Sputtering target for magnetic recording film
09683284 ยท 2017-06-20
Assignee
Inventors
Cpc classification
C22C38/002
CHEMISTRY; METALLURGY
C22C30/00
CHEMISTRY; METALLURGY
C23C14/3407
CHEMISTRY; METALLURGY
C22C33/0278
CHEMISTRY; METALLURGY
C22C33/0228
CHEMISTRY; METALLURGY
C23C14/3414
CHEMISTRY; METALLURGY
International classification
C22C30/00
CHEMISTRY; METALLURGY
Abstract
A sputtering target for a magnetic recording film which contains carbon, the sputtering target is characterized in that the ratio (I.sub.G/I.sub.D) of peak intensities of the G-band to the D-band in Raman scattering spectrometry is 5.0 or less. The sputtering target for a magnetic recording film, which contains carbon powders dispersed therein, makes it possible to produce a magnetic thin film having a granular structure without using an expensive apparatus for co-sputtering; and in particular, the target is an FePt-based sputtering target. Carbon is a material which is difficult to sinter and has a problem that carbon particles are apt to form agglomerates. There is hence a problem that carbon masses are readily detached during sputtering to generate a large number of particles on the film after sputtering. The high-density sputtering target can solve these problems.
Claims
1. A sputtering target for a magnetic recording film, the sputtering target having a composition comprising 5 mol % or more and 60 mol % or less of Pt, 20 mol % or more and 70 mol % or less of C, and the balance of Fe, and having a ratio (I.sub.G/I.sub.D) of a peak intensity of G-band (I.sub.G) to a peak intensity of D-band (I.sub.D) of 5.0 or less in Raman scattering spectrometry of the sputtering target, and having a relative density of 90% or more.
2. A sputtering target for a magnetic recording film, the sputtering target having a composition comprising 0.5 mol % or more and 20 mol % or less of at least one element selected from the group consisting of B, Ru, Ag, Au, and Cu, 5 mol % or more and 60 mol % or less of Pt, 20 mol % or more and 70 mol % or less of C, and Fe, and having a ratio (I.sub.G/I.sub.D) of a peak intensity of G-band (I.sub.G) to a peak intensity of D-band (I.sub.D) of 5.0 or less in Raman scattering spectrometry of the sputtering target.
3. The sputtering target for a magnetic recording film according to claim 2, wherein the sputtering target further comprises 0.5 mol % or more and 20 mol % or less of at least one oxide selected from the group consisting of SiO.sub.2, Cr.sub.2O.sub.3, CoO, Ta.sub.2O.sub.5, B.sub.2O.sub.3, MgO, and Co.sub.3O.sub.4.
4. The sputtering target for a magnetic recording film according to claim 2, wherein the sputtering target has a relative density of 90% or more.
5. A sputtering target for a magnetic recording film, the sputtering target having a composition comprising 0.5 mol % or more and 20 mol % or less of at least one oxide selected from the group consisting of SiO.sub.2, Cr.sub.2O.sub.3, CoO, Ta.sub.2O.sub.5, B.sub.2O.sub.3, MgO, and Co.sub.3O.sub.4, 5 mol % or more and 60 mol % or less of Pt, 20 mol % or more and 70 mol % or less of C, and the balance of Fe, and having a ratio (I.sub.G/I.sub.D) of a peak intensity of G-band (I.sub.G) to a peak intensity of D-band (I.sub.D) of 5.0 or less in Raman scattering spectrometry of the sputtering target.
6. The sputtering target for a magnetic recording film according to claim 5, wherein the sputtering target has a relative density of 90% or more.
7. The sputtering target according to claim 1, wherein the 20 mol % or more and 70 mol % or less of C is in the form of carbon black.
8. The sputtering target according to claim 1, wherein the 20 mol % or more and 70 mol % or less of C is in the form of glassy carbon.
9. The sputtering target according to claim 1, wherein the 20 mol % or more and 70 mol % or less of C is in the form of graphite.
10. The sputtering target according to claim 1, wherein the sputtering target is a sintered compact of raw material powders having been mixed, pulverized, compacted, and sintered.
