WO2014141737A1 - Cible de pulvérisation - Google Patents

Cible de pulvérisation Download PDF

Info

Publication number
WO2014141737A1
WO2014141737A1 PCT/JP2014/050980 JP2014050980W WO2014141737A1 WO 2014141737 A1 WO2014141737 A1 WO 2014141737A1 JP 2014050980 W JP2014050980 W JP 2014050980W WO 2014141737 A1 WO2014141737 A1 WO 2014141737A1
Authority
WO
WIPO (PCT)
Prior art keywords
oxide
phase
powder
sputtering
sputtering target
Prior art date
Application number
PCT/JP2014/050980
Other languages
English (en)
Japanese (ja)
Inventor
佐藤　敦
荒川　篤俊
英生 高見
中村　祐一郎
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 JP2014533302A priority Critical patent/JP5801496B2/ja
Priority to SG11201501365WA priority patent/SG11201501365WA/en
Publication of WO2014141737A1 publication Critical patent/WO2014141737A1/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
    • G11B5/62—Record carriers characterised by the selection of the material
    • G11B5/64—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent
    • G11B5/65—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition
    • G11B5/658—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition containing oxygen, e.g. molecular oxygen or magnetic oxide
    • 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 forming a thin film of a magnetic recording medium.
  • the present invention relates to a sputtering target having a structure in which an oxide phase is dispersed in a metal phase containing Co as a main component.
  • a ferromagnetic alloy containing Co as a main component is used for the magnetic crystal particles, and an oxide is used for the nonmagnetic material.
  • Such a granular structure type magnetic thin film is produced by sputtering a sputtering target having a structure in which an oxide phase is dispersed in a metal phase onto a substrate by a magnetron sputtering apparatus.
  • deposits on the thin film forming substrate called particles are a problem in the sputtering process. It is known that many of the particles generated during film formation are oxides in the target. It is considered that abnormal discharge occurs on the sputtering surface of the target during sputtering, and that the oxide falls off from the sputtering surface of the target as a cause of generation of particles. In recent years, as the recording density of hard disk drives has increased, the flying height of the magnetic head has become smaller, so the size and number of particles allowed in magnetic recording media have become increasingly severely limited. .
  • Patent Documents 1 to 8, etc. Various techniques are known regarding a sputtering target having a structure in which an oxide phase is dispersed in a metal phase, and a method for producing the sputtering target.
  • Patent Document 1 when mixing and pulverizing raw material powder with a ball mill or the like, a primary sintered body powder obtained by mixing, sintering, and pulverizing a part of the raw material powder in advance is mixed to oxidize.
  • a method for reducing the generation of particles while minimizing the target structure by suppressing the aggregation of objects is disclosed.
  • the oxide when producing a sputtering target in which an oxide phase is dispersed in a metal phase, the oxide may aggregate, and this aggregated oxide may cause particles during sputtering.
  • the oxide phase in order to suppress the generation of such particles, the oxide phase is finely dispersed in the metal phase.
  • an object of the present invention is to provide a sputtering target that generates less particles during sputtering.
  • the present inventors have conducted intensive research, and as a result, by adding Mn to each of the metal phase and the oxide phase, it becomes possible to reduce particle generation more effectively.
  • the inventors have found that the yield during film formation can be improved.
  • the present invention 1) A sintered sputtering target having a structure in which a metal phase and an oxide phase are uniformly dispersed, wherein the metal phase contains Co, Pt, and Mn as components, and the oxide phase contains at least Mn as a component.
  • a sputtering target comprising an oxide 2 The sputtering target according to 1) above, wherein a part of the metal phase is a Pt—Mn phase, 3)
