown in Table 1 were measured with a particle size distribution meter (model number: LA-920 manufactured by HORIBA). These powders were weighed with the following composition so that the total weight was 2600 g. Composition formula: 60 (50Fe-50Pt) -40C (mol%)
  • the Fe—Pt alloy powder was encapsulated in a ball mill pot with a capacity of 5 liters together with zirconia balls as a grinding medium, and rotated and ground for 4 hours.
  • the C powder weighed above was mixed with the Fe—Pt alloy powder taken out from the ball mill pot. Then, the sieve of 150 micrometers was passed 5 times and mixed.
  • this mixed powder was filled into a carbon mold and hot pressed.
  • the hot pressing conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and the pressure was increased from 30 MPa to the end of holding. After completion of the holding, it was naturally cooled in the chamber.
  • hot isostatic pressing HIP was applied to the sintered body taken out from the hot press mold.
  • the conditions for hot isothermal heating were as follows: the temperature rising rate was 300 ° C./hour, the holding temperature was 1350 ° C., and the holding time was 2 hours. Pressurization was performed at 150 MPa. After completion of the holding, it was naturally cooled in the furnace.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva) and subjected to sputtering.
  • the sputtering conditions were an input power of 1 kW and an Ar gas pressure of 1.7 Pa.
  • a film was formed on a 4-inch diameter silicon substrate for 20 seconds.
  • a surface foreign matter inspection device Surfscan 6420, manufactured by KLA-Tencor
  • Example 2 As a raw material powder, a C-powder (exfoliated graphite) having the particle size distribution shown in Table 1 was prepared by separating Fe-Pt alloy powder having an average particle size of 100 ⁇ m and small-diameter particles by airflow classification. The median diameter and particle size distribution shown in Table 1 were measured using the same method as in Example 1. These powders were weighed with the following composition so that the total weight was 2600 g. Composition formula: 60 (50Fe-50Pt) -40C (mol%)
  • the Fe—Pt alloy powder was encapsulated in a ball mill pot with a capacity of 5 liters together with zirconia balls as a grinding medium, and rotated and ground for 4 hours.
  • the C powder weighed above was mixed with the Fe—Pt alloy powder taken out from the ball mill pot. Then, the sieve of 150 micrometers was passed 5 times and mixed.
  • this mixed powder was filled into a carbon mold and hot pressed.
  • the hot pressing conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and the pressure was increased from 30 MPa to the end of holding. After completion of the holding, it was naturally cooled in the chamber.
  • hot isostatic pressing HIP was applied to the sintered body taken out from the hot press mold.
  • the conditions for hot isothermal heating were as follows: the temperature rising rate was 300 ° C./hour, the holding temperature was 1350 ° C., and the holding time was 2 hours. Pressurization was performed at 150 MPa. After completion of the holding, it was naturally cooled in the furnace.
  • tissue images were taken at a field size of 550 ⁇ m ⁇ 700 ⁇ m at three arbitrarily selected points on the vertical and horizontal cross sections with respect to the sputtering surface of the target. The results are shown in FIG. 3 (vertical section) and FIG. 4 (horizontal section). Then, the photographed image was binarized by image processing software, and the number, area, and perimeter of the portion corresponding to the C particles (the black portion of the tissue image) were obtained.
  • average particle area per C particles, in vertical section and a horizontal section for the sputtering surface 102.3Myuemu 2 were 199.5Myuemu 2 respectively.
  • the average value of the peripheral length of the particle per C particle was 48.0 ⁇ m and 50.7 ⁇ m, respectively, in the vertical and horizontal cross sections with respect to the sputtering surface.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva) and subjected to sputtering.
  • the sputtering conditions were an input power of 1 kW and an Ar gas pressure of 1.7 Pa.
  • a film was formed on a 4-inch diameter silicon substrate for 20 seconds.
  • the number of particles adhering to the substrate was measured with a surface foreign matter inspection apparatus (Surfscan 6420, manufactured by KLA-Tencor), and as a result, the number was clearly reduced to 200 as compared with Comparative Example 1 described later.
  • Comparative Example 1 As raw material powders, Fe—Pt alloy powder having an average particle size of 100 ⁇ m and C powder (exfoliated graphite) having the particle size distribution shown in Table 1 were prepared. In Comparative Example 1, no classification was performed. These powders were weighed with the following composition so that the total weight was 2600 g. Composition formula: 60 (50Fe-50Pt) -40C (mol%)