Description
BRIEF DESCRIPTION OF DRAWING
(1)
(2)
(3)
(4)
(5)
(6)
DETAILED DESCRIPTION OF THE INVENTION
(7) A common carbon material excluding diamond has a strong covalent bond involving an sp.sup.2 hybrid orbital, and it is difficult to cleave the covalent bond even in sputtering. Consequently, it is believed that masses of carbon atoms bound with covalent bonds fly directly as particles during sputtering.
(8) Then, the present inventors came to think that intentional destruction of the crystallinity of carbon can improve the sputtering characteristics of the carbon material and reduce the occurrence of particles during sputtering; and found that the intensity ratio of the G (graphite) band to the D (disorder) band obtained in Raman scattering spectrometry of a sintered compact containing carbon shows a correlation with the number of particles generated during sputtering.
(9) Accordingly, the sputtering target for a magnetic recording film of the present invention contains carbon (C), and the ratio (I.sub.G/I.sub.D) of peak intensities of the G-band to the D-band in Raman scattering spectrometry of the sputtering target is 5.0 or less.
(10) Such a case is particularly effective in a sputtering target for a magnetic recording film composed of C and a metal component having a composition including 5 mol % or more and 60 mol % or less of Pt and the balance of Fe. The contents of these components are requirements for providing satisfactory magnetic characteristics.
(11) The content of C is preferably 5 mol % or more and 70 mol % or less. A content of C in a target composition of less than 5 mol % may not provide sufficient magnetic characteristics, whereas a content of higher than 70 mol % may cause agglomerates of C powders to increase the occurrence of particles. In order to obtain desired magnetic characteristics, the content of C is desirably 20 mol % or more and 70 mol % or less.
(12) The sputtering target for a magnetic recording film can have a relative density of 90% or more. The relative density of 90% or more is one of requirements of the present invention. A high relative density prevents the problem caused by degassing from the sputtering target during sputtering and enhances the adhesion between the alloy and the C powders. As a result, occurrence of particles is effectively prevented. The relative density is more preferably 95% or more.
(13) The relative density in the present invention is a value determined by dividing the measured density of a target by the calculated density (theoretical density). The calculated density is a density when it is assumed that the constituent elements of a target do not diffuse to or react with each other and is calculated by the following on:
calculated density=[(atomic weight of a constituent element)(atomic ratio of the constituent element)]/[(atomic weight of the constituent element)(atomic ratio of the constituent element)/(literature density data of the constituent element)],Expression
wherein, means the sum of the values of all constituent elements of the target.
(14) The sputtering target for a magnetic recording film may further contain 0.5 mol % or more and 20 mol % or less of at least one additional element selected from B, Ru, Ag, Au, and Cu. The addition of these elements is optional, and these elements can be added depending on the sputtering target material for improving the magnetic characteristics.
(15) The sputtering target for a magnetic recording film may further contain 0.5 mol % or more and 20 mol % or less of at least one oxide additive selected from SiO.sub.2, Cr.sub.2O.sub.3, CoO, Ta.sub.2O.sub.5, B.sub.2O.sub.3, MgO, and Co.sub.3O.sub.4. The addition of these oxides is optional, and these oxides can be added depending on the sputtering target material for improving the magnetic characteristics.
(16) As described above, it is difficult to cleave the covalent bond involving an sp.sup.2 hybrid orbital in a carbon material even in sputtering. Thus, the covalent bond involving an sp.sup.2 hybrid orbital in the carbon material is destroyed in advance for allowing the bonds between carbon atoms to be readily cleaved during sputtering. This prevents carbon from flying in large masses, resulting in a reduction of particles.
(17) On this occasion, Raman scattering spectrometry can be employed as an index for evaluating the crystallinity (completeness of the sp.sup.2 hybrid orbital) of a carbon material.
(18) In evaluation of the crystallinity of a carbon material by Raman scattering spectrometry, vibration modes called G-band and D-band are measured.
(19) The G-band is a vibration mode originated from the six-membered ring structure of graphite and appears as a peak at approximately 1570 cm.sup.1. The peak intensity increases with an increase in completeness of the crystalline structure.
(20) The D-band is a vibration mode originated from the defect structure of graphite and appears as a peak at approximately 1350 cm.sup.1. The peak intensity increases with an increase of the defect.
(21)
(22) In the curve fitting of the measurement results, a Lorentz function was used.