  • the oxide phase further includes Al, B, Ba, Be, Bi, Ca, Ce, Co, Cr, Cs, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Ho, La, From 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
  • 4) The sputtering target according to any one of 1) to 3) above, wherein the oxide phase is a composite oxide containing Mn as one of the constituent components.
  • the sputtering target of the present invention has an excellent effect that the amount of particles generated during sputtering can be reduced and the yield during film formation can be improved.
  • the sputtering target of the present invention is a sintered sputtering target having a structure in which a metal phase and an oxide phase are uniformly dispersed, wherein the metal phase contains Co, Pt, and Mn as components, and the oxide phase is at least It contains an oxide containing Mn as a constituent component.
  • a Co—Pt alloy is a material that has been known for a long time as a magnetic crystal grain, but it contains Mn in addition to Co and Pt as a component of the metal phase, and the oxide phase is at least Mn. It is important in the present invention to contain an oxide containing as a constituent component.
  • Patent Documents 5 to 6 disclose that a sintered body sputtering target made of a ferromagnetic alloy and a nonmetallic inorganic material contains an oxide of Mn as an inorganic material. It does not teach a technique for improving adhesion by containing Mn in both the phase and the oxide phase.
  • the sputtering target of the present invention includes a case where a part of the metal phase is a Pt—Mn phase.
  • the Pt—Mn phase can improve the adhesion with the oxide phase, and since the Pt—Mn phase is a stable form, the Pt—Mn phase itself does not cause particles. It is effective in suppressing the generation of particles.
  • the Mn content ratio in the metal phase it is desirable to adjust the Mn content ratio in the metal phase to 0.5% or more and 20% or less in the atomic ratio in the metal phase.
  • the content ratio of Mn in the metal phase is less than 0.5%, the effect of increasing the adhesion with the oxide phase is reduced, and thus the generation of particles may not be sufficiently suppressed.
  • it is larger than 20% the toughness of the sputtering target is lowered, and there may be a problem that the target breaks during sputtering.
  • composition (100- ⁇ - ⁇ - ⁇ ) Co- ⁇ Pt- ⁇ Mn- ⁇ M (wherein ⁇ is 5 ⁇ ⁇ ⁇ 30, ⁇ is 0.5 ⁇ ⁇ ⁇ 20, and ⁇ is 0.5 ⁇ The condition of ⁇ ⁇ 20 is satisfied.
  • the M means an additive metal element described later.
  • the range of the above composition is a range for improving the magnetic characteristics as the recording layer of the hard disk medium, and is outside this range and has the characteristics as the recording layer, so that the amount of particles generated during sputtering can be reduced. It does not impair the excellent effect.
  • the oxide phase further includes 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,
  • an oxide containing one or more elements selected from Yb, Zn, and Zr as a constituent component is also included.
  • the sputtering target of the present invention includes a case where the oxide phase is a complex oxide having Mn as one of the constituent components. Mn oxides easily form complex oxides with other oxides. In this case, however, the adhesion between the metal phase and the oxide phase will be further improved, so the generation of particles will be more effectively suppressed. can do.
  • the metal phase further contains Ag, Au, B, Cr, Cu, Fe, Ga, Ge, Mo, Nb, Ni, Pd, Re, Rh, Ru, Sn, The case where one or more elements selected from Ta, W, V, and Zn are contained is also included. These metal components can be appropriately added according to the desired magnetic properties.
  • the sputtering target of the present invention includes a case where the oxide phase is 10% or more and less than 55% by volume in the sputtering target.
  • the volume ratio of the oxide phase is 10% or more and less than 55% by volume in the sputtering target.
  • the magnetic properties can be further improved in the formed magnetic thin film.
  • the volume ratio of the oxide phase is less than 10%, the effect of the oxide blocking the magnetic interaction between the magnetic particles is reduced, and when the volume ratio of the oxide phase is 55% or more, Since the dispersibility of the oxide phase is deteriorated, a problem that the amount of particles increases may occur.
