JP6514654B2 - Magnetic film suitable for magnetic recording medium and method of manufacturing the same - Google Patents

Description

  The present invention relates to a magnetic film suitable for a magnetic recording medium such as a hard disk drive and a method of manufacturing the same.

  In the field of magnetic recording represented by a hard disk drive, materials based on Co, Fe or Ni, which are ferromagnetic metals, have been used as the material of the magnetic thin film in the magnetic recording medium. For example, as a magnetic thin film of a hard disk adopting an in-plane magnetic recording method, a Co-Cr-based or Co-Cr-Pt-based ferromagnetic alloy containing Co as a main component has been used. In addition, many of composite materials consisting of Co-Cr-Pt based ferromagnetic alloy and nonmagnetic inorganic particles mainly composed of Co are used for magnetic thin films of hard disks adopting the perpendicular magnetic recording system that has been put into practical use in recent years. It is done. Then, the above-mentioned magnetic thin film is often produced by sputtering a sputtering target containing the above-mentioned material as a component with a DC magnetron sputtering apparatus because of high productivity.

The recording density of hard disks is rapidly increasing year by year, and when the recording density reaches 1 Tbit / in ² , the recording bit size becomes smaller than 10 nm. In this case, the superparamagnetization due to thermal fluctuation becomes a problem It is expected that materials of magnetic recording media currently being used, for example, materials in which Pt is added to a Co-Cr based alloy to enhance the magnetocrystalline anisotropy are not sufficient. This is because magnetic particles that stably behave as ferromagnetism in a size of 10 nm or less need to have higher magnetocrystalline anisotropy.

For the reasons described above, FePt phase having an L1 ₀ structure is attracting attention as a material for an ultra-high density recording medium. FePt phase having an L1 ₀ structure with a high magnetocrystalline anisotropy, corrosion resistance and excellent oxidation resistance, is what is expected as a material suitable for the application as a magnetic recording medium. And, when using the FePt phase as a material for ultra-high density recording media, development of a technology to disperse the ordered FePt magnetic phase in the magnetically isolated state as high density as possible with uniform orientation It has been demanded.

For this reason, oxide FePt magnetic phase having an L1 ₀ structure, nitrides, carbides, granular structure magnetic thin film was isolated by non-magnetic material such carbon, the next generation hard disk employing a thermally assisted magnetic recording method It has been proposed for magnetic recording media. The granular magnetic thin film has a structure in which magnetic particles are magnetically isolated by the presence of a nonmagnetic substance. In general, a granular magnetic thin film having an FePt phase is prepared using a Fe—Pt based sintered body sputtering target.

  When an FePt film is produced by sputtering, it becomes an irregular phase in which Fe atoms and Pt atoms are randomly arranged. Therefore, in order to form an ordered FePt phase, it is necessary to perform heat treatment at about 600 ° C. after film formation, but for practical use, it is required to lower this temperature as much as possible. In this respect, Patent Document 1 describes that the amount of residual gas component represented by the amount of residual oxygen is reduced in order to lower the annealing temperature required for ordering the alloy film such as FePt alloy. However, when dealing with oxides, carbides, nitrides and the like as nonmagnetic materials, it has not been easy to control the amount of such gas components.

Patent Document 2, is deposited FePt layer by sputtering, then after depositing a sealing layer on the FePt layer performs annealing in the temperature range of 400 to 800 ° C., FePt substantially in L1 ₀ phase After ordering, it is described that the sealing layer is removed. However, this method enables high temperature annealing and does not lower the annealing temperature for ordering.
Further, Patent Document 3, L1 ₀ form ordered alloy mixture films with added MgO are described that can be manufactured under a low film formation temperature than the mixture thin film obtained by adding SiO ₂ and Al ₂ O ₃ . However, this only indicates that when MgO is added, the substrate heating temperature during film formation is relatively low, and it is not intended to lower the ordering temperature.

  The applicant of the present invention previously provided the invention regarding the sputtering target for magnetic recording media of Fe-Pt system (patent documents 4-5). These inventions are excellent techniques that can effectively suppress the generation of particles due to the dropout of carbon contained as non-magnetic material during sputtering, but these particularly mention the reduction of the ordering temperature is not. In addition, although FePt-based sputtering targets and magnetic recording media are disclosed also in Patent Documents 6 to 7, none of them mentions the ordering temperature.