(23) A D-band also appears at approximately 1620 cm.sup.1 and is a vibration mode originated from a defect structure of graphite, but it does not directly relate to the present invention. As a matter of convenience of curve fitting, the D-band is not used in the curve fitting and is merely shown in the figure.
(24) In the present invention, the vibration modes of G-band and D-band in Raman scattering spectrometry are measured using a laser excitation wavelength of 532 nm. The excitation light source may be a gas laser such as an Ar laser, a HeNe laser, or a Kr laser. These lasers can be appropriately selected depending on the desired excitation wavelength.
(25) In the Raman spectrum of this case, an intensity I.sub.G of the G-band having a peak at 1520 to 1600 cm.sup.1 and an intensity I.sub.D of the D-band having a peak at 1320 to 1450 cm.sup.1 appear. The present invention can be applied to such a case.
(26) From the above, the crystallinity of a carbon material can be evaluated by calculating the ratio of peak intensities of the G-band to the D-band (hereinafter, referred to as I.sub.G/I.sub.D ratio). That is, a carbon material having higher crystallinity has a higher I.sub.G/I.sub.D ratio. A crystalline structure having higher completeness (higher crystallinity) has a higher intensity of the G-band, and a crystalline structure having lower completeness (lower crystallinity) has a lower intensity of the G-band.
(27) As obvious from the above, in the present invention, the crystallinity is reduced, namely, the crystallinity of a carbon material is intentionally destroyed to improve the sputtering characteristics and to reduce occurrence of particles during sputtering, and the ratio (I.sub.G/I.sub.D) of peak intensities of the G-band to the D-band in Raman scattering spectrometry of the sputtering target is reduced to 5.0 or less.
(28) As a result, a problem that carbon is apt to form agglomerates is solved, and it is possible to prevent carbon masses from readily detaching during sputtering and to prevent a large amount of particles from occurring on the film after sputtering.
(29) The lower limit of the ratio (I.sub.G/I.sub.D) of peak intensities of the G-band to the D-band is not particularly limited and is 1 or higher in many cases. A ratio (I.sub.G/I.sub.D) of peak intensities of 5.0 or less can effectively prevent occurrence of particles.
(30) The sputtering target of the present invention is produced by a powder sintering method. Prior to the production, each raw material powder such as a typical example of a Fe, Pt and C powder is prepared. The Fe powder and the Pt powder desirably have an average particle diameter of 0.5 m or more and 10 m or less. If these raw material powders have too small particles, oxidation is facilitated to cause, for example, a problem of increasing the oxygen concentration in the sputtering target. Thus, the diameter is desirably 0.5 m or more.
(31) In contrast, if these raw material powders have large particle diameters, it is difficult to finely disperse C powders in the alloy. Thus, the particle diameter is further desirably 10 m or less.
(32) The C powder can be carbon black having an average primary particle diameter of 30 to 50 nm, graphite having an average particle diameter of 1 to 100 m, or glassy carbon having an average particle diameter of 0.4 to 100 m. The usable type of the C powder is not particularly limited. The C powder is appropriately selected and used depending on the type of the target.
(33) Furthermore, as the raw material powder, an alloy powder such as a FePt powder, a FeCu powder, a PtCu powder, or a FePtCu powder may be used. These alloy powders also optionally contain various materials described in paragraphs [0024] and [0025] for improving the magnetic characteristics.
(34) Though it depends on the composition, among the alloy powders, in particular, an alloy powder containing Pt is effective for reducing the amount of oxygen in the raw material powder. In also the case of using an alloy powder, the powder desirably has an average particle diameter of 0.5 m or more and 10 m or less.
(35) Subsequently, the above-mentioned powders are weighed to give a desired composition and are mixed and pulverized by a technique such as a ball mill. The mixing and pulverization are important. That is, the crystallinity of the carbon material is intentionally destroyed by simultaneously mixing the carbon material and the matrix materials with a ball mill. On this occasion, the crystallinity of the carbon material is controlled by selecting the mixing time and the carbon material.
(36) The thus prepared powder mixture is molded and sintered by hot pressing. Instead of the hot pressing, plasma arc sintering or hot hydrostatic pressure sintering may be employed. Though it depends on the composition of a sputtering target, the retention temperature for the sintering is in a range of 1200 to 1500 C. in many cases. The applied pressure is 25 MPa to 35 MPa. Under such sintering conditions, it is also necessary to prevent agglomerate formation of the C powders.
