WO2014171161A1 - Cible de pulvérisation cathodique - Google Patents

Cible de pulvérisation cathodique Download PDF

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Publication number
WO2014171161A1
WO2014171161A1 PCT/JP2014/051970 JP2014051970W WO2014171161A1 WO 2014171161 A1 WO2014171161 A1 WO 2014171161A1 JP 2014051970 W JP2014051970 W JP 2014051970W WO 2014171161 A1 WO2014171161 A1 WO 2014171161A1
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phase
sputtering target
powder
sputtering
atomic ratio
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PCT/JP2014/051970
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English (en)
Japanese (ja)
Inventor
佐藤　敦
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Jx日鉱日石金属株式会社
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Priority to JP2015512326A priority Critical patent/JP5944580B2/ja
Priority to SG11201506140WA priority patent/SG11201506140WA/en
Publication of WO2014171161A1 publication Critical patent/WO2014171161A1/fr

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    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
    • G11B5/851—Coating a support with a magnetic layer by sputtering
    • 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
    • C22C1/0466—Alloys based on noble metals
    • 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
    • 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 forming a magnetic thin film in a magnetic recording medium.
  • materials based on Co, Fe, or Ni which are ferromagnetic metals, are used as materials for magnetic thin films of magnetic recording media.
  • a Co—Cr-based or Co—Cr—Pt-based ferromagnetic alloy containing Co as a main component has been used for a magnetic thin film of a hard disk employing an in-plane magnetic recording method.
  • a composite material composed of a Co—Cr—Pt-based ferromagnetic alloy mainly composed of Co and an oxide is often used for a magnetic thin film of a hard disk adopting a perpendicular magnetic recording system that has been put into practical use in recent years.
  • the above-mentioned magnetic thin film is often produced by sputtering a sputtering target containing the above material as a component with a magnetron sputtering apparatus because of its high productivity.
  • the recording density of the hard disk is increasing rapidly year by year and is exceeding 1 Tbit / in 2 .
  • the size of the recording bit becomes less than 10 nm, and in that case, superparamagnetization due to thermal fluctuation is expected to be a problem.
  • materials for magnetic recording media currently used for example, materials in which Pt is added to a Co-based alloy to increase the magnetocrystalline anisotropy are 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.
  • L1 0 with Fe-Pt alloy has a high crystalline magnetic anisotropy having the structure, because of its excellent corrosion resistance, oxidation resistance, is what is expected as a material suitable for the application as a magnetic recording medium.
  • Fe-Pt film formed by the sputtering method is a disordered phase of a metastable phase, in order to express the L1 0 structure is an ordered phase, it is necessary to heat treatment at ordering temperature. Since this ordering temperature is high, the problem of heat resistance of the substrate occurs. Therefore, attempts have been made to lower the ordering temperature by adding Ag or Cu to the Fe—Pt alloy.
  • such a magnetic thin film having a granular structure is often produced by preparing a target made of each material and co-sputtering.
  • a target made of each material and co-sputtering.
  • the co-sputtering apparatus is expensive and the apparatus itself is large, it is common to produce a magnetic thin film using an integrated sputtering target made of an Fe—Pt alloy and a nonmagnetic material during mass production.
  • Such a target is produced by a powder sintering method.
  • An object of the present invention is to provide a sputtering target composed of an Fe—Pt alloy and Ag and C in which the amount of particles generated during sputtering is greatly reduced.
  • the present inventors have conducted intensive research. As a result, the amount of particles generated during sputtering can be significantly reduced by adjusting the composition and structure of the sputtering target. I found out.
  • the target cross section or cut surface described later is perpendicular to the sputtering surface. It means a cross section.
  • a sputtering target composed of an Fe—Pt alloy phase, an Ag phase, and a C phase, and the value obtained by dividing the atomic ratio of C by the atomic ratio of Ag in the composition of the entire sputtering target is 4 or more and 10 or less.