JP 2003-313659 A JP, 2013-77370, A Japanese Patent Application Publication No. 2002-123920 International Publication WO2014 / 196377 International Publication WO2014 / 188916 JP, 2008-59733, A JP, 2012-214874, A

The present invention relates to a Fe-Pt-based magnetic film formed by sputtering, and to provide a magnetic film which express relatively low temperature L1 ₀ ordered structure.

As a result of intensive research conducted by the present inventors in order to solve the above problems, as a result of selecting a metal component which does not react with Fe-Pt at around 500 ° C. and which can increase the driving force of transformation temperature. and, by adding at a predetermined ratio as an additive metal it to Fe-Pt alloy, it is finding that it is possible to lower the heat treatment temperature for expressing an L1 ₀ ordered structure was obtained.
Based on such findings, the present invention provides the following inventions.
1) A magnetic film composed of a magnetic metal containing Fe and Pt and a nonmagnetic material, further containing Mg, and having an atomic ratio of (Fe _1-α Pt _α ) _1-β Mg _β (α, β is A magnetic film characterized by having a composition represented by 0.35 ≦ α ≦ 0.55, and a number satisfying 0.01 ≦ β ≦ 0.2.
2) A magnetic film comprising a magnetic metal containing Fe and Pt and a nonmagnetic material, and further containing at least one metal selected from the metal group M1 consisting of Ge, Ag, Au, and having an atomic ratio Have a composition represented by (Fe _1-α Pt _α ) _1-β M _{1 β} (where α and β are numbers satisfying 0.35 ≦ α ≦ 0.55 and 0.01 ≦ β ≦ 0.2) Magnetic film characterized by
3) A magnetic film comprising a magnetic metal containing Fe and Pt and a nonmagnetic material, and further containing at least one metal selected from the metal group M2 consisting of Pd, Re and Ni, and having an atomic ratio Have a composition represented by (Fe _1-α Pt _α ) _1-β M 2 _β (where α and β are numbers satisfying 0.35 ≦ α ≦ 0.55 and 0.01 ≦ β ≦ 0.2) Magnetic film characterized by
4) The magnetic film according to any one of the above 1) to 3), wherein the ordering temperature is 500 ° C. or less.
5) L1 ₀ the 1 and having a crystal structure of the structure) to 4) magnetic film according to any one of.
6) The nonmagnetic material comprises at least one selected from carbon, carbide, oxide and nitride, and the volume ratio of the nonmagnetic material is 10 to 60 vol% with respect to the total amount of the film The magnetic film according to any one of the above 1) to 5).
7) A method for producing the magnetic film according to any one of the above 1) to 3), wherein a film obtained by sputtering a sputtering target is vacuum heat treated at a temperature of 500 ° C. or less A method of manufacturing a magnetic film characterized by

According to the present invention, it is possible to provide a magnetic film capable of reducing the heat treatment temperature for ordering the FePt magnetic phase. Thus, the ease of formation of the FePt magnetic phase having an L1 ₀ ordered structure, has an excellent effect that it is possible to improve the productivity of the high-density magnetic recording medium.

  The magnetic film of the present invention is composed of a magnetic metal containing Fe and Pt and a nonmagnetic material. Generally as a composition of a FePt alloy, what mix | blended Pt in the ratio of 0.35 or more and 0.55 or less in atomic ratio, and remainder with Fe can be used. This ratio is a range in which effective characteristics as a magnetic recording film can be maintained. The magnetic film of the present invention can be deposited by sputtering. In that case, the composition of the film is usually substantially the same as the composition of the film of the sputtering target.

What is important in the present invention is that the magnetic metal is any one or more metals selected from the metal group M1 consisting of 1) Mg or 2) Ge, Ag, Au, or 3) Pd, Re, Ni And any one or more metals selected from the metal group M2 consisting of and in a predetermined ratio. These metal elements, not react with FePt at about 500 ° C., and, since it is possible to increase the driving force of the transformation temperature, excellent in order to maintain the stability of the L1 ₀ ordered structure of FePt component It is.