(37) The sintered compact taken out from the hot press is subjected to hot isostatic pressing. The hot isostatic pressing is effective for increasing the density of the sintered compact. The retention temperature in the hot isostatic pressing depends on the composition of the sintered compact and is in the range of 1000 to 1500 C. in many cases. The applied pressure is set to 100 MPa or more.
(38) The thus prepared sintered compact is processed into a desired shape with a lathe so as to be able to produce a sputtering target of the present invention.
(39) It is thus possible to produce a sputtering target for a magnetic recording film, the sputtering target including C powders uniformly and finely dispersed in an alloy, having a high density, and showing a ratio (I.sub.G/I.sub.D) of peak intensities of the G-band to the D-band of 5.0 or less in Raman scattering spectrometry. The thus-produced sputtering target of the present invention is useful as a sputtering target for forming a magnetic thin film having a granular structure.
EXAMPLES
(40) The present invention will now be described by examples and comparative Examples. These examples are merely exemplary and are not intended to limit the scope of the invention. That is, the present invention is limited only by the claims and encompasses various modifications in addition to examples included in the present invention.
Comparative Example 1
(41) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, and carbon black having an average primary particle diameter of 48 nm were prepared as raw material powders. In Comparative Example 1, these powders were weighed to give a composition of 30Fe-30Pt-40C (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(42) Subsequently, the weighed powders were placed in a mortar and were mixed and pulvelized for 4 hours. The powder mixture taken out from the mortar was charged in a carbon mold and was hot pressed.
(43) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber and was then hot isostatic pressed at 1100 C. and 150 MPa. The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 93.6%.
(44) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(45) The curve fitting of the measurement results was performed using a Lorentz function.
(46) The I.sub.G/I.sub.D ratio determined from
(47) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(48) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter and was 19600, as shown in the Table 1.
(49) TABLE-US-00001 TABLE 1 Number Hot press HIP Composition Type of of temperature temperature (mol %) carbon I.sub.G I.sub.D I.sub.G/I.sub.D particles ( C.) ( C.) Comparative Fe30Pt40C carbon black 16228.2 3166.7 5.12 19600 1400 1100 Example 1 Comparative Fe30Pt40C graphite 1 urn 16135 2768.4 5.83 21600 1400 1100 Example 2 Comparative Fe30Pt40C graphite 20 um 19256 2973.8 6.48 28600 1400 1100 Example 3 Example 1 Fe30Pt40C graphite 1um 9441 1904.6 4.96 490 1400 1100 Example 2 Fe30Pt40C carbon black 6565.7 1573.6 4.17 350 1400 1100 Example 3 Fe30Pt40C glassy carbon 5163.3 1483.5 3.48 330 1400 1100 Example 4 Fe30Pt40C graphite 20 um 7121.3 2340.5 3.04 250 1400 1100 Example 5 Fe60Pt10C carbon black 8617.1 2215.1 3.89 80 1400 1100 Example 6 Fe60Pt20C carbon black 7031.7 1819.7 3.86 165 1400 1100 Example 7 Fe60Pt5C carbon black 5822.8 2103.3 2.77 35 1400 1100 Example 8 Fe34Pt2B30C carbon black 6055 1915.2 3.16 280 1400 1100 Example 9 Fe35Pt5Ru25C carbon black 7311.7 1809.4 4.04 200 1400 1100 Example 10 Fe35Pt10Ag30C carbon black 8877.1 8049.6 1.10 305 950 950 Example 11 Fe34Pt2Au30C carbon black 7133.6 1971.4 3.62 270 1400 1100 Example 12 Fe30Pt10Cu30C carbon black 8622.1 2349.8 3.67 300 1400 1100 Example 13 Fe25Pt20Ru5C carbon black 5369.9 1682.4 3.19 25 1400 1100 Example 14 Fe34Pt20C5TiO.sub.25SiO.sub.22Cr.sub.2O.sub.3 carbon black 6606.4 1996.6 3.31 75 1100 1100 Example 15 Fe35Pt20C5Ta.sub.2O.sub.55SiO.sub.2 carbon black 6956.8 2169.2 3.21 60 1100 1100 Example 16 Fe40Pt20C2B.sub.2O.sub.33CoO carbon black 7433 1986.7 3.74 65 1100 1100 Example 17 Fe31Pt20C5SiO.sub.23Co.sub.3O.sub.4 carbon black 8651.7 2729.4 3.17 80 1100 1100 Example 18 Fe25Pt50C carbon black 9384.5 2233.4 4.20 670 1400 1100 Example 19 Fe20Pt60C carbon black 9124.9 2160.6 4.22 980 1400 1100
Comparative Example 2
(50) A Fe powder having an average particle diameter of 3 m, a Pt powder havingan average particle diameter of 3 m, and graphite having an average particle diameter of 1 m were prepared as raw material powders. In Comparative Example 2, these powders were weighed to give a composition of 30Fe-30Pt-40C (mol %) and the total weight of 2600 g. The graphite used as the C powder was commercially available one.