  • the volume ratio of the oxide phase can be obtained from the area ratio of the oxide phase at an arbitrary cut surface of the sputtering target.
  • the volume ratio of the oxide phase in the sputtering target can be the area ratio at the cut surface.
  • the area ratio can be obtained as an average by observing a region of approximately 1 mm 2 or more in order to reduce variation due to the observation place.
  • the sputtering target of the present invention can be produced, for example, by the following method.
  • Co powder, Pt powder, and Mn powder are prepared as metal powder.
  • metal powders preferably have a particle size in the range of 1 to 10 ⁇ m.
  • the particle size is 1 to 10 ⁇ m, more uniform mixing is possible, and segregation and coarse crystallization of the sintered target can be prevented.
  • the metal powder is larger than 10 ⁇ m, the oxide phase may not be finely dispersed.
  • the metal powder is smaller than 1 ⁇ m, the influence of the oxidation of the metal powder may be a problem.
  • this particle size range is a preferable range, and that deviating from this range is not a condition for denying the present invention.
  • Mn oxide powder and oxide powder composed of other elements as required are prepared.
  • Mn 3 O 4 powder or Mn 2 O 3 powder can be used as the Mn oxide powder.
  • the average particle size of the oxide powder is larger than 5 ⁇ m, a coarse oxide phase may be formed after sintering, and when smaller than 0.2 ⁇ m, the oxide powder may be aggregated. is there.
  • this range is merely a preferable range, and it should be understood that deviating from this range is not a condition for denying the present invention.
  • the raw material powder is measured so that it may become a desired composition, and it mixes also using a well-known method, such as a ball mill, also as a grinding
  • a well-known method such as a ball mill, also as a grinding
  • 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 for sintering depends on the composition but is often in the range of 700 ° C. to 1100 ° C.
  • the sputtering target of the present invention can be manufactured.
  • the sputtering target manufactured in this way has an excellent effect that the amount of particles generated during sputtering can be reduced and the yield during film formation can be improved.
  • Example 1 A Co—Cr—Pt—Mn powder having an average particle diameter of 10 ⁇ m prepared by a gas atomization method was prepared as a metal powder, and an MnO powder having an average particle diameter of 3 ⁇ m and a Y 2 O 3 powder having an average particle diameter of 3 ⁇ m were prepared as oxide powders. And it weighed so that the total weight might be 2000g with the following composition ratios. Weighing composition (number ratio): 65Co-5Cr-15Pt-5Mn-5MnO-5Y 2 O 3
  • Each of the weighed powders was enclosed in a ball mill pot having a capacity of 10 liters together with zirconia balls as a grinding medium, and mixed by rotating for 8 hours.
  • the mixed powder taken out from the ball mill was filled in a carbon mold having a diameter of 190 mm and sintered by hot pressing.
  • the conditions for hot pressing are a vacuum atmosphere, a heating rate of 300 ° C / hour, and a holding temperature of 100.
  • the temperature was 0 ° C. and the holding time was 2 hours, and the pressure was increased from 30 MPa until the end of the heating. After completion of the holding, it was naturally cooled in the chamber.
  • the metal phase was an alloy phase containing Co, Cr, Pt, and Mn as components.
  • an oxide phase was a Mn oxide and a Y oxide.
  • 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. The number of particles at this time was 13.
  • Each of the weighed powders was enclosed in a ball mill pot having a capacity of 10 liters together with zirconia balls as a grinding medium, and mixed by rotating for 8 hours.
  • the mixed powder taken out from the ball mill was filled in a carbon mold having a diameter of 190 mm and sintered by hot pressing.
  • the conditions for hot pressing are a vacuum atmosphere, a heating rate of 300 ° C / hour, and a holding temperature of 100.
  • the temperature was 0 ° C. and the holding time was 2 hours, and the pressure was increased from 30 MPa until the end of the heating. After completion of the holding, it was naturally cooled in the chamber.