In the present invention, the composition satisfies the atomic ratio (Fe _1-α Pt _α ) _1-β Mg _β (α, β is 0.35 ≦ α ≦ 0.55, 0.01 ≦ β ≦ 0.2. It is adding Mg so that it may become. If the atomic ratio of Mg is less than 0.01, the effect of lowering the ordering temperature can not be obtained sufficiently, while if the atomic ratio of Mg exceeds 0.2, the magnetic properties sufficient for a magnetic thin film May not be obtained.

In the present invention, the composition has an atomic ratio (Fe _1-α Pt _α ) _1-β M _{1 β} (α, β is 0.35 ≦ α ≦ 0.55, 0.01 ≦ β ≦ 0.2. One or more metal elements selected from the metal group M1 consisting of Ge, Ag, and Au are added so as to satisfy the number). If the atomic ratio of M1 is less than 0.01, the effect of lowering the ordering temperature can not be sufficiently obtained, while if the atomic ratio of M1 exceeds 0.2, sufficient magnetic properties as a magnetic film can be obtained. May not be obtained.

In the present invention, the composition has an atomic ratio (Fe _1-α Pt _α ) _1-β M 2 _β (α, β is 0.35 ≦ α ≦ 0.55, 0.01 ≦ β ≦ 0.2 One or more metal elements selected from the metal group M2 consisting of Pd, Re, and Ni are added so as to satisfy the number). When the atomic ratio of M2 is less than 0.01, the effect of lowering the ordering temperature can not be sufficiently obtained. On the other hand, when the atomic ratio of M2 exceeds 0.2, sufficient magnetic properties as a magnetic film can be obtained. May not be obtained.

  In addition, the magnetic film of the present invention can contain carbon, carbide, nitride, and oxide as a nonmagnetic material. Such a magnetic film has a structure in which carbon, carbides, nitrides, and carbides insulate the magnetic interaction between the magnetic phases, and therefore good magnetic properties are expected. The compounding amount of the nonmagnetic material is not particularly limited as long as the characteristics as an effective magnetic recording medium can be maintained, but the volume ratio in the magnetic film is preferably 10 vol% to 60 vol%.

Magnetic film of the present invention, ordering temperature (i.e., L1 ₀ structure type heat treatment temperature for expressing the crystal structure of) can be 500 ° C. or less. The energy consumption of the magnetic film formation process can be reduced by lowering the ordering temperature. By adjusting the composition, the ordering temperature can be further reduced to 400 ° C. or less. Whether are ordered to measure the XRD of heat-treated sputtered film (X-ray diffraction method) profile, determines the presence or absence of the superlattice reflection peak from (110) plane in the L1 ₀ structure FePt.

  In the examples and comparative examples, measurement of the XRD profile was performed using a fully automatic horizontal multipurpose X-ray diffractometer SmartLab manufactured by Rigaku Corporation. A Cu tube was used as the X-ray tube, and the tube output was set to 40 kV × 30 mA. In addition, the optical system was arranged in the concentration method, and the measurement was performed in 2θ / θ mode. The scan speed was 10 degrees / minute, and the sampling width was 0.05 degrees. The analysis software PDXL attached to the device was used to analyze the profile. Then, when the integral intensity of the diffraction peak from the (110) plane was 3% or more with respect to the integral intensity of the diffraction peak from the (111) plane, it was considered that Fe—Pt was ordered. The measurement method of the XRD profile is not limited to the above, and similar results can be obtained even if another measurement method such as a thin film method is used.

  Hereinafter, the present invention will be described based on Examples and Comparative Examples. The present embodiment is merely an example, and the present invention is not limited in any way. That is, the present invention is limited only by the scope of claims, and includes various modifications other than the embodiments included in the present invention.