  • the Fe—Pt alloy powder was encapsulated in a ball mill pot with a capacity of 5 liters together with zirconia balls as a grinding medium, and rotated and ground for 4 hours.
  • the C powder weighed above was mixed with the Fe—Pt alloy powder taken out from the ball mill pot. Then, the sieve of 150 micrometers was passed 5 times and mixed.
  • this mixed powder was filled into a carbon mold and hot pressed.
  • the hot pressing conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and the pressure was increased from 30 MPa to the end of holding. After completion of the holding, it was naturally cooled in the chamber.
  • hot isostatic pressing HIP was applied to the sintered body taken out from the hot press mold.
  • the conditions for hot isothermal heating were as follows: the temperature rising rate was 300 ° C./hour, the holding temperature was 1350 ° C., and the holding time was 2 hours. Pressurization was performed at 150 MPa. After completion of the holding, it was naturally cooled in the furnace.
  • tissue images were taken at a field size of 550 ⁇ m ⁇ 700 ⁇ m at three arbitrarily selected points on the vertical and horizontal cross sections with respect to the sputtering surface of the target. The results are shown in FIG. 5 (vertical section) and FIG. 6 (horizontal section). Then, the photographed image was binarized by image processing software, and the number, area, and perimeter of the portion corresponding to the C particles (the black portion of the tissue image) were obtained.
  • average particle area per C particles, in vertical section and a horizontal section for the sputtering surface 46.3Myuemu 2, were 232.8Myuemu 2 respectively.
  • the average value of the peripheral length of the particle per C particle was 31.3 ⁇ m and 58.6 ⁇ m in the vertical and horizontal cross sections with respect to the sputtering surface, respectively.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva) and subjected to sputtering.
  • the sputtering conditions were an input power of 1 kW and an Ar gas pressure of 1.7 Pa.
  • a surface foreign matter inspection apparatus As a result of measuring the number of particles adhering to the substrate with a surface foreign matter inspection apparatus (Surfscan 6420, manufactured by KLA-Tencor), it was 450.
  • Example 3 As raw material powders, an Fe—Pt alloy powder having an average particle diameter of 100 ⁇ m, a C powder (exfoliated graphite) similar to that used in Example 2, and an Ag powder having an average particle diameter of 5 ⁇ m were prepared. These powders were weighed so as to have a total weight of 2600 g with the following composition. Composition formula: 60 (45Fe-45Pt-10Ag) -40C (mol%)
  • the Fe—Pt alloy powder was encapsulated in a ball mill pot with a capacity of 5 liters together with zirconia balls as a grinding medium, and rotated and ground for 4 hours. Then, the C powder and Ag powder weighed above were mixed with the Fe—Pt alloy powder taken out from the ball mill pot. Then, the sieve of 150 micrometers was passed 5 times and mixed.
  • this mixed powder was filled into a carbon mold and hot pressed.
  • the hot pressing conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurization was performed at 30 MPa from the start of heating to the end of holding. After completion of the holding, it was naturally cooled in the chamber.
  • hot isostatic pressing HIP was applied to the sintered body taken out from the hot press mold.
  • the conditions for hot isothermal heating were as follows: the temperature rising rate was 300 ° C./hour, the holding temperature was 950 ° C., the holding time was 2 hours, and the gas pressure of Ar gas was gradually increased from the start of the temperature rising. Pressurization was performed at 150 MPa. After completion of the holding, it was naturally cooled in the furnace.
  • tissue images were taken at a field size of 550 ⁇ m ⁇ 700 ⁇ m at three arbitrarily selected points on the vertical and horizontal cross sections with respect to the sputtering surface of the target. Then, the photographed image was binarized by image processing software, and the number, area, and perimeter of the portion corresponding to the C particles (the black portion of the tissue image) were obtained.
  • average particle area per C particles, in vertical section and a horizontal section for the sputtering surface 94.6Myuemu 2
  • 94.6Myuemu 2 94.6Myuemu 2
  • the average value of the peripheral length of the particle per C particle was 46.5 ⁇ m and 50.4 ⁇ m, respectively, in the vertical section and the horizontal section with respect to the sputtering surface.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe, and then attached to a magnetron sputtering apparatus and subjected to sputtering.
  • the sputtering conditions were the same as in Example 1, and a film was formed on a 4-inch diameter silicon substrate for 20 seconds.