(51) Subsequently, the weighed powders were placed in a mortar and were mixed and pulvelized for 4 hours. The powder mixture taken out from the mortar was charged in a carbon mold and was hot pressed.
(52) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber and was then hot isostatic pressed at 1100 C. and 150 MPa. The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 94.2%.
(53) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(54) The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtC in Comparative Example 2 and the result of curve fitting thereof. As obvious from Table 1, the I.sub.G/I.sub.D ratio was 5.83, which was higher than 5.0 defined in the present invention.
(55) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(56) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 21600 as shown in Table 1.
Comparative Example 3
(57) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, graphite having an average particle diameter of 20 mwere prepared as raw material powders. In Comparative Example 3, these powders were weighed to give a composition of 30Fe-30Pt-40C (mol %) and the total weight of 2600 g. The graphite used as the C powder was commercially available one.
(58) Subsequently, the weighed powders were placed in a mortar and were mixed and pulvelized for 4 hours. The powder mixture taken out from the mortar was charged in a carbon mold and was hot pressed.
(59) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber and was then hot isostatic pressed at 1100 C. and 150 MPa. The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 93.8%.
(60) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(61) The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtC in Comparative Example 3 and the result of curve fitting thereof As obvious from Table 1, the I.sub.G/I.sub.D ratio was 6.48, which was higher than 5.0 defined in the present invention.
(62) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(63) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 28600 as shown in Table 1.
Example 1
(64) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, graphite having an average particle diameter of 1 m, were prepared as raw material powders. In Example 1, these powders were weighed to give acomposition of 30Fe-30Pt-40C (mol %) and the total weight of 2600 g. The graphite used as the C powder was commercially available one.
(65) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(66) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(67) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(68) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 96.6%.
(69) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(70) The curve fitting of the measurement results was performed using a Lorentz function.
(71) Table 1 shows the I.sub.G/I.sub.D ratio determined from
(72) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(73) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 490 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 2
(74) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, carbon black having an average primary particle diameter of 48 nm were prepared as raw material powders. In Example 2, these powders were weighed to give a composition of 30Fe-30Pt-40C (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(75) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(76) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(77) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(78) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 96.9%.
(79) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(80) The curve fitting of the measurement results was performed using a Lorentz function.
(81) Table 1 shows the I.sub.G/I.sub.D ratio determined from
(82) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(83) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 350 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 3
(84) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, and glassy carbon having an average particle diameter of 80 m were prepared as raw material powders. In Example 3, these powders were weighed to give a composition of 30Fe-30Pt-40C (mol %) and the total weight of 2600 g. The amorphous carbon used as the C powder was commercially available one.
(85) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(86) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(87) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(88) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 96.8%.
(89) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(90) The curve fitting of the measurement results was performed using a Lorentz function.
(91) Table 1 shows the I.sub.G/I.sub.D ratio determined from
(92) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(93) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 330 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 4
(94) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, and graphite having an average particle diameter of 20 m were prepared as raw material powders. In Example 4, these powders were weighed to give a composition of 30Fe-30Pt-40C (mol %) and the total weight of 2600 g. The graphite used as the C powder was commercially available one.
(95) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(96) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(97) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(98) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 97.1%.
(99) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(100) The curve fitting of the measurement results was performed using a Lorentz function.
(101) Table 1 shows the I.sub.G/I.sub.D ratio determined from
(102) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(103) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 330 as shown in Table 1, which was notably reduced compared with Comparative Examples.