(Example 1-4: additive metal Mg)
As raw material powders, Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, and Mg powder having an average particle diameter of 30 μm were prepared and weighed so as to have a total weight of 2000 g at the following composition ratio.
Example 1: 45Fe-45Pt-10Mg (at%)
Example 2: 40.5 Fe-49.5 Pt-10 Mg (at%)
Example 3: 70Fe-28Pt-20Mg (at%)
Example 4: 49.5 Fe-49.5 Pt-1 Mg (at%)

  The weighed raw material powder was put into a 10 liter ball mill pot together with a grinding medium of SUS balls, and rotated for 5 hours in an Ar atmosphere to mix and grind. Next, the powder taken out from the pot was filled in a mold made of carbon, and was molded and sintered using a hot press. The conditions of the hot press were a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 600 ° C., and a holding time of 2 hours, and pressure was applied at 30 MPa from the temperature rising start to the holding end. After the end of the holding, the chamber was naturally cooled as it was. Thereafter, composition analysis was performed on small pieces collected from the sintered body using an ICP-AES apparatus, and it was confirmed that the composition of any target was substantially the same as the composition of the weight.

  Next, using a lathe, each sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 3.0 mm to obtain a sputtering target on a disk. Next, the target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed. Sputtering conditions were: input power: 1 kW, Ar gas pressure: 1.7 Pa, and film formation was performed for 20 seconds on a silicon substrate. Thereafter, the thin film on the substrate is heated at 400 ° C. for 1 hour in a high vacuum furnace and analyzed by XRD (X-ray diffraction method). As a result, the peak of the Fe-Pt ordered phase is confirmed for any thin film. The

(Comparative Example 1-3: Additive Metal Mg)
Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, and Mg powder having an average particle diameter of 30 μm were prepared, and weighed so as to have a total weight of 2000 g at the following composition ratio.
Comparative Example 1: 49.9 Fe-49.9 Pt-0.2 Mg (at%)
Comparative Example 2: 63Fe-27Pt-10Mg (at%)
Comparative Example 3: 36Fe-54Pt-10Mg (at%)

  The weighed raw material powder was put into a 10-liter ball mill pot together with a grinding medium of SUS balls, and was rotated for 5 hours in an Ar atmosphere to mix and grind. Next, the powder taken out from the pot was filled in a mold made of carbon, and was molded and sintered using a hot press. The conditions of the hot press were the same as in Example 1. After that, the small pieces collected from the sintered body were subjected to compositional analysis using an ICP-AES apparatus, and it was confirmed that the composition of any target was substantially the same as the composition for weighing.

  Next, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 3.0 mm to obtain a sputtering target on a disk. Next, the target was attached to a magnetron sputtering apparatus, and sputtering was performed under the same conditions as in Example 1. Thereafter, the thin film on the substrate was heated at 400 ° C. for 1 hour in a high vacuum furnace and analyzed by XRD (X-ray diffraction method). As a result, no peak of the Fe—Pt ordered phase was confirmed.

(Example 5-8: additive metal M1)
Prepare Fe powder with an average particle size of 3 μm, Pt powder with an average particle size of 3 μm, Ge powder with an average particle size of 20 μm, and Ag powder with an average particle size of 5 μm. did.
Example 5: 45Fe-45Pt-10Ge (at%)
Example 6: 40Fe-40Pt-20Ge (at%)
Example 7: 45Fe-45Pt-10Ag (at%)
Example 8: 40Fe-40Pt-20Ag (at%)

  The weighed raw material powder was put into a 10-liter ball mill pot together with a grinding medium of SUS balls, and was rotated for 5 hours in an Ar atmosphere to mix and grind. Next, the powder taken out from the pot was filled in a mold made of carbon, and was molded and sintered using a hot press. The hot pressing conditions were the same as in Example 1 except that the holding temperature was 900 ° C. (Examples 5 and 6) and 800 ° C. (Examples 7 and 8). After that, the small pieces collected from the sintered body were subjected to compositional analysis using an ICP-AES apparatus, and it was confirmed that the composition of any target was substantially the same as the composition for weighing.

  Next, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 3.0 mm to obtain a sputtering target on a disk. Next, the target was attached to a magnetron sputtering apparatus, and sputtering was performed under the same conditions as in Example 1. Then, after heating the thin film on a substrate at 400 ° C. for 1 hour in a high vacuum furnace, as a result of analysis by XRD (X-ray diffraction method), a peak of Fe—Pt ordered phase was confirmed.