  • the number of particles adhering to the substrate was measured with a surface foreign matter inspection apparatus. As a result, the number was clearly reduced compared with 30 in Comparative Example 2 described later.
  • Comparative Example 2 As raw material powders, an Fe—Pt alloy powder having an average particle diameter of 100 ⁇ m, a C powder (exfoliated graphite) similar to that used in Comparative Example 1, and an Ag powder having an average particle diameter of 5 ⁇ m were prepared. These powders were weighed so as to have a total weight of 2600 g with the following composition. Composition formula: 60 (45Fe-45Pt-10Ag) -40C (mol%)
  • the Fe—Pt alloy powder was encapsulated in a ball mill pot with a capacity of 5 liters together with zirconia balls as a grinding medium, and rotated and ground for 4 hours. Then, the C powder and Ag powder weighed above were mixed with the Fe—Pt alloy powder taken out from the ball mill pot. Then, the sieve of 150 micrometers was passed 5 times and mixed.
  • this mixed powder was filled into a carbon mold and hot pressed.
  • the hot pressing conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurization was performed at 30 MPa from the start of heating to the end of holding. After completion of the holding, it was naturally cooled in the chamber.
  • hot isostatic pressing HIP was applied to the sintered body taken out from the hot press mold.
  • the conditions for hot isothermal heating were as follows: the temperature rising rate was 300 ° C./hour, the holding temperature was 950 ° C., the holding time was 2 hours, and the gas pressure of Ar gas was gradually increased from the start of the temperature rising. Pressurization was performed at 150 MPa. After completion of the holding, it was naturally cooled in the furnace.
  • tissue images were taken at a field size of 550 ⁇ m ⁇ 700 ⁇ m at three arbitrarily selected points on the vertical and horizontal cross sections with respect to the sputtering surface of the target. Then, the photographed image was binarized by image processing software, and the number, area, and perimeter of the portion corresponding to the C particles (the black portion of the tissue image) were obtained.
  • average particle area per C particles, in vertical section and a horizontal section for the sputtering surface 43.8Myuemu 2, were 244.3Myuemu 2 respectively.
  • the average value of the circumference of the particle per C particle was 30.4 ⁇ m and 60.7 ⁇ m in the vertical and horizontal cross sections with respect to the sputtering surface, respectively.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe, and then attached to a magnetron sputtering apparatus and subjected to sputtering.
  • the sputtering conditions were the same as in Example 1, and the film was formed on a 4-inch diameter silicon substrate for 20 seconds. As a result of measuring the number of particles adhering to the substrate with the surface foreign matter inspection apparatus, it was 120.
  • Example 4 As raw material powder, Fe-Pt alloy powder having an average particle diameter of 100 ⁇ m, C powder (exfoliated graphite) similar to that used in Example 2, Cu powder having an average particle diameter of 5 ⁇ m, and SiO 2 powder having an average particle diameter of 1 ⁇ m. Prepared. These powders were weighed so as to have a total weight of 2600 g with the following composition. Composition formula: 65 (45Fe-45Pt-10Cu) -30C-5SiO 2 (mol%)
  • the Fe—Pt alloy powder was encapsulated in a ball mill pot with a capacity of 5 liters together with zirconia balls as a grinding medium, and pulverized by rotating for 4 hours. Then, the C powder, Cu powder, and SiO 2 powder weighed above were mixed with the Fe—Pt alloy powder taken out from the ball mill pot. Then, the sieve of 150 micrometers was passed 5 times and mixed.
  • this mixed powder was filled into a carbon mold and hot pressed.
  • the hot pressing conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1000 ° C., and a holding time of 2 hours, and pressurization was performed at 30 MPa from the start of heating to the end of holding. After completion of the holding, it was naturally cooled in the chamber.
  • hot isostatic pressing HIP was applied to the sintered body taken out from the hot press mold.
  • the conditions for hot isothermal heating were as follows: the temperature rising rate was 300 ° C./hour, the holding temperature was 950 ° C., the holding time was 2 hours, and the gas pressure of Ar gas was gradually increased from the start of the temperature rising. Pressurization was performed at 150 MPa. After completion of the holding, it was naturally cooled in the furnace.
  • tissue images were taken at a field size of 550 ⁇ m ⁇ 700 ⁇ m at three arbitrarily selected points on the vertical and horizontal cross sections with respect to the sputtering surface of the target. Then, the photographed image was binarized by image processing software, and the number, area, and perimeter of the portion corresponding to the C particles (the black portion of the tissue image) were obtained.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe, and then attached to a magnetron sputtering apparatus and subjected to sputtering.