  • the metal phase was an alloy phase containing Co, Cr, Pt, and Mn as components. Furthermore, it was confirmed that a part of the metal phase was a Pt—Mn phase.
  • the oxide phase was confirmed to be Mn oxide and Y oxide.
  • 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. At this time, the number of particles was eight.
  • Co powder having an average particle diameter of 3 ⁇ m, Cr powder having an average particle diameter of 5 ⁇ m, and Pt powder having an average particle diameter of 3 ⁇ m were prepared as metal powder, and Y 2 O 3 powder having an average particle diameter of 3 ⁇ m was prepared as oxide powder. And it weighed so that the total weight might be 1850g with the following composition ratios. Weighing composition (number ratio of molecules): 70Co-5Cr-15Pt-10Y 2 O 3
  • each weighed powder was enclosed in a ball mill pot with a capacity of 10 liters together with zirconia balls as a grinding medium, and rotated and mixed for 8 hours.
  • the mixed powder taken out from the ball mill was filled in a carbon mold having a diameter of 190 mm and sintered by hot pressing.
  • 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.
  • the metal phase was an alloy phase containing Co, Cr, and Pt as components.
  • This metal phase was a uniform alloy phase of Co—Cr—Pt.
  • an oxide phase was Y oxide.
  • 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. The number of particles at this time was 52, which was larger than those in Examples 1 and 2.
  • each weighed powder was enclosed in a ball mill pot with a capacity of 10 liters together with zirconia balls as a grinding medium, and rotated and mixed for 8 hours.
  • the mixed powder taken out from the ball mill was filled in a carbon mold having a diameter of 190 mm and sintered by hot pressing.
  • 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.
  • the metal phase was an alloy phase containing Co, Cr, and Pt as components.
  • the oxide phase was confirmed to be Mn oxide and Y oxide.
  • 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. The number of particles at this time was 27, which was larger than those in Examples 1 and 2.
  • each weighed powder was enclosed in a ball mill pot with a capacity of 10 liters together with zirconia balls as a grinding medium, and rotated and mixed for 8 hours.
  • the mixed powder taken out from the ball mill was filled in a carbon mold having a diameter of 190 mm and sintered by hot pressing.
  • 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.
  • the metal phase was an alloy phase containing Co, Cr, Pt, and Mn as components.
  • an oxide phase was Y oxide.
  • 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.
  • the number of particles at this time was 82, which was larger than those in Examples 1 and 2.
  • each weighed powder was enclosed in a ball mill pot with a capacity of 10 liters together with zirconia balls as a grinding medium, and rotated and mixed for 8 hours.
  • the mixed powder taken out from the ball mill was filled in a carbon mold having a diameter of 190 mm and sintered by hot pressing.
  • 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.
  • the metal phase was an alloy phase containing Co, Cr, Pt, and Mn as components. Furthermore, it was confirmed that a part of the metal phase was a Pt—Mn phase. Further, it was confirmed that the oxide phase was a complex oxide containing Si and Mn and Si oxide.
  • 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. The number of particles at this time was 12.
  • Example 4 Co powder having an average particle size of 3 ⁇ m, Cr powder having an average particle size of 5 ⁇ m, Pt powder having an average particle size of 3 ⁇ m, Mn powder having an average particle size of 20 ⁇ m, and Ru powder having an average particle size of 10 ⁇ m are used as the oxide powder. Mn 2 O 3 powder having a diameter of 3 ⁇ m and TiO 2 powder having an average particle diameter of 1 ⁇ m were prepared. And it weighed so that the total weight might become 2100g with the following composition ratios. Weighing composition (ratio of the number of molecules): 62.5Co-5Cr-15Pt-5Mn-5Ru-2.5Mn 2 O 3 -5TiO 2
  • each weighed powder was enclosed in a ball mill pot with a capacity of 10 liters together with zirconia balls as a grinding medium, and rotated and mixed for 8 hours.