(104) As shown in Examples above, the ratio (I.sub.G/I.sub.D) of peak intensities of the G-band to the D-band in Raman scattering spectrometry was 5.0 or less, and also there was a tendency that the number of particles decreases with a reduction of the intensity ratio.
(105) From the results above, intentional destruction of the crystallinity of carbon has excellent effects of improving the sputtering characteristics of the carbon material and reducing the occurrence of particles during sputtering.
Example 5
(106) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, carbon black having an average primary particle diameter of 48 nm were prepared as raw material powders. In Example 5, these powders were weighed to give a composition of 30Fe-60Pt-10C (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(107) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(108) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(109) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(110) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 98.2%.
(111) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(112) The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtC in Example 5 and the result of curve fitting thereof. As obvious from Table 1, the I.sub.G/I.sub.D ratio was 3.89, which satisfied the I.sub.G/I.sub.D ratio condition of 5.0 or less of the present invention.
(113) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(114) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 80 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 6
(115) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, and carbon black having an average primary particle diameter of 48 m were prepared as raw material powders. In Example 6, these powders were weighed to give a composition of 20Fe-60Pt-20C (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(116) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(117) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(118) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(119) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 97.7%.
(120) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(121) The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtC in Example 6 and the result of curve fitting thereof. As obvious from Table 1, the I.sub.G/I.sub.D ratio was 3.86, which satisfied the I.sub.G/I.sub.D ratio condition of 5.0 or less of the present invention.
(122) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(123) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 165 as shown in Table 1 which was notably reduced compared with Comparative Examples.
Example 7
(124) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, and carbon black having an average primary particle diameter of 48 nm were prepared as raw material powders. In Example 7, these powders were weighed to give a composition of 35Fe-60Pt-5C (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(125) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(126) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(127) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(128) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 99.2%.
(129) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm. The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtC in Example 7and the result of curve fitting thereof As obvious from Table 1, the I.sub.G/I.sub.D ratio was 2.77, which satisfied the I.sub.G/I.sub.D ratio condition of 5.0 or less of the present invention.
(130) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(131) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 35 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 8
(132) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, a B powder having an average particle diameter of 10 m, and carbon black having an average primary particle diameter of 48 nm were prepared as raw material powders. In Example 8, these powders were weighed to give a composition of 34Fe-34Pt-2B-30C (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(133) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(134) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(135) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(136) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 97.3%.
(137) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 Umm.
(138) The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtB-C in Example 8 and the result of curve fitting thereof. As obvious from Table 1, the I.sub.G/I.sub.D ratio was 3.16, which satisfied the I.sub.G/I.sub.D ratio condition of 5.0 or less of the present invention.
(139) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(140) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 280 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 9
(141) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, a Ru powder having an average particle diameter of 3 m, and carbon black having an average primary particle diameter of 48 nm were prepared as raw material powders. In Example 9, these powders were weighed to give a composition of 35Fe-35Pt-5Ru-25C(mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(142) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(143) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(144) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(145) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 98.0%.
(146) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(147) The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtRuC in Example 9 and the result of curve fitting thereof. As obvious from Table 1, the I.sub.G/I.sub.D ratio was 4.04, which satisfied the I.sub.G/I.sub.D ratio condition of 5.0 or less of the present invention.
(148) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(149) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 200 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 10
(150) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, an Ag powder having an average particle diameter of 3 m, and carbon black having an average primary particle diameter of 48 nm were prepared as raw material powders. In Example 10, these powders were weighed to give a composition of 25Fe-35Pt-10Ag-30C (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(151) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(152) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 950 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(153) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 950 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 950 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(154) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 96.1%.
(155) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(156) The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtAgC in Example 10 and the result of curve fitting thereof. As obvious from Table 1, the I.sub.G/I.sub.D ratio was 1.10, which satisfied the I.sub.G/I.sub.D ratio condition of 5.0 or less of the present invention.
(157) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(158) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 305 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 11
(159) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, an Au powder having an average particle diameter of 5 m, and carbon black having an average primary particle diameter of 48 nm were prepared as raw material powders. In Example 11, these powders were weighed to give a composition of 34Fe-34Pt-2Au-30C (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(160) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(161) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(162) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(163) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 972%.
(164) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(165) The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtAuC in Example 11 and the result of curve fitting thereof. As obvious from Table 1, the I.sub.G/I.sub.D ratio was 3.62, which satisfied the I.sub.G/I.sub.D ratio condition of 5.0 or less of the present invention.