(Comparative Example 4-6: additive metal M1)
Prepare Fe powder with an average particle size of 3 μm, Pt powder with an average particle size of 3 μm, Ge powder with an average particle size of 20 μm, and Ag powder with an average particle size of 5 μm. did.
Comparative Example 4: 49.9 Fe-49.9 Pt-0.2 Ge (at%)
Comparative Example 5: 63Fe-27Pt-10Ge (at%)
Comparative Example 6: 49.95 Fe-49. 95 Pt-0.1 Ag (at%)

  The weighed raw material powder was put into a 10-liter ball mill pot together with a grinding medium of SUS balls, and was rotated for 5 hours in an Ar atmosphere to mix and grind. Next, the powder taken out of the pot was filled into a carbon mold, and was molded and sintered using a hot press. The conditions of the hot press were the same as in Example 1 except that the holding temperatures were set to 900 ° C. (Examples 4 and 5) and 800 ° C. (Example 6). After that, the small pieces collected from the sintered body were subjected to compositional analysis using an ICP-AES apparatus, and it was confirmed that the composition of any target was substantially the same as the composition for weighing.

  Next, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 3.0 mm to obtain a sputtering target on a disk. Next, the target was attached to a magnetron sputtering apparatus, and sputtering was performed under the same conditions as in Example 1. Thereafter, the thin film on the substrate was heated at 400 ° C. for 1 hour in a high vacuum furnace and analyzed by XRD (X-ray diffraction method). As a result, no peak of the Fe—Pt ordered phase was confirmed.

(Example 9-10: additive metal M2)
Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, and Pd powder having an average particle diameter of 10 μm were prepared, and weighed so as to have a total weight of 2000 g at the following composition ratio.
Example 9 49.5 Fe-49.5 Pt-1 Pd (at%)
Example 10: 45Fe-45Pt-10Pd (at%)

  The weighed raw material powder was put into a 10-liter ball mill pot together with a grinding medium of SUS balls, and was rotated for 5 hours in an Ar atmosphere to mix and grind. Next, the powder taken out from the pot was filled in a mold made of carbon, and was molded and sintered using a hot press. The conditions of the hot press were the same as in Example 1 except that the holding temperature was 1000 ° C. After that, the small pieces collected from the sintered body were subjected to compositional analysis using an ICP-AES apparatus, and it was confirmed that the composition of any target was substantially the same as the composition for weighing.

  Next, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 3.0 mm to obtain a sputtering target on a disk. Next, the target was attached to a magnetron sputtering apparatus, and sputtering was performed under the same conditions as in Example 1. Then, after heating the thin film on a substrate at 400 ° C. for 1 hour in a high vacuum furnace, as a result of analysis by XRD (X-ray diffraction method), a peak of Fe—Pt ordered phase was confirmed.

(Example 11, Comparative Example 7: Nonmagnetic Material C)
Prepare Fe powder with an average particle diameter of 3 μm, Pt powder with an average particle diameter of 3 μm, Ag powder with an average particle diameter of 5 μm, and C powder with an average particle diameter of 10 μm, and weigh it so that the total weight becomes 2000 g with the following composition ratio did. The volume ratio of the nonmagnetic material (C) at this time is 29.9 vol%.
Example 11: 27Fe-27Pt-6Ag-40C (at%)
Comparative Example 7: 22.5 Fe-22.5 Pt-15 Ag-40 C (at%)
In addition, the calculation method of volume ratio can be calculated | required from the weight ratio and density of each element.
The weight ratio of Fe, Pt, Ag, C is W1, W2, W3, W4 (wt%), and the density of Fe, Pt, Ag, C is D1, D2, D3, D4 (g / cm ³ ) It can be obtained by introducing it into the following equation.
Volume ratio of C (%) = C volume (W4 / D4) / total volume (W1 / D1 + W2 / D2 + W3 / D3 + W4 / D4) × 100

  The weighed raw material powder was put into a 10-liter ball mill pot together with a grinding medium of SUS balls, and was rotated for 5 hours in an Ar atmosphere to mix and grind. Next, the powder taken out from the pot was filled in a mold made of carbon, and was molded and sintered using a hot press. The conditions of the hot press were the same as in Example 1 except that the holding temperature was 800 ° C. Thereafter, the sintered body was further subjected to HIP treatment at 900 ° C. About the small piece collected from the obtained sintered body, the metal component is analyzed by ICP-AES device, the carbon is analyzed by carbon analysis device adopting high frequency induction heating furnace combustion-infrared absorption method, and the composition of the target is substantially It was confirmed that the composition was the same as the composition for weighing. The relative density of the sintered body was 95%.