  • the Ag phase is included in all virtual circles having a radius of 10 ⁇ m drawn around an arbitrary point in the Ag phase, or at least two points between the virtual circle and the outer periphery of the Ag phase
  • a sputtering target characterized by having a shape having the above-mentioned contact or intersection 2) The sputtering target according to 1) above, wherein the area ratio of the C phase in the cross section of the sputtering target is 10% or more and 45% or less, 3)
  • the Ag phase is included in all virtual circles having a radius of 10 ⁇ m drawn around an arbitrary point in the Ag phase, or between the virtual circle and the outer pe
  • a sputtering target comprising a shape having at least two contact points or intersections 4)
  • the oxide phase is Al, B, Ba, Be, Bi, Ca, Ce, Co, Cr, Cs, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Ho, La, Li , Lu, Mg, Mo, Nb, Nd, Ni, Pr, Sb, Sc, Si, Sm, Sn, Sr, Ta, Tb, Te, Ti, Tm, V, W, Y, Yb, Zn, Zr
  • the present invention it is possible to provide a sputtering target in which the amount of particles generated during sputtering is greatly reduced. Therefore, it has the outstanding effect that the yield at the time of sputtering film formation can be improved.
  • the sputtering target of the present invention is characterized by comprising an Fe—Pt alloy phase, an Ag phase, and a C phase.
  • the Fe—Pt alloy phase means an alloy containing Fe and Pt as main components, and not only a binary alloy containing only Fe and Pt but also Fe and Pt as main components,
  • a ternary or higher alloy containing a metal element other than Pt is also included. Examples of ternary or higher alloys include Fe—Pt—Cu.
  • the sputtering target of the present invention is characterized in that the value obtained by dividing the atomic ratio of C by the atomic ratio of Ag in the composition of the entire sputtering target is 4 or more and 10 or less.
  • the Ag phase has an effect of suppressing the loss of C on the surface of the target during sputtering, and the generation of particles can be remarkably suppressed. According to the study by the present inventors, it is clear that the effect of suppressing the generation of particles is greatly reduced when the value obtained by dividing the atomic ratio of C by the atomic ratio of Ag is less than 4. . On the other hand, when this value is larger than 10, although there is an effect of suppressing the generation of particles, Ag may be segregated in the sputtered film, which may impair the magnetic properties of the magnetic thin film.
  • the Ag phase is included in all virtual circles having a radius of 10 ⁇ m drawn around an arbitrary point in the Ag phase, or between the virtual circle and the outer periphery of the Ag phase. It is characterized by having a shape having at least two or more contacts or intersections between them. This feature means that there is almost no coarse Ag phase in the target structure.
  • a coarse Ag phase is present in the target structure, Ag having a high sputter rate is selectively sputtered, resulting in a problem that the smoothness of the sputter surface is impaired and the amount of particles increases.
  • the effect of the present invention can be obtained if the area ratio is less than 20% with respect to the total area of the Ag phase.
  • the area ratio of C phase is 10% or more and 45% or less in the cross section of the sputtering target of this invention.
  • the area ratio of the C phase is less than 10%, C cannot sufficiently insulate the magnetic interaction between the magnetic particles in the sputtered film, so that good magnetic properties may not be obtained.
  • it is larger than 45% C may aggregate and a coarse C phase may be generated in the target structure, resulting in increased generation of particles.
  • the area ratio of the C phase is preferably obtained from the average of a plurality of cross sections having a total of about 1 mm 2 in order to reduce variation due to the observation location.
  • the sputtering target of the present invention can further contain an oxide phase in a structure composed of an Fe—Pt alloy phase, an Ag phase, and a C phase.
  • the oxide phase is effective in insulating the magnetic interaction between the magnetic particles in the sputtered film in the same manner as C.
  • An oxide containing one or more selected elements as constituent components can be given. These can be arbitrarily selected according to the desired magnetic properties.
  • the sum total of the area ratio of C phase and an oxide phase in the sputtering target containing the said oxide phase shall be 10% or more and 45% or less. If the total area ratio of the C phase and the oxide phase is less than 10%, the C and oxide cannot sufficiently insulate the magnetic interaction between the magnetic particles in the sputtered film, so that good magnetic properties are obtained. It may not be obtained. On the other hand, if it is larger than 45%, C and oxides may aggregate to produce coarse C and oxide phases in the target, resulting in increased generation of particles.
  • the area ratio between the C phase and the oxide phase is preferably obtained from an average of a plurality of cross sections having a total of about 1 mm 2 in order to reduce variation depending on the observation location.
  • the sputtering target of the present invention is selected from Au, B, Co, Cr, Cu, Ga, Ge, Mn, Mo, Nb, Ni, Pd, Re, Rh, Ru, Sn, Ta, W, V, and Zn. It is preferable to contain one or more metal elements.
