TW201510257A - Sputtering target for magnetic recording medium - Google Patents

Abstract

A sintered sputtering target containing a Fe-Pt alloy and a non-magnetic material as the main components, said sintered sputtering target being characterized in that at least C (carbon) is contained as the non-magnetic material, an additional trace element other than the above-mentioned main components is contained in an amount of 50 to 5000 ppm by mass, and the standard free energy of formation ([Delta]G DEG ) of the additional trace element per 1 mole of carbon in a carbide is -5000 [cal/mol] or less. The present invention addresses the problem of providing a sputtering target which undergoes the formation of particles in a greatly reduced amount upon sputtering and contains a Fe-Pt alloy and a non-magnetic material as the main components.

Description

Sputter target for magnetic recording media

The present invention relates to a sputtering target for forming a magnetic thin film in a magnetic recording medium.

In the field of magnetic recording represented by a hard disk drive machine, a material of a magnetic film of a magnetic recording medium has been mainly made of a material having a ferromagnetic metal Co, Fe or Ni as a base. For example, a magnetic film of a hard disk using a horizontal magnetic recording method is a Co-Cr-based or Co-Cr-Pt-based ferromagnetic alloy containing Co as a main component.

Further, a magnetic material of a hard disk having a perpendicular magnetic recording method which has been put into practical use in recent years is often a composite material composed of a Co-Cr-Pt-based ferromagnetic alloy having a main component of Co and an oxide. Further, since the magnetic properties are high, the magnetic thin film is often produced by sputtering a sputtering target having the above-mentioned material as a component by a magnetron sputtering apparatus.

On the other hand, the recording density of hard disks has rapidly increased year by year, surpassing 1Tbit/in ² . If the recording density reaches 1 Tbit/in ² , the size of the recording bit will be less than 10 nm, and it is expected that superparamagnetization caused by thermal fluctuations in this case will become a problem. It is also expected that the material of the magnetic recording medium used today, for example, a material in which Pt is added to a Co-based alloy to increase crystal magnetic anisotropy is not sufficient.

The reason for this is that magnetic particles which are stably magnetized with a size of 10 nm or less are required to have higher crystal magnetic anisotropy.

For the above reasons, an Fe-Pt alloy having an L1 ₀ structure has been attracting attention as a material for an ultrahigh-density recording medium. The Fe-Pt alloy having the L1 ₀ structure not only has high crystal magnetic anisotropy, but also has excellent corrosion resistance and oxidation resistance, and therefore is expected to be suitable as a material for a magnetic recording medium.

Further, when a Fe-Pt alloy having an L1 ₀ structure is used as a material for an ultrahigh-density recording medium, it is required to develop a technique in which a Fe-Pt magnetic particle regularized in an L1 ₀ structure is magnetically isolated. The direction is as high as possible and the direction is uniform and dispersed.

Therefore, a granular magnetic film having an isolated structure of Fe-Pt magnetic particles having an L1 ₀ structure is proposed as a non-magnetic material such as C (carbon) or oxide, and is proposed as a next generation hard using a thermally assisted magnetic recording method. The magnetic recording medium of the disc is used. The granular magnetic film has a structure in which a magnetic interaction between magnetic particles is blocked by surrounding a magnetic particle with a non-magnetic material.

A magnetic recording medium having a magnetic film having a granular structure and a related document related thereto include Patent Document 1, Patent Document 2, Patent Document 3, Patent Document 4, and Patent Document 5.

In the granular magnetic thin film having the Fe-Pt magnetic particles having the L1 ₀ structure, the magnetic thin film containing C as a nonmagnetic material is attracting attention because of its particularly high magnetic properties. However, if a sputtering target composed of an Fe-Pt alloy and C is to be sputtered, there is a problem in that C is inadvertently detached during sputtering to generate a large amount of particles (attached to the substrate). dust).

In order to solve this problem, it is necessary to provide a sputtering target in which the adhesion of the Fe-Pt alloy to C is improved. Further, although a magnetic thin film containing a carbide or a nitride instead of C is used, an excellent magnetic thin film can be obtained, but in this case, there is also a problem that a large amount of particles are generated at the time of sputtering.

Patent Document 6 shown below includes a sputtering target containing Fe, Pt, and C, and further contains a metal element other than Fe or Pt, and contains more than 0 at% and 20 at% as a metal element other than Fe or Pt. The following are Cu, Ag, Mn, Ni, Co, Pd, Cr, V, and B. However, in Patent Document 6, only one example of 10% by weight of Cu is contained, and the type and content of the additive element of the present invention described later are largely different.