  • the sputtering conditions were the same as in Example 1, and a film was formed on a 4-inch diameter silicon substrate for 20 seconds.
  • the number of particles adhering to the substrate was measured with a surface foreign matter inspection apparatus. As a result, the number was clearly reduced as compared with 12 in Comparative Example 3 described later.
  • Comparative Example 3 As raw material powders, Fe-Pt alloy powder having an average particle diameter of 100 ⁇ m, C powder (exfoliated graphite) similar to that used in Comparative Example 1, Cu powder having an average particle diameter of 5 ⁇ m, and SiO 2 powder having an average particle diameter of 1 ⁇ m were used. Prepared. These powders were weighed so as to have a total weight of 2600 g with the following composition. Composition formula: 65 (45Fe-45Pt-10Cu) -30C-5SiO 2 (mol%)
  • the Fe—Pt alloy powder was encapsulated in a ball mill pot with a capacity of 5 liters together with zirconia balls as a grinding medium, and pulverized by rotating for 4 hours. Then, the C powder, Cu powder and SiO 2 powder weighed above were mixed with the Fe—Pt—Cu alloy powder taken out from the ball mill pot. Then, the sieve of 150 micrometers was passed 5 times and mixed.
  • this mixed powder was filled into a carbon mold and hot pressed.
  • the hot pressing conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1000 ° C., and a holding time of 2 hours, and pressurization was performed at 30 MPa from the start of heating to the end of holding. After completion of the holding, it was naturally cooled in the chamber.
  • hot isostatic pressing HIP was applied to the sintered body taken out from the hot press mold.
  • the conditions for hot isothermal heating were as follows: the temperature rising rate was 300 ° C./hour, the holding temperature was 950 ° C., the holding time was 2 hours, and the gas pressure of Ar gas was gradually increased from the start of the temperature rising. Pressurization was performed at 150 MPa. After completion of the holding, it was naturally cooled in the furnace.
  • tissue images were taken at a field size of 550 ⁇ m ⁇ 700 ⁇ m at three arbitrarily selected points on the vertical and horizontal cross sections with respect to the sputtering surface of the target. Then, the photographed image was binarized by image processing software, and the number, area, and perimeter of the portion corresponding to the C particles (the black portion of the tissue image) were obtained.
  • average particle area per C particles, in vertical section and a horizontal section for the sputtering surface 44.8Myuemu 2, were 235.7Myuemu 2 respectively.
  • the average value of the peripheral length of the particles per C particle was 30.8 ⁇ m and 59.6 ⁇ m in the vertical and horizontal cross sections with respect to the sputtering surface, respectively.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe, and then attached to a magnetron sputtering apparatus and subjected to sputtering.
  • the sputtering conditions were the same as in Example 1, and the film was formed on a 4-inch diameter silicon substrate for 20 seconds. As a result of measuring the number of particles adhering to the substrate with the surface foreign matter inspection apparatus, it was 65.
  • Example 5 As raw material powder, Fe-Pt alloy powder having an average particle diameter of 100 ⁇ m, C powder (exfoliated graphite) similar to that used in Example 2, Au powder having an average particle diameter of 10 ⁇ m, and TiO 2 powder having an average particle diameter of 1 ⁇ m were used. Prepared. These powders were weighed so as to have a total weight of 2600 g with the following composition. Composition formula: 65 (45Fe-45Pt-10Au) -30C-5TiO 2 (mol%)
  • the Fe—Pt alloy powder was encapsulated in a ball mill pot with a capacity of 5 liters together with zirconia balls as a grinding medium, and pulverized by rotating for 4 hours. Then, the C powder, Au powder, and TiO 2 powder weighed above were mixed with the Fe—Pt alloy powder taken out from the ball mill pot. Then, the sieve of 150 micrometers was passed 5 times and mixed.
  • this mixed powder was filled into a carbon mold and hot pressed.
  • the hot pressing conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1000 ° C., and a holding time of 2 hours, and pressurization was performed at 30 MPa from the start of heating to the end of holding. After completion of the holding, it was naturally cooled in the chamber.
  • hot isostatic pressing HIP was applied to the sintered body taken out from the hot press mold.
  • the conditions for hot isothermal heating were as follows: the temperature rising rate was 300 ° C./hour, the holding temperature was 950 ° C., the holding time was 2 hours, and the gas pressure of Ar gas was gradually increased from the start of the temperature rising. Pressurization was performed at 150 MPa. After completion of the holding, it was naturally cooled in the furnace.