  • the content is preferably 0.5 to 15% in terms of the number of atoms in the metal component. These additive metals are those which primarily added to reduce the temperature of the heat treatment for the expression of the L1 0 structure. When the content is less than 0.5%, it is difficult to obtain the above effect. On the other hand, when the content is more than 15%, the magnetic properties of the magnetic thin film may be impaired.
  • the sputtering target of the present invention is produced by a powder sintering method.
  • a powder sintering method For example, it can be produced by the following method.
  • the average particle size of the metal powder is more than 10 ⁇ m, the C phase and the oxide phase may not be uniformly dispersed, and when it is less than 1 ⁇ m, the influence of the oxidation of the metal powder may be a problem. is there.
  • this particle size range is a preferable condition, and exceeding this range does not deny the present invention.
  • Some Ag powders have strong cohesiveness depending on the particle size and shape, and in that case, it is preferable to use those that have been subjected to a coating treatment for preventing aggregation.
  • C powder having an average particle size of 1 to 30 ⁇ m When the average particle size is 1 to 30 ⁇ m, C powders hardly aggregate when mixed with metal powder, and the C phase can be uniformly dispersed. However, this particle size range is a preferable condition, and exceeding this range does not deny the present invention.
  • Types of C powder include those having a crystal structure such as graphite (graphite) and nanotubes and amorphous ones typified by carbon black, and any C powder may be used.
  • oxide powder having an average particle size of 0.2 to 5 ⁇ m.
  • the average particle size is 0.2 to 5 ⁇ m, there is an advantage that uniform mixing with the metal powder becomes easy.
  • the average particle size of the oxide powder is more than 5 ⁇ m, a coarse oxide phase may be produced after sintering, and if it is less than 0.2 ⁇ m, the oxide powder may be aggregated. .
  • this particle size range is a preferable condition, and exceeding this range does not deny the present invention.
  • the above raw material powder is weighed so as to have a desired composition, and mixed using a known method such as a ball mill also for pulverization. At this time, it is desirable to contain an inert gas in the pulverization vessel to suppress oxidation of the raw material powder.
  • the mixed powder thus obtained is molded and sintered by a hot press method in a vacuum atmosphere or an inert gas atmosphere.
  • various pressure sintering methods such as a plasma discharge sintering method can be used.
  • the hot isostatic pressing is effective for improving the density of the sintered body.
  • the holding temperature at the time of sintering depends on the constituent components of the target, in many cases, it is preferably in the temperature range of 500 to 950 ° C.
  • the Ag phase is smaller than all the virtual circles having a radius of 10 ⁇ m drawn around an arbitrary point in the Ag phase in the cross section of the target, or at least two or more points between the virtual circle and the outer periphery of the Ag phase.
  • the sputtering target of the present invention can be produced.
  • the sputtering target manufactured in this way can reduce the amount of particles generated during sputtering, and thus has an excellent effect of improving the yield during film formation.
  • Example 1 Fe powder having an average particle size of 3 ⁇ m, Pt powder having an average particle size of 3 ⁇ m, Ag powder having an average particle size of 2 ⁇ m, and C powder (graphite powder) having an average particle size of 10 ⁇ m were prepared as raw material powders.
  • As the Ag powder a powder coated with an organic material for preventing aggregation was used. And it weighed so that the total weight might be 2500g with the following composition ratios. Weighing composition (molar fraction): 30Fe-30Pt-5Ag-35C
  • the weighed powder was sealed in a 10-liter ball mill pot together with zirconia balls as a grinding medium in an Ar atmosphere, and rotated and mixed for 4 hours. Then, the powder taken out from the pot was filled in a carbon mold and molded and sintered using a hot press apparatus.
  • the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 900 ° 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. In addition, after the holding, it was naturally cooled in the chamber as it was.
  • a part of the sintered body thus produced was cut out, and the cut surface was polished and observed with an electron probe microanalyzer (EPMA).
  • EPMA electron probe microanalyzer
  • 80% or more of the Ag phase in terms of area ratio is included in all virtual circles having a radius of 10 ⁇ m drawn around an arbitrary point in the Ag phase. It was also confirmed that a shape having at least two contact points or intersections between the virtual circle and the outer periphery of the Ag phase was provided.