(166) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(167) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 270 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 12
(168) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, a Cu powder having an average particle diameter of 5 m, and carbon black having an average primary particle diameter of 48 nm were prepared as raw material powders. In Example 12, these powders were weighed to give a composition of 30Fe-30Pt-10Cu-30C (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(169) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(170) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(171) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(172) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 97.9%.
(173) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(174) The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtCuC in Example 12 and the result of curve fitting thereof. As obvious from Table 1, the I.sub.G/I.sub.D ratio was 3.67, which satisfied the I.sub.G/I.sub.D ratio condition of 5.0 or less of the present invention.
(175) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(176) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 300 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 13
(177) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, a Ru powder having an average particle diameter of 3 m, and carbon black having an average primary particle diameter of 48 nm were prepared as raw material powders. In Example 13, these powders were weighed to give a composition of 50Fe-25Pt-20Ru-5C (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(178) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(179) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(180) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(181) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 99.3%.
(182) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(183) The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtRuC in Example 13 and the result of curve fitting thereof. As obvious from Table 1, the I.sub.G/I.sub.D ratio was 3.19, which satisfied the I.sub.G/I.sub.D ratio condition of 5.0 or less of the present invention.
(184) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(185) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 25 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 14
(186) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, carbon black having an average primary particle diameter of 48 nm, and oxide powders, i.e., a TiO.sub.2 powder having an average particle diameter of 1 m, a SiO.sub.2 powder having an average particle diameter of 0.5 m, and a Cr.sub.2O.sub.3 powder having an average particle diameter of 1 m, were prepared as raw material powders. In Example 14, these powders were weighed to give a composition of 34Fe-34Pt-20C-5TiO.sub.2-5SiO.sub.2-2Cr.sub.2O.sub.3 (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(187) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(188) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(189) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(190) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 98.1%.
(191) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(192) The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtCTiO.sub.2SiO.sub.2Cr.sub.2O.sub.3 in Example 14 and the result of curve fitting thereof. As obvious from Table 1, the I.sub.G/I.sub.D ratio was 3.31, which satisfied the I.sub.G/I.sub.D ratio condition of 5.0 or less of the present invention.
(193) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(194) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 75 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 15
(195) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, carbon black having an average primary particle diameter of 48 nm, and oxide powders, i.e., a Ta.sub.2O.sub.5 powder having an average particle diameter of 1 m and a SiO.sub.2 powder having an average particle diameter of 0.5 m, were prepared as raw material powders. In Example 15, these powders were weighed to give a composition of 35Fe-35Pt-20C-5Ta.sub.2O.sub.5-5SiO.sub.2 (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(196) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(197) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(198) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(199) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 98.3%.
(200) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 Umm.
(201) The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtCTa.sub.2O.sub.5SiO.sub.2 in Example 15 and the result of curve fitting thereof. As obvious from Table 1, the I.sub.G/I.sub.D ratio was 3.21, which satisfied the I.sub.G/I.sub.D ratio condition of 5.0 or less of the present invention.
(202) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(203) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 60 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 16
(204) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, carbon black having an average primary particle diameter of 48 nm, and oxide powders, i.e., a B.sub.2O.sub.3 powder having an average particle diameter of 10 m and a CoO powder having an average particle diameter of 1 m, were prepared as raw material powders. In Example 16, these powders were weighed to give a composition of 35Fe-40Pt-20C-2B.sub.2O.sub.3-3CoO (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(205) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(206) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(207) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(208) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 97.9%.
(209) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(210) The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtCB.sub.2O.sub.3CoO in Example 16 and the result of curve fitting thereof. As obvious from Table 1, the I.sub.G/I.sub.D ratio was 3.74, which satisfied the I.sub.G/I.sub.D ratio condition of 5.0 or less of the present invention.
(211) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(212) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 65 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 17
(213) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, carbon black having an average primary particle diameter of 48 nm, and oxide powders, i.e., a SiO.sub.2 powder having an average particle diameter of 0.5 m and a Co.sub.3O.sub.4 powder having an average particle diameter of 1 m, were prepared as raw material powders. In Example 17, these powders were weighed to give a composition of 41Fe-31Pt-20C-5SiO.sub.2-3Co.sub.3O.sub.4 (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one .