  Next, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 3.0 mm to obtain a sputtering target on a disk. Next, the target was attached to a magnetron sputtering apparatus, and sputtering was performed under the same conditions as in Example 1. Thereafter, the thin film on the substrate is heated at 400 ° C. for 1 hour in a high vacuum furnace and analyzed by XRD (X-ray diffraction method). As a result, for Example 11, a peak of Fe-Pt ordered phase is confirmed. The On the other hand, in Comparative Example 7, the peak of the Fe-Pt regular phase was only slightly confirmed, and it was judged to be insufficient.

The results of the above are summarized in Table 1.

(Examples 12-14, Comparative Example 8: Nonmagnetic Material C)
Prepare Fe powder of average particle diameter 3 μm, Pt powder of average particle diameter 3 μm, Ag powder of average particle diameter 5 μm, Ni powder of average particle diameter 1 μm, Ge powder of average particle diameter 20 μm, C powder of average particle diameter 10 μm It weighed so that the total weight might be 2000 g in the following composition ratios.
Example 12: 27Fe-27Pt-6Ag-40C (at%)
Example 13: 27Fe-27Pt-3Ag-3Ge-40C (at%)
Example 14: 27Fe-27Pt-3Ni-3Ge-40C (at%)
Comparative Example 8: 30Fe-30Pt-40C (at%)

  The weighed raw material powder was put into a 10-liter ball mill pot together with a grinding medium of SUS balls, and was rotated for 5 hours in an Ar atmosphere to mix and grind. Next, the powder taken out from the pot was filled in a mold made of carbon, and was molded and sintered using a hot press. The hot pressing conditions were the same as in Example 1 except that the holding temperature was changed to 750 ° C. (Examples 12 and 14), 650 ° C. (Example 13), and 1100 ° C. (Comparative Example 8). After that, the small pieces collected from the sintered body were subjected to compositional analysis using an ICP-AES apparatus, and it was confirmed that the composition of any target was substantially the same as the composition for weighing.

  Next, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 3.0 mm to obtain a sputtering target on a disk. Next, the target was attached to a magnetron sputtering apparatus, and sputtering was performed under the same conditions as in Example 1. Thereafter, the thin film on the substrate is heated at 500 ° C. for 1 hour in a high vacuum furnace and analyzed by XRD (X-ray diffraction method). As a result, in Examples 12 to 14, the peak of Fe-Pt ordered phase is confirmed It was done. On the other hand, in Comparative Example 8, the peak of the Fe-Pt ordered phase was not confirmed.

(Examples 15-17, Comparative Example 9: Nonmagnetic Material BN, C)
Fe powder of average particle diameter 3 μm, Pt powder of average particle diameter 3 μm, Ag powder of average particle diameter 5 μm, Ni powder of average particle diameter 1 μm, Ge powder of average particle diameter 20 μm, C powder of average particle diameter 10 μm, average particle BN powder having a diameter of 15 μm was prepared, and weighed so that the total weight became 2000 g at the following composition ratio.
Example 15: 27Fe-27Pt-6Ge-10BN-30C (at%)
Example 16: 27Fe-27Pt-3Ag-3Ge-10BN-30C (at%)
Example 17: 27Fe-27Pt-3Ni-3Ge-10BN-30C (at%)
Comparative Example 8: 30Fe-30Pt-10BN-30C (at%)

  The weighed raw material powder was put into a 10-liter ball mill pot together with a grinding medium of SUS balls, and was rotated for 5 hours in an Ar atmosphere to mix and grind. Next, the powder taken out from the pot was filled in a mold made of carbon, and was molded and sintered using a hot press. The hot pressing conditions were the same as in Example 1 except that the holding temperature was changed to 750 ° C. (Examples 15 and 17), 650 ° C. (Example 16), and 1100 ° C. (Comparative Example 9). After that, the small pieces collected from the sintered body were subjected to compositional analysis using an ICP-AES apparatus, and it was confirmed that the composition of any target was substantially the same as the composition for weighing.