  • the area ratio of the C phase from an image obtained by observing the range of 1 mm 2 with an optical microscope, it was 25.5%.
  • composition analysis was performed using small pieces collected from the sintered body.
  • Fe, Pt, and Ag were measured using an ICP-AES apparatus, and C was measured using a carbon analyzer employing a high frequency induction furnace combustion-infrared absorption method.
  • the value obtained by dividing the atomic ratio of C by the atomic ratio of Ag was 6.9.
  • 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 to produce a disk-shaped target.
  • This was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva) and sputtering was performed.
  • 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 particle counter. As a result, the number of particles was 83.
  • the weighed powder was enclosed in a 10-liter ball mill pot together with zirconia balls as a grinding medium in an Ar atmosphere, and rotated and mixed for 4 hours. Then, the powder taken out from the pot was filled in a carbon mold and molded and sintered using a hot press apparatus.
  • the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 900 ° 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.
  • composition analysis was performed using small pieces collected from the sintered body.
  • Fe, Pt, and Ag were measured using an ICP-AES apparatus, and C was measured using a carbon analyzer employing a high frequency induction furnace combustion-infrared absorption method.
  • the atomic ratio was calculated from the weight ratio thus obtained, and the atomic ratio of C was divided by the atomic ratio of Ag to be 18.5. This value deviated from the range specified in the claims of this application.
  • 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 to produce a disk-shaped target.
  • This was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed under the same conditions as in Example 1.
  • the number of particles was 561, which was significantly larger than that of Example 1.
  • Comparative Example 2 Fe powder having an average particle size of 3 ⁇ m, Pt powder having an average particle size of 3 ⁇ m, Ag powder having an average particle size of 30 ⁇ m, and C powder (graphite powder) having an average particle size of 10 ⁇ m were prepared as raw material powders. And it weighed so that the total weight might be 2500g with the following composition ratios. Weighing composition (molar fraction): 30Fe-30Pt-5Ag-35C
  • the weighed powder was sealed in a 10-liter ball mill pot together with zirconia balls as a grinding medium in an Ar atmosphere, and rotated and mixed for 4 hours. Then, the powder taken out from the pot was filled in a carbon mold and molded and sintered using a hot press apparatus.
  • the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 960 ° 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.
  • a part of the sintered body thus produced was cut out, its cross section was polished, and observed with an electron beam probe microanalyzer.
  • a structure in which the Fe—Pt alloy phase, Ag phase, and C phase were uniformly dispersed with each other was obtained.
  • a coarse Ag phase is observed, and the Ag phase is included in all virtual circles having a radius of 10 ⁇ m drawn around an arbitrary point in the phase or the virtual phase It was confirmed that those having no shape having at least two contact points or intersections between the circle and the outer periphery of the Ag phase were present in an area ratio of 20% or more with respect to the total area of the Ag phase.
  • composition analysis was performed using small pieces collected from the sintered body.
  • Fe, Pt, and Ag were measured using an ICP-AES apparatus, and C was measured using a carbon analyzer employing a high frequency induction furnace combustion-infrared absorption method.
  • the atomic ratio was calculated from the weight ratio thus obtained, and the atomic ratio of C divided by the atomic ratio of Ag was 7.0.
  • 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 to produce a disk-shaped target.
  • This was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed under the same conditions as in Example 1.
  • the number of particles was 245, which was larger than that of Example 1.
  • the weighed powder was sealed with Ar in a 10-liter ball mill pot together with zirconia balls as a grinding medium, and mixed and pulverized by rotating for 4 hours. Then, the powder taken out from the pot was filled in a carbon mold, and molded and sintered using a hot press apparatus.
  • the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 900 ° 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.
  • composition analysis was performed using small pieces collected from the sintered body.
  • Fe, Pt, and Ag were measured using an ICP-AES apparatus, and C was measured using an oxygen analyzer employing an inert gas melting-infrared absorption method.
  • an oxygen analyzer employing an inert gas melting-infrared absorption method.
  • 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 to produce a disk-shaped target.
  • This was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed under the same conditions as in Example 1.
  • the number of particles was 880, which was significantly increased from that in Example 1.