(214) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(215) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(216) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(217) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 98.4%.
(218) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm. The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtCSiO.sub.2Co.sub.3O.sub.4 in Example 17 and the result of curve fitting thereof. As obvious from Table 1, the I.sub.G/I.sub.D ratio was 3.17, which satisfied the I.sub.G/I.sub.D ratio condition of 5.0 or less of the present invention.
(219) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(220) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 80 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 18
(221) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, and carbon black having an average primary particle diameter of 48 nm were prepared as raw material powders. In Example 18, these powders were weighed to give a composition of 25Fe-25Pt-50C (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(222) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(223) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(224) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(225) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 96.1%.
(226) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(227) The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtC in Example 18 and the result of curve fitting thereof. As obvious from Table 1, the I.sub.G/I.sub.D ratio was 4.20, which satisfied the I.sub.G/I.sub.D ratio condition of 5.0 or less of the present invention.
(228) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(229) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 670 as shown in Table 1, which was notably reduced compared with Comparative Examples.
Example 19
(230) A Fe powder having an average particle diameter of 3 m, a Pt powder having an average particle diameter of 3 m, and carbon black having an average primary particle diameter of 48 nm were prepared as raw material powders. In Example 19, these powders were weighed to give a composition of 20Fe-20Pt-60C (mol %) and the total weight of 2600 g. The carbon black used as the C powder was commercially available one.
(231) Subsequently, the weighed powders were charged in a 10-Liter ball mill pot together with zirconia balls as a pulverizing medium, and mixed and pulverized by rotating for 4 hours. The powder mixture taken out from the ball mill was charged in a carbon mold and was hot pressed.
(232) The conditions of hot pressing were a vacuum atmosphere, a rate of temperature increase of 300 C./hour, a retention temperature of 1400 C., a retention time of 2 hours, and a pressure of 30 MPa from the start of the increase in temperature until the end of the retention. After the completion of the retention, the hot pressed powder was naturally cooled inside the chamber.
(233) The sintered compact taken out from the mold for hot pressing was hot isostatic pressed under conditions of a rate of temperature increase of 300 C./hour, a retention temperature of 1100 C., and a retention time of 2 hours, with gradually increasing the Ar gas pressure from the start of the increase in temperature and maintaining the Ar gas pressure at 150 MPa during the retention at 1100 C. After the completion of the retention, the sintered compact was naturally cooled inside the furnace.
(234) The density of the thus produced sintered compact was measured by an Archimedes method, and the relative density calculated was 95.9%.
(235) The sintered compact was cut with a lathe to give a target having a diameter of 180.0 mm and a thickness of 5.0 mm. The conditions for Raman scattering spectrometry of the target were an excitation wavelength of 532 nm, an output of 5 mW, and diffraction grating of 1800 L/mm.
(236) The curve fitting of the measurement results was performed using a Lorentz function. Table 1 shows the I.sub.G/I.sub.D ratio determined from the Raman scattering spectrum of FePtC in Example 19 and the result of curve fitting thereof. As obvious from Table 1, the I.sub.G/I.sub.D ratio was 4.22, which satisfied the I.sub.G/I.sub.D ratio condition of 5.0 or less of the present invention.
(237) The target was set in a magnetron sputtering apparatus (C-3010 sputtering system, manufactured by Canon ANELVA Corporation) and was sputtered.
(238) Under sputtering conditions of an applied power of 1 kW and an Ar gas pressure of 1.7 Pa, after presputtering at 2 kWhr, a film was formed on an aluminum substrate having a diameter of 3.5 inches for 20 seconds. The number of particles adhered onto the substrate was counted with a particle counter, and was 980 as shown in Table 1, which was notably reduced compared with Comparative Examples.
(239) The sputtering target for a magnetic recording film of the present invention allows production of a magnetic thin film having a granular structure without using an expensive co-sputtering apparatus. The invention can provide a sputtering target, in particular, FePt-based sputtering target, for a magnetic recording film, where C powders are dispersed in the target. The sputtering target has an excellent effect of solving the problems that Carbon is a material which is difficult to sinter and is apt to form agglomerates and that carbon masses are readily detached during sputtering to generate a large number of particles on the film after sputtering. Accordingly, the sputtering target is useful for forming a magnetic thin film having a granular structure.