  • tissue images were taken at a field size of 550 ⁇ m ⁇ 700 ⁇ m at three arbitrarily selected points on the vertical and horizontal cross sections with respect to the sputtering surface of the target. Then, the photographed image was binarized by image processing software, and the number, area, and perimeter of the portion corresponding to the C particles (the black portion of the tissue image) were obtained.
  • average particle area per C particles, in vertical section and a horizontal section for the sputtering surface 101.0Myuemu 2 were 196.6Myuemu 2 respectively.
  • the average value of the peripheral length of the particles per C particle was 49.0 ⁇ m and 49.1 ⁇ m in the vertical and horizontal cross sections with respect to the sputtering surface, respectively.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe, and then attached to a magnetron sputtering apparatus and subjected to sputtering.
  • the sputtering conditions were the same as in Example 1, and a film was formed on a 4-inch diameter silicon substrate for 20 seconds. Then, the number of particles adhering to the substrate was measured with a surface foreign matter inspection apparatus. As a result, it was clearly reduced as compared with 22 and Comparative Example 3 described later.
  • Comparative Example 4 As raw material powders, Fe-Pt alloy powder having an average particle diameter of 100 ⁇ m, C powder (exfoliated graphite) similar to that used in Comparative Example 1, Au powder having an average particle diameter of 10 ⁇ m, and TiO 2 powder having an average particle diameter of 1 ⁇ m were used. Prepared. These powders were weighed so as to have a total weight of 2600 g with the following composition. Composition formula: 65 (45Fe-45Pt-10Au) -30C-5TiO 2 (mol%)
  • the Fe—Pt alloy powder was encapsulated in a ball mill pot with a capacity of 5 liters together with zirconia balls as a grinding medium, and pulverized by rotating for 4 hours. Then, the C powder, Au powder, and TiO 2 powder weighed above were mixed with the Fe—Pt alloy powder taken out from the ball mill pot. Then, the sieve of 150 micrometers was passed 5 times and mixed.
  • this mixed powder was filled into a carbon mold and hot pressed.
  • the hot pressing conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1000 ° C., and a holding time of 2 hours, and pressurization was performed at 30 MPa from the start of heating to the end of holding. After completion of the holding, it was naturally cooled in the chamber.
  • hot isostatic pressing HIP was applied to the sintered body taken out from the hot press mold.
  • the conditions for hot isothermal heating were as follows: the temperature rising rate was 300 ° C./hour, the holding temperature was 950 ° C., the holding time was 2 hours, and the gas pressure of Ar gas was gradually increased from the start of the temperature rising. Pressurization was performed at 150 MPa. After completion of the holding, it was naturally cooled in the furnace.
  • tissue images were taken at a field size of 550 ⁇ m ⁇ 700 ⁇ m at three arbitrarily selected points on the vertical and horizontal cross sections with respect to the sputtering surface of the target. Then, the photographed image was binarized by image processing software, and the number, area, and perimeter of the portion corresponding to the C particles (the black portion of the tissue image) were obtained.
  • average particle area per C particles, in vertical section and a horizontal section for the sputtering surface, 45.1Myuemu 2 were 236.8Myuemu 2 respectively.
  • the average value of the peripheral length of the particle per C particle was 30.5 ⁇ m and 57.9 ⁇ m in the vertical and horizontal cross sections with respect to the sputtering surface, respectively.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe, and then attached to a magnetron sputtering apparatus and subjected to sputtering.
  • the sputtering conditions were the same as in Example 1, and the film was formed on a 4-inch diameter silicon substrate for 20 seconds. As a result of measuring the number of particles adhering to the substrate with the surface foreign matter inspection apparatus, it was 80.
  • the C particles were not aggregated into a large lump in the target structure, and were uniformly and finely dispersed. And when sputtering was performed using the target provided with such a structure
  • the present invention makes it possible to form a magnetic thin film of a heat-assisted magnetic recording medium without using an expensive simultaneous sputtering apparatus, and further reduces the amount of particles generated during sputtering and reduces the aggregation of C particles. It has an excellent effect of providing a Pt-based sputtering target. Therefore, it is useful as a sputtering target for forming a magnetic thin film of a heat-assisted magnetic recording medium.