  • the mixed powder taken out from the ball mill was filled in a carbon mold having a diameter of 190 mm and sintered by hot pressing.
  • 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.
  • the metal phase was an alloy phase containing Co, Cr, Pt, Mn, and Ru as components. Furthermore, it was confirmed that a part of the metal phase was a Pt—Mn phase. It was also confirmed that the oxide phase was a complex oxide containing Mn and Ti as components.
  • 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. At this time, the number of particles was seven.
  • the cut surface of the sintered body was polished, and the area ratio of the oxide phase when observed on the polished surface in the range of 1 mm 2 was 21%. That is, the volume ratio of the oxide phase in the target was 21%.
  • Co powder with an average particle size of 3 ⁇ m, Cr powder with an average particle size of 5 ⁇ m, Pt powder with an average particle size of 3 ⁇ m, Mn powder with an average particle size of 20 ⁇ m, Ru powder with an average particle size of 10 ⁇ m as the metal powder are used as oxide powders.
  • Mn 2 O 3 powder having a diameter of 3 ⁇ m and TiO 2 powder having an average particle diameter of 1 ⁇ m were prepared. And it weighed so that the total weight might be 1650g with the following composition ratios. Weighing composition (ratio of molecular number): 37.5Co-5Cr-15Pt-5Mn-5Ru-2.5Mn 2 O 3 -30TiO 2
  • each weighed powder was enclosed in a ball mill pot with a capacity of 10 liters together with zirconia balls as a grinding medium, and rotated and mixed for 8 hours.
  • the mixed powder taken out from the ball mill was filled in a carbon mold having a diameter of 190 mm and sintered by hot pressing.
  • 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.
  • the metal phase was an alloy phase containing Co, Cr, Pt, Mn, and Ru as components. Furthermore, it was confirmed that a part of the metal phase was a Pt—Mn phase. It was also confirmed that the oxide phase was a complex oxide and Ti oxide containing Mn and Ti as components.
  • 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. The number of particles at this time was 82.
  • the cut surface of the sintered body was polished, and the area ratio of the oxide phase when observed on the polished surface in the range of 1 mm 2 was 57%. That is, the volume ratio of the oxide phase in the target was 57%. Compared with Example 4 in which the volume ratio of the oxide phase was 21%, it was confirmed that the particles increased significantly.
  • Example 5 A Co—Pt—Mn powder having an average particle diameter of 10 ⁇ m prepared by a gas atomization method was prepared as a metal powder, and a MnO powder having an average particle diameter of 3 ⁇ m and a Ta 2 O 5 powder having an average particle diameter of 3 ⁇ m were prepared as oxide powders. And it weighed so that the total weight might be 2300g with the following composition ratios. Weighing composition (number ratio): 65Co-20Pt-5Mn-5MnO-5Ta 2 O 5
  • Each of the weighed powders was enclosed in a ball mill pot having a capacity of 10 liters together with zirconia balls as a grinding medium, and mixed by rotating for 8 hours.
  • the mixed powder taken out from the ball mill was filled in a carbon mold having a diameter of 190 mm and sintered by hot pressing.
  • the conditions for hot pressing are a vacuum atmosphere, a heating rate of 300 ° C./hour, and a holding temperature of 110.
  • the temperature was 0 ° C. and the holding time was 2 hours, and the pressure was increased from 30 MPa until the end of the heating. After completion of the holding, it was naturally cooled in the chamber.
  • the metal phase was an alloy phase containing Co, Pt and Mn as components.
  • the oxide phase was confirmed to be Mn oxide and Ta oxide.
  • 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. The number of particles at this time was 16.
  • the amount of particles generated during sputtering can be reduced, and Mn present in the metal phase and the oxidation phase plays a very important role in improving the yield during film formation. It was found to have
  • 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.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Vapour Deposition (AREA)
  • Manufacturing Of Magnetic Record Carriers (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Magnetic Record Carriers (AREA)