  Next, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 3.0 mm to obtain a sputtering target on a disk. Next, the target was attached to a magnetron sputtering apparatus, and sputtering was performed under the same conditions as in Example 1. Thereafter, the thin film on the substrate is heated at 500 ° C. for 1 hour in a high vacuum furnace and analyzed by XRD (X-ray diffraction method). As a result, for Examples 15 to 17, the peak of Fe-Pt ordered phase is confirmed It was done. On the other hand, in Comparative Example 9, the peak of the Fe-Pt ordered phase was not confirmed.

(Example 18-20, Comparative Example 10: Nonmagnetic Material SiO ₂ , C)
Fe powder of average particle diameter 3 μm, Pt powder of average particle diameter 3 μm, Ag powder of average particle diameter 5 μm, Ni powder of average particle diameter 1 μm, Ge powder of average particle diameter 20 μm, C powder of average particle diameter 10 μm, average particle An SiO ₂ powder having a diameter of 0.5 μm was prepared, and was weighed so that the total weight became 2000 g at the following composition ratio.
Example _{18: 27Fe-27Pt-6Ge-} 6SiO 2 -34C (at%)
Example _{19: 27Fe-27Pt-3Ag-} 3Ge-6SiO 2 -34C (at%)
Example _{20: 27Fe-27Pt-3Ni-} 3Ge-6SiO 2 -34C (at%)
Comparative Example _{10: 30Fe-30Pt-6SiO 2} -34C (at%)

  The weighed raw material powder was put into a 10-liter ball mill pot together with a grinding medium of SUS balls, and was rotated for 5 hours in an Ar atmosphere to mix and grind. Next, the powder taken out of the pot was filled into a carbon mold, and was molded and sintered using a hot press. The hot pressing conditions were the same as in Example 1 except that the holding temperature was changed to 750 ° C. (Examples 18 and 20), 650 ° C. (Example 19), and 1100 ° C. (Comparative Example 10). After that, the small pieces collected from the sintered body were subjected to compositional analysis using an ICP-AES apparatus, and it was confirmed that the composition of any target was substantially the same as the composition for weighing.

  Next, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 3.0 mm to obtain a sputtering target on a disk. Next, the target was attached to a magnetron sputtering apparatus, and sputtering was performed under the same conditions as in Example 1. Thereafter, the thin film on the substrate is heated at 500 ° C. for 1 hour in a high vacuum furnace and analyzed by XRD (X-ray diffraction method). As a result, for Examples 18 to 20, the peak of the Fe-Pt ordered phase is confirmed. On the other hand, in Comparative Example 10, the peak of the Fe-Pt ordered phase was not confirmed.

(Example 21-23, Comparative Example 11: Nonmagnetic Material MgO, TiN)
Fe powder of average particle diameter 3 μm, Pt powder of average particle diameter 3 μm, Ag powder of average particle diameter 5 μm, Ni powder of average particle diameter 1 μm, Ge powder of average particle diameter 20 μm, C powder of average particle diameter 10 μm, average particle MgO powder with a diameter of 1 μm and TiN with an average particle diameter of 1 μm were prepared, and weighed so that the total weight became 2000 g with the following composition ratio.
Example 21: 36Fe-36Pt-8Ge-10MgO-10TiN (at%)
Example 22: 36Fe-36Pt-4Ag-4Ge-10MgO-10TiN (at%)
Example 23: 36Fe-36Pt-4Ni-4Ge-10MgO-10TiN (at%)
Comparative example 11: 40 Fe-40 Pt-10 MgO-10 TiN (at%)

  The weighed raw material powder was put into a 10-liter ball mill pot together with a grinding medium of SUS balls, and was rotated for 5 hours in an Ar atmosphere to mix and grind. Next, the powder taken out from the pot was filled in a mold made of carbon, and was molded and sintered using a hot press. The hot pressing conditions were the same as in Example 1 except that the holding temperature was changed to 750 ° C. (Examples 21 and 23), 650 ° C. (Example 22), and 1100 ° C. (Comparative Example 11). After that, the small pieces collected from the sintered body were subjected to compositional analysis using an ICP-AES apparatus, and it was confirmed that the composition of any target was substantially the same as the composition for weighing.