Landscapes

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

Abstract

La présente invention concerne une cible de pulvérisation d'objet fritté comprenant un alliage ayant une composition contenant de 5 à 60 % en moles de Pt, le complément étant constitué de Fe, et de matières non magnétiques dispersées dans l'alliage, la cible de pulvérisation étant caractérisée en ce que les matières non magnétiques comprennent au moins du C à hauteur de 5 à 60 % en moles et en ce que les grains de C présents dans une section transversale perpendiculaire à la surface de pulvérisation de la cible ont une surface moyenne des grains supérieure ou égale à 50 μm2. La cible de pulvérisation permet de produire le film mince magnétique du support d'enregistrement magnétique thermoassisté sans avoir besoin d'utiliser de dispositif couteux de pulvérisation simultanée, et génère peu de particules pendant la pulvérisation.
PCT/JP2014/061594 2013-04-26 2014-04-24 Cible de pulvérisation pour film d'enregistrement magnétique, et matière carbonée brute destinée à être utilisée dans la production de celle-ci WO2014175392A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
SG11201506097YA SG11201506097YA (en) 2013-04-26 2014-04-24 Sputtering target for magnetic recording film, and raw carbon material for use in producing same
JP2014530046A JP5876155B2 (ja) 2013-04-26 2014-04-24 磁気記録膜用スパッタリングターゲット及びその製造に用いる炭素原料
CN201480006305.1A CN104955981B (zh) 2013-04-26 2014-04-24 磁记录膜用溅射靶及用于制造该溅射靶的碳原料

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2013-094300 2013-04-26
JP2013094300 2013-04-26

Publications (1)

Publication Number Publication Date
WO2014175392A1 true WO2014175392A1 (fr) 2014-10-30

Family

ID=51791958

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2014/061594 WO2014175392A1 (fr) 2013-04-26 2014-04-24 Cible de pulvérisation pour film d'enregistrement magnétique, et matière carbonée brute destinée à être utilisée dans la production de celle-ci

Country Status (6)

Country Link
JP (1) JP5876155B2 (fr)
CN (1) CN104955981B (fr)
MY (1) MY175409A (fr)
SG (1) SG11201506097YA (fr)
TW (1) TWI595103B (fr)
WO (1) WO2014175392A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017154741A1 (fr) * 2016-03-07 2017-09-14 田中貴金属工業株式会社 Cible de pulvérisation à base de fept-c
JP7483999B1 (ja) 2023-09-22 2024-05-15 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組立品

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021085410A1 (fr) * 2019-11-01 2021-05-06 田中貴金属工業株式会社 Cible de pulvérisation pour support d'enregistrement magnétique à assistance thermique

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012086335A1 (fr) * 2010-12-20 2012-06-28 Jx日鉱日石金属株式会社 Cible de pulvérisation cathodique fe-pt avec dispersion de particules de c
WO2012133166A1 (fr) * 2011-03-30 2012-10-04 Jx日鉱日石金属株式会社 Cible de pulvérisation pour pellicule d'enregistrement magnétique
JP2012214874A (ja) * 2011-03-30 2012-11-08 Tanaka Kikinzoku Kogyo Kk ＦｅＰｔ−Ｃ系スパッタリングターゲット及びその製造方法
JP2012252768A (ja) * 2011-05-09 2012-12-20 Mitsubishi Materials Corp 磁気記録媒体膜形成用スパッタリングターゲットおよびその製造方法

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000012020A (ja) * 1998-06-23 2000-01-14 Nippon Steel Corp リチウム二次電池負極用炭素材料
US20070189916A1 (en) * 2002-07-23 2007-08-16 Heraeus Incorporated Sputtering targets and methods for fabricating sputtering targets having multiple materials
KR100470151B1 (ko) * 2002-10-29 2005-02-05 한국과학기술원 ＦｅＰｔＣ 박막을 이용한 고밀도 자기기록매체 및 그제조방법
JP5428561B2 (ja) * 2009-06-16 2014-02-26 株式会社Ｇｓユアサ 直接形燃料電池システム及びその運転停止方法
JP5678414B2 (ja) * 2009-06-17 2015-03-04 三菱化学株式会社 黒鉛負極材料及びその製造方法、並びにそれを用いたリチウム二次電池用負極及びリチウム二次電池