Abstract

L'invention concerne une cible de pulvérisation frittée dotée d'une structure dans laquelle des phases de métal et des phases d'oxyde sont dispersées de façon homogène, la cible de pulvérisation étant caractérisée en ce que les phases de métal contiennent Co, Pt et Mn comme composants et les phases d'oxyde contiennent un oxyde ayant au moins Mn comme constituant. La cible de pulvérisation a pour effet de réduire la quantité de particules générées pendant la pulvérisation et d'améliorer le rendement pendant le dépôt de film.
PCT/JP2014/050980 2013-03-12 2014-01-20 Cible de pulvérisation WO2014141737A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP2014533302A JP5801496B2 (ja) 2013-03-12 2014-01-20 スパッタリングターゲット
SG11201501365WA SG11201501365WA (en) 2013-03-12 2014-01-20 Sputtering target

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2013-049130 2013-03-12
JP2013049130 2013-03-12

Publications (1)

Publication Number Publication Date
WO2014141737A1 true WO2014141737A1 (fr) 2014-09-18

Family

ID=51536414

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2014/050980 WO2014141737A1 (fr) 2013-03-12 2014-01-20 Cible de pulvérisation

Country Status (5)

Country Link
JP (1) JP5801496B2 (fr)
MY (1) MY170314A (fr)
SG (1) SG11201501365WA (fr)
TW (1) TWI608113B (fr)
WO (1) WO2014141737A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6027699B1 (ja) * 2016-02-19 2016-11-16 デクセリアルズ株式会社 Ｍｎ−Ｚｎ−Ｗ−Ｏ系スパッタリングターゲット及びその製造方法
WO2020031460A1 (fr) * 2018-08-09 2020-02-13 Ｊｘ金属株式会社 Cible de pulvérisation, film magnétique et support d'enregistrement magnétique perpendiculaire
US11591688B2 (en) 2018-08-09 2023-02-28 Jx Nippon Mining & Metals Corporation Sputtering target, granular film and perpendicular magnetic recording medium
US11837450B2 (en) 2016-02-19 2023-12-05 Jx Metals Corporation Sputtering target for magnetic recording medium, and magnetic thin film
US11894221B2 (en) 2018-08-09 2024-02-06 Jx Metals Corporation Sputtering target and magnetic film

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011514432A (ja) * 2007-09-07 2011-05-06 イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー 銀および少なくとも２種の非銀含有元素を含有する多元素合金粉末
WO2012011294A1 (fr) * 2010-07-20 2012-01-26 Jx日鉱日石金属株式会社 Cible de pulvérisation de matériau ferromagnétique présentant une faible production de particules
JP2012117147A (ja) * 2010-11-12 2012-06-21 Jx Nippon Mining & Metals Corp コバルト酸化物が残留したスパッタリングターゲット

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080131735A1 (en) * 2006-12-05 2008-06-05 Heraeus Incorporated Ni-X, Ni-Y, and Ni-X-Y alloys with or without oxides as sputter targets for perpendicular magnetic recording
US20130213802A1 (en) * 2010-12-22 2013-08-22 Jx Nippon Mining & Metals Corporation Sintered Compact Sputtering Target

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011514432A (ja) * 2007-09-07 2011-05-06 イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー 銀および少なくとも２種の非銀含有元素を含有する多元素合金粉末
WO2012011294A1 (fr) * 2010-07-20 2012-01-26 Jx日鉱日石金属株式会社 Cible de pulvérisation de matériau ferromagnétique présentant une faible production de particules
JP2012117147A (ja) * 2010-11-12 2012-06-21 Jx Nippon Mining & Metals Corp コバルト酸化物が残留したスパッタリングターゲット