  Next, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 3.0 mm to obtain a sputtering target on a disk. Next, the target was attached to a magnetron sputtering apparatus, and sputtering was performed under the same conditions as in Example 1. Thereafter, the thin film on the substrate is heated at 500 ° C. for 1 hour in a high vacuum furnace and analyzed by XRD (X-ray diffraction method). As a result, for Examples 21 to 23, the peak of Fe-Pt ordered phase is confirmed It was done. On the other hand, in Comparative Example 11, the peak of the Fe-Pt ordered phase was not confirmed.

(Examples 24 to 26, Comparative Example 12: Nonmagnetic Material C)
In Example 24-26, a target having a composition of 18.75 Fe-18.75 Ge-62.5 C (at%), and in Example 24, a pure Ge target in Example 24, and in Example 25, a composition of 50 Ag-50 Ge (at. %) In Example 26, a target having a composition of 50 Ni-50 Ge (at%) was prepared. Then, the above two targets were alternately sputtered by a sputtering apparatus so that the composition of the entire sputtered film had the following composition, to form a laminated film on a silicon substrate. On the other hand, in Comparative Example 12, sputter deposition was performed using only a target having a composition of 18.75 Fe-18.75 Ge-62.5 C (at%).
Example 24: 18Fe-18Pt-4Ge-60C (at%)
Example 25: 18Fe-18Pt-2Ag-2Ge-60C (at%)
Example 26: 18Fe-18Pt-2Ni-2Ge-60C (at%)
Comparative Example 12: 18.75 Fe-18.75 Ge-62.5 C (at%)
Sputtering conditions were: input power: 1 kW, Ar gas pressure: 1.7 Pa, and film formation was performed for a total of 20 seconds on a silicon substrate. Thereafter, the thin film on the substrate is heated at 500 ° C. for 1 hour in a high vacuum furnace and then analyzed by XRD (X-ray diffraction method). Peak was confirmed. However, for the thin film of Comparative Example 12, no peak of the Fe-Pt ordered phase was confirmed.

The results of the above are summarized in Table 2.

Magnetic thin film was deposited by sputtering of the present invention has an excellent effect of heat treatment temperature for expressing an L1 ₀ ordered structure is low. The magnetic film of the present invention is particularly useful as a recording film of a magnetic recording medium.

Claims (7)

A magnetic film consisting of a magnetic metal containing Fe and Pt and a nonmagnetic material, further containing Mg as a metal, and having an atomic ratio of (Fe _1-α Pt _α ) _{1 -β} Mg _β (α, β is A magnetic film characterized by having a composition represented by 0.35 ≦ α ≦ 0.55, and a number satisfying 0.01 ≦ β ≦ 0.2. A magnetic film composed of a magnetic metal containing Fe and Pt and a nonmagnetic material, further containing Ge as a metal, and having an atomic ratio of (Fe _{1 -α} Pt _α ) _{1 -β} Ge _β (α, β is A magnetic film characterized by having a composition represented by 0.35 ≦ α ≦ 0.55, and a number satisfying 0.01 ≦ β ≦ 0.2. A magnetic film composed of a magnetic metal containing Fe and Pt and a nonmagnetic material, further containing Pd as a metal, and having an atomic ratio of (Fe _{1 -α} Pt _α ) _{1 -β} Pd _β (α, β is A magnetic film characterized by having a composition represented by 0.35 ≦ α ≦ 0.55, and a number satisfying 0.01 ≦ β ≦ 0.2.   The magnetic film according to any one of claims 1 to 3, wherein the ordering temperature is 500 ° C or less. L1 ₀ structure type magnetic film according to claim 1 having a crystal structure.   The nonmagnetic material is at least one selected from carbon, carbide, oxide and nitride, and the volume ratio of the nonmagnetic material is 10 to 60 vol% with respect to the total amount of the film. The magnetic film according to any one of claims 1 to 5. A method for producing a magnetic film according to any one of claims 1 to 6, wherein a film obtained by sputtering a sputtering target is heat-treated at a temperature of 500 ° C or less in vacuum. A method of manufacturing a magnetic film characterized by