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012086335A1 (fr) * 2010-12-20 2012-06-28 Jx日鉱日石金属株式会社 Cible de pulvérisation cathodique fe-pt avec dispersion de particules de c
WO2012133166A1 (fr) * 2011-03-30 2012-10-04 Jx日鉱日石金属株式会社 Cible de pulvérisation pour pellicule d'enregistrement magnétique
JP2012214874A (ja) * 2011-03-30 2012-11-08 Tanaka Kikinzoku Kogyo Kk ＦｅＰｔ−Ｃ系スパッタリングターゲット及びその製造方法
JP2012252768A (ja) * 2011-05-09 2012-12-20 Mitsubishi Materials Corp 磁気記録媒体膜形成用スパッタリングターゲットおよびその製造方法

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017154741A1 (fr) * 2016-03-07 2017-09-14 田中貴金属工業株式会社 Cible de pulvérisation à base de fept-c
JP6383510B2 (ja) * 2016-03-07 2018-08-29 田中貴金属工業株式会社 ＦｅＰｔ−Ｃ系スパッタリングターゲット
JPWO2017154741A1 (ja) * 2016-03-07 2018-10-04 田中貴金属工業株式会社 ＦｅＰｔ−Ｃ系スパッタリングターゲット
CN108699679A (zh) * 2016-03-07 2018-10-23 田中贵金属工业株式会社 FePt-C系溅射靶
TWI675926B (zh) * 2016-03-07 2019-11-01 日商田中貴金屬工業股份有限公司 ＦｅＰｔ－Ｃ系濺鍍靶
US10787732B2 (en) 2016-03-07 2020-09-29 Tanaka Kikinzoku Kogyo K.K. FePt-C-based sputtering target
CN108699679B (zh) * 2016-03-07 2020-09-29 田中贵金属工业株式会社 FePt-C系溅射靶
JP7483999B1 (ja) 2023-09-22 2024-05-15 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組立品

Also Published As

Publication number Publication date
CN104955981A (zh) 2015-09-30
MY175409A (en) 2020-06-24
SG11201506097YA (en) 2015-09-29
JP5876155B2 (ja) 2016-03-02
CN104955981B (zh) 2018-01-23
TW201508074A (zh) 2015-03-01
TWI595103B (zh) 2017-08-11
JPWO2014175392A1 (ja) 2017-02-23

Similar Documents

Publication Publication Date Title
US10937455B2 (en) Fe—Pt based magnetic material sintered compact
TWI547579B (zh) Fe-Pt sputtering target with dispersed C particles
TWI550114B (zh) Ｆｅ－Ｐｔ－Ｃ系濺鍍靶
JP5457615B1 (ja) 磁気記録膜形成用スパッタリングターゲット及びその製造方法
JP5587495B2 (ja) Ｃ粒子が分散したＦｅ−Ｐｔ系スパッタリングターゲット
JP6285043B2 (ja) 磁気記録膜形成用スパッタリングターゲット及びその製造方法
JP5913620B2 (ja) Ｆｅ−Ｐｔ系焼結体スパッタリングターゲット及びその製造方法
WO2012133166A1 (fr) Cible de pulvérisation pour pellicule d'enregistrement magnétique
JP6084711B2 (ja) 磁気記録膜形成用スパッタリングターゲット及びその製造方法
JP5876155B2 (ja) 磁気記録膜用スパッタリングターゲット及びその製造に用いる炭素原料
JP6305881B2 (ja) 磁気記録媒体用スパッタリングターゲット
JP7005647B2 (ja) スパッタリングターゲット及びその製造方法、並びに磁気記録媒体の製造方法
WO2018123500A1 (fr) Cible de pulvérisation de matériau magnétique et procédé de production de ladite cible
WO2017141558A1 (fr) Cible de pulvérisation pour support d'enregistrement magnétique, et film mince magnétique
JP6484276B2 (ja) 磁気記録膜形成用スパッタリングターゲット及びその製造方法
JP6062586B2 (ja) 磁気記録膜形成用スパッタリングターゲット

Legal Events

Date Code Title Description
ENP Entry into the national phase

Ref document number: 2014530046

Country of ref document: JP

Kind code of ref document: A

121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 14787898

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 14787898

Country of ref document: EP

Kind code of ref document: A1