  • Example 2 Fe powder having an average particle diameter of 3 ⁇ m, Pt powder having an average particle diameter of 3 ⁇ m, Ag powder having an average particle diameter of 2 ⁇ m, C powder (graphite powder) having an average particle diameter of 10 ⁇ m, and SiO 2 powder having an average particle diameter of 1 ⁇ m were prepared as raw material powders. .
  • As the Ag powder a powder coated with an organic material for preventing aggregation was used. And it weighed so that the total weight might be 2200g with the following composition ratios. Weighing composition (molar fraction): 30Fe-30Pt-5Ag-30C-5SiO 2
  • the weighed powder was enclosed in a 10-liter ball mill pot together with zirconia balls as a grinding medium in an Ar atmosphere, and rotated and mixed for 4 hours.
  • the powder taken out from the pot was filled in a carbon mold and molded and sintered using a hot press apparatus.
  • the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 900 ° 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.
  • composition analysis was performed using small pieces collected from the sintered body.
  • Fe, Pt, Ag, and Si are measured using an ICP-AES apparatus, C is measured using a carbon analyzer employing a high frequency induction furnace combustion-infrared absorption method, and O is an inert gas melting-infrared absorption method.
  • the measurement was performed with the employed oxygen analyzer.
  • the atomic ratio was calculated from the weight ratio thus obtained, and the atomic ratio of C divided by the atomic ratio of Ag was 6.0.
  • 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 to produce a disk-shaped target.
  • This was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed under the same conditions as in Example 1. As a result, the number of particles was 34.
  • the weighed powder was sealed in a 10-liter ball mill pot together with zirconia balls as a grinding medium in an Ar atmosphere, and rotated and mixed for 4 hours.
  • the powder taken out from the pot was filled in a carbon mold and molded and sintered using a hot press apparatus.
  • the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 900 ° 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.
  • composition analysis was performed using small pieces collected from the sintered body.
  • Fe, Pt, Ag, and Si are measured using an ICP-AES apparatus, C is measured using a carbon analyzer employing a high frequency induction furnace combustion-infrared absorption method, and O is an inert gas melting-infrared absorption method.
  • the measurement was performed with the employed oxygen analyzer.
  • the atomic ratio was calculated from the weight ratio thus obtained, and the atomic ratio of C divided by the atomic ratio of Ag was 13.9. This value deviated from the range specified in the claims of this application.
  • 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 to produce a disk-shaped target.
  • This was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed under the same conditions as in Example 2.
  • the number of particles was 189, which was significantly larger than that of Example 2.
  • the weighed powder was sealed with Ar in a 10-liter ball mill pot together with zirconia balls as a grinding medium, and mixed and pulverized by rotating for 4 hours. Then, the powder taken out from the pot was filled in a carbon mold, and molded and sintered using a hot press apparatus.
  • the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 900 ° 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.
  • the Fe—Pt alloy phase, the Ag phase, the C phase, and the oxide phase (SiO 2 ) were mutually in contact.
  • a uniformly dispersed structure was confirmed.
  • 80% or more of the Ag phase in terms of area ratio is included in all virtual circles having a radius of 10 ⁇ m formed around an arbitrary point in the Ag phase.
  • a shape having at least two contact points or intersections was provided between the virtual circle and the outer periphery of the Ag phase.
  • the total area ratio of the C phase and the oxide phase was determined from an image obtained by observing the range of 1 mm 2 with an optical microscope, and as a result, it was 47.4%. This value deviated from the range specified in the claims of this application.
  • composition analysis was performed using small pieces collected from the sintered body.
  • Fe, Pt, Ag, and Si are measured using an ICP-AES apparatus, C is measured using a carbon analyzer employing a high frequency induction furnace combustion-infrared absorption method, and O is an inert gas melting-infrared absorption method.
  • the measurement was performed with the employed oxygen analyzer.
  • the atomic ratio of C was divided by the atomic ratio of Ag to be 7.9.
  • 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 to produce a disk-shaped target.
  • This was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed under the same conditions as in Example 1.
  • the number of particles was 716, which was significantly larger than that of Example 1.
  • Example 3 Fe powder having an average particle size of 3 ⁇ m, Pt powder having an average particle size of 3 ⁇ m, Ag powder having an average particle size of 2 ⁇ m, Cu powder having an average particle size of 3 ⁇ m, Co powder having an average particle size of 3 ⁇ m, and C powder having an average particle size of 10 ⁇ m (Graphite powder) was prepared.