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6027699B1 (ja) * 2016-02-19 2016-11-16 デクセリアルズ株式会社 Ｍｎ−Ｚｎ−Ｗ−Ｏ系スパッタリングターゲット及びその製造方法
JP2017145492A (ja) * 2016-02-19 2017-08-24 デクセリアルズ株式会社 Ｍｎ−Ｚｎ−Ｗ−Ｏ系スパッタリングターゲット及びその製造方法
US11837450B2 (en) 2016-02-19 2023-12-05 Jx Metals Corporation Sputtering target for magnetic recording medium, and magnetic thin film
WO2020031460A1 (fr) * 2018-08-09 2020-02-13 Ｊｘ金属株式会社 Cible de pulvérisation, film magnétique et support d'enregistrement magnétique perpendiculaire
JPWO2020031460A1 (ja) * 2018-08-09 2021-10-07 Ｊｘ金属株式会社 スパッタリングターゲット、磁性膜および垂直磁気記録媒体
JP7076555B2 (ja) 2018-08-09 2022-05-27 Ｊｘ金属株式会社 スパッタリングターゲット、磁性膜および垂直磁気記録媒体
US11591688B2 (en) 2018-08-09 2023-02-28 Jx Nippon Mining & Metals Corporation Sputtering target, granular film and perpendicular magnetic recording medium
US11618944B2 (en) 2018-08-09 2023-04-04 Jx Nippon Mining & Metals Corporation Sputtering target, magnetic film, and perpendicular magnetic recording medium
US11894221B2 (en) 2018-08-09 2024-02-06 Jx Metals Corporation Sputtering target and magnetic film
US11939663B2 (en) 2018-08-09 2024-03-26 Jx Metals Corporation Magnetic film and perpendicular magnetic recording medium

Also Published As

Publication number Publication date
TWI608113B (zh) 2017-12-11
MY170314A (en) 2019-07-17
JP5801496B2 (ja) 2015-10-28
TW201443261A (zh) 2014-11-16
SG11201501365WA (en) 2015-05-28
JPWO2014141737A1 (ja) 2017-02-16

Similar Documents

Publication Publication Date Title
JP5290468B2 (ja) Ｃ粒子が分散したＦｅ−Ｐｔ系スパッタリングターゲット
JP5623552B2 (ja) Ｆｅ−Ｐｔ系強磁性材スパッタリングターゲット及びその製造方法
JP5705993B2 (ja) Ｃ粒子が分散したＦｅ−Ｐｔ−Ａｇ−Ｃ系スパッタリングターゲット及びその製造方法
JP5801496B2 (ja) スパッタリングターゲット
JP5960287B2 (ja) 焼結体スパッタリングターゲット
WO2018043680A1 (fr) Cible de pulvérisation à base de fer/platine dispersée dans un matériau non magnétique
JP6437427B2 (ja) 磁気記録媒体用スパッタリングターゲット
JP5944580B2 (ja) スパッタリングターゲット
WO2018123500A1 (fr) Cible de pulvérisation de matériau magnétique et procédé de production de ladite cible
JP5946922B2 (ja) 磁性記録媒体用スパッタリングターゲット
CN111183244B (zh) 强磁性材料溅射靶
JP6728094B2 (ja) 強磁性材スパッタリングターゲット
TW202009307A (zh) 濺鍍靶及磁性膜
WO2017141558A1 (fr) Cible de pulvérisation pour support d'enregistrement magnétique, et film mince magnétique
CN111183243B (zh) 溅射靶、磁性膜和磁性膜的制造方法
JP7412659B2 (ja) スパッタリングターゲット部材、スパッタリングターゲット組立品、及び成膜方法
TWI681067B (zh) 濺鍍靶、磁性膜和磁性膜的製造方法
WO2023079857A1 (fr) ÉLÉMENT DE CIBLE DE PULVÉRISATION CATHODIQUE À BASE DE Fe-Pt-C, ENSEMBLE DE CIBLE DE PULVÉRISATION CATHODIQUE, PROCÉDÉ DE FORMATION DE FILM, ET PROCÉDÉ DE FABRICATION D'ÉLÉMENT DE CIBLE DE PULVÉRISATION CATHODIQUE
TW201915205A (zh) 濺鍍靶、積層膜之製造方法、積層膜及磁記錄媒體
JP2018172762A (ja) スパッタリングターゲット、磁性膜および、磁性膜の製造方法

Legal Events

Date Code Title Description
ENP Entry into the national phase

Ref document number: 2014533302

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: 14764675

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: 14764675

Country of ref document: EP

Kind code of ref document: A1