  • As the Ag powder a powder coated with an organic material for preventing aggregation was used. And it weighed so that the total weight might be 2200g with the following composition ratios. Weighing composition (molar fraction): 26Fe-26Pt-6Cu-5Co-7Ag-30C
  • the weighed powder was enclosed in a 10-liter ball mill pot together with zirconia balls as a grinding medium in an Ar atmosphere, and rotated and mixed for 4 hours.
  • the powder taken out from the pot was filled in a carbon mold and molded and sintered using a hot press apparatus.
  • the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 900 ° 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.
  • a part of the sintered body thus produced was cut out, and the cut surface was polished and observed with an electron probe microanalyzer (EPMA).
  • EPMA electron probe microanalyzer
  • a structure in which the Fe—Pt—Cu—Co alloy phase, the Ag phase, and the C phase were uniformly dispersed was confirmed.
  • 80% or more of the Ag phase in terms of area ratio is included in all virtual circles having a radius of 10 ⁇ m formed around an arbitrary point in the Ag phase, or It was confirmed that a shape having at least two contact points or intersections was provided between the virtual circle and the outer periphery of the Ag phase.
  • the area ratio of the C phase from an image obtained by observing the range of 1 mm 2 with an optical microscope, it was 21.6%.
  • composition analysis was performed using small pieces collected from the sintered body.
  • Fe, Pt, Ag, Cu, and Co were measured using an ICP-AES apparatus, and C was measured using a carbon analyzer employing a high frequency induction furnace combustion-infrared absorption method.
  • the atomic ratio was calculated from the weight ratio thus obtained, and the atomic ratio of C divided by the atomic ratio of Ag was 4.2.
  • 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 to produce a disk-shaped target.
  • This was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed under the same conditions as in Example 1. As a result, the number of particles was 17.
  • the weighed powder was sealed in a 10-liter ball mill pot together with zirconia balls as a grinding medium in an Ar atmosphere, and rotated and mixed for 4 hours. Then, the powder taken out from the pot was filled in a carbon mold and molded and sintered using a hot press apparatus.
  • the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 900 ° 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.
  • a part of the sintered body thus prepared was cut out, the cross section was polished, and observed with an electron probe microanalyzer (EPMA).
  • EPMA electron probe microanalyzer
  • the Fe—Pt—Cu—Co alloy phase, Ag phase and C phase were observed. Were confirmed to be uniformly dispersed in each other.
  • a coarse Ag phase is observed, and the Ag phase is included in all virtual circles having a radius of 10 ⁇ m drawn around an arbitrary point in the phase, or It was confirmed that 20% or more of the Ag phase was present in terms of area ratio, which did not have a shape having at least two contact points or intersections between the virtual circle and the outer periphery of the Ag phase.
  • composition analysis was performed using small pieces collected from the sintered body.
  • Fe, Pt, and Ag were measured using an ICP-AES apparatus, and C was measured using a carbon analyzer employing a high frequency induction furnace combustion-infrared absorption method.
  • the atomic ratio was calculated from the weight ratio thus obtained, and the atomic ratio of C was divided by the atomic ratio of Ag to be 4.2.
  • 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 to produce a disk-shaped target.
  • This was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed under the same conditions as in Example 1.
  • the number of particles was 183, which was larger than that of Example 3.
  • any of the examples it was found that the amount of particles generated during sputtering can be reduced, and it has a very important role in improving the yield during film formation.
  • the target which contained Cu and Co as an additional metal was illustrated in the Example, other metal elements (Au, B, Cr, Ga, Ge, Mn, Mo, Nb, Ni, Pd, Re, Rh , Ru, Sn, Ta, W, V, Zn), the same results were obtained.
  • the sputtering target of the present invention has an excellent effect that the amount of particles generated at the time of sputtering can be reduced and the yield at the time of film formation can be improved. Therefore, it is useful as a sputtering target for forming a granular structure type magnetic thin film.

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

Abstract

L'invention porte sur une cible de pulvérisation cathodique qui est composée d'une phase alliage à base de Fe-Pt, d'une phase Ag et d'une phase C, caractérisée en ce que : dans la composition dans sa totalité de la cible de pulvérisation cathodique, la valeur obtenue par division du rapport atomique de C par le rapport atomique de Ag est de 4 à 10; et, dans la section transversale de la cible de pulvérisation cathodique, la phase Ag a une forme telle que la phase Ag soit contenue dans un cercle virtuel quelconque de 10 µm de diamètre tracé autour d'un point arbitraire présent dans la phase Ag, ou qu'au moins deux points de contact d'intersection soient formés entre ledit cercle virtuel et la circonférence extérieure de la phase Ag. La présente invention résout le problème consistant à fournir une cible de pulvérisation cathodique intégrée, composée d'un alliage à base de Fe-Pt, d'Ag et de C, et qui peut conduire à une forte réduction de la quantité de particules générées pendant la pulvérisation cathodique.
PCT/JP2014/051970 2013-04-15 2014-01-29 Cible de pulvérisation cathodique WO2014171161A1 (fr)

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JP2015512326A JP5944580B2 (ja) 2013-04-15 2014-01-29 スパッタリングターゲット
SG11201506140WA SG11201506140WA (en) 2013-04-15 2014-01-29 Sputtering target

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016047236A1 (fr) * 2014-09-22 2016-03-31 Ｊｘ金属株式会社 Cible de pulvérisation cathodique permettant la formation d'un film d'enregistrement magnétique et procédé de production s'y rapportant
CN106378455A (zh) * 2015-07-31 2017-02-08 汉能新材料科技有限公司 一种钼合金旋转金属管材及其制备方法
JP2023013901A (ja) * 2021-07-15 2023-01-26 光洋應用材料科技股▲分▼有限公司 Ｆｅ－Ｐｔ－Ａｇ系ターゲット及びその製造方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007080781A1 (fr) * 2006-01-13 2007-07-19 Nippon Mining & Metals Co., Ltd. Cible de pulverisation cathodique en materiau ferromagnetique contenant des particules dispersees de materiau non magnetique
WO2012073882A1 (fr) * 2010-11-29 2012-06-07 三井金属鉱業株式会社 Cible de pulvérisation
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
WO2013046882A1 (fr) * 2011-09-26 2013-04-04 Jx日鉱日石金属株式会社 Cible de pulvérisation cathodique en fer/platine/carbone
WO2014024519A1 (fr) * 2012-08-10 2014-02-13 三井金属鉱業株式会社 Corps fritté et cible de pulvérisation

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007080781A1 (fr) * 2006-01-13 2007-07-19 Nippon Mining & Metals Co., Ltd. Cible de pulverisation cathodique en materiau ferromagnetique contenant des particules dispersees de materiau non magnetique
WO2012073882A1 (fr) * 2010-11-29 2012-06-07 三井金属鉱業株式会社 Cible de pulvérisation
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
WO2013046882A1 (fr) * 2011-09-26 2013-04-04 Jx日鉱日石金属株式会社 Cible de pulvérisation cathodique en fer/platine/carbone
WO2014024519A1 (fr) * 2012-08-10 2014-02-13 三井金属鉱業株式会社 Corps fritté et cible de pulvérisation

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016047236A1 (fr) * 2014-09-22 2016-03-31 Ｊｘ金属株式会社 Cible de pulvérisation cathodique permettant la formation d'un film d'enregistrement magnétique et procédé de production s'y rapportant
JPWO2016047236A1 (ja) * 2014-09-22 2017-05-25 Ｊｘ金属株式会社 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
US10600440B2 (en) 2014-09-22 2020-03-24 Jx Nippon Mining & Metals Corporation Sputtering target for forming magnetic recording film and method for producing same
CN106378455A (zh) * 2015-07-31 2017-02-08 汉能新材料科技有限公司 一种钼合金旋转金属管材及其制备方法
JP2023013901A (ja) * 2021-07-15 2023-01-26 光洋應用材料科技股▲分▼有限公司 Ｆｅ－Ｐｔ－Ａｇ系ターゲット及びその製造方法
JP7245303B2 (ja) 2021-07-15 2023-03-23 光洋應用材料科技股▲分▼有限公司 Ｆｅ－Ｐｔ－Ａｇ系ターゲット及びその製造方法

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JP5944580B2 (ja) 2016-07-05
TW201446975A (zh) 2014-12-16
JPWO2014171161A1 (ja) 2017-02-16
SG11201506140WA (en) 2015-09-29
TWI593810B (zh) 2017-08-01

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