Further, in the following Patent Document 7, a technique of mixing FePt alloy powder with Pt powder and carbon black powder and hot pressing is disclosed for the purpose of producing a sintered body of a C phase in a FePt alloy phase. However, there is no discussion on the solution to this problem in the case where C is detached during sputtering and a large amount of particles (dust attached to the substrate) are generated.

Further, Patent Document 8 listed below discloses a sputtering target for forming a magnetic recording medium film of FePt (Au and/or Cu) C type. A technique for replacing one of the above Au and/or Cu with Ag is disclosed, and a technique for suppressing particle generation is disclosed.

Further, Patent Document 9 listed below discloses a FePtAgC-based sputtering target for forming a magnetic recording medium film. There is disclosed a technique in which one part of the above Ag can be replaced with Au and/or Cu, and a technique for suppressing particle generation is disclosed.

Patent Document 8 and Patent Document 9 are similar techniques, but are described as follows: Since Ag, Au, and Cu added to suppress generation of particles have a low melting point, there is a problem that they are first melted at the time of hot pressing, and must be Reduce the sintering temperature.

Therefore, in order to prevent the above, it is described that Ag, Au, and Cu powders as raw materials are prepared into AgPt powder, AuPt powder, and CuPt powder, and are mixed with other raw material powders to be sintered. It has the problem of making the production steps cumbersome, and it is also necessary to increase the amount of addition of these elements.

Patent Document 1: Japanese Laid-Open Patent Publication No. 2000-306228

Patent Document 2: Japanese Laid-Open Patent Publication No. 2000-311329

Patent Document 3: Japanese Laid-Open Patent Publication No. 2008-59733

Patent Document 4: Japanese Laid-Open Patent Publication No. 2008-169464

Patent Document 5: Japanese Patent Laid-Open Publication No. 2004-152471

Patent Document 6: Japanese Laid-Open Patent Publication No. 2012-214874

Patent Document 7: Japanese Laid-Open Patent Publication No. 2012-102387

Patent Document 8: Japanese Laid-Open Patent Publication No. 2012-178210 (Patent No. 5041261)

Patent Document 9: Japanese Laid-Open Patent Publication No. 2012-178211 (Patent No. 5041262)

Although the Fe-Pt alloy forms an L1 ₀ regular lattice near the 1:1 composition, there is a problem that the material having a regular crystal lattice is generally not ductile, and the material is subjected to pressure sintering. It is also difficult to increase the density of the sintered body by sintering the apparatus. In particular, the Fe-Pt-C system containing C (carbon) which is a hard-to-sinter material is extremely difficult to obtain a dense sintered body. Therefore, if such a low-density sintered sputtering target is sputtered, there is a problem in that a large amount of particles (dust adhering to the substrate) are generated by inadvertently removing the non-magnetic material.

Further, when the L1 ₀ regular crystal lattice of the Fe-Pt alloy is heated to 1300 ° C or higher, the ductility is changed from a regular state to an irregular state, but the ductility is increased depending on the kind of the non-magnetic material contained therein. The temperature is decomposed above °C. Further, there is a problem that in the high temperature region of 1300 ° C or higher, the sintered body structure is coarsened due to the growth of crystal grains, and such coarse crystal grains become the starting point of abnormal discharge (arc) at the time of sputtering. And produce particles.

Accordingly, an object of the present invention is to provide a sintered body sputtering target which can be efficiently produced by reducing the amount of particles generated during sputtering, and which is composed of an Fe-Pt-based alloy and a non-magnetic material.

When the present inventors produced a sintered body sputtering target having a Fe-Pt alloy and a non-magnetic material containing at least C (carbon) as a main component, the present invention contains a trace amount of an additive element of 50 ppm by mass to 5000 ppm by mass. By adding the following trace elements as the trace addition elements (that is, adding an element which is likely to be a carbide), a carbide having a better wettability than the C element can be formed, whereby the Fe-Pt-based alloy can be improved by the carbide In addition, the standard production free energy ΔG° per 1 mol of the above-mentioned trace element-based carbide is not more than -5000 [cal/mol].

This is the basis of the invention of the present invention, and as a result, it is obtained that the particles generated during the sputtering of the sintered body sputtering target can be greatly reduced. Further, all of the sintering raw materials described below use the raw material powder.

According to the above findings, the present invention provides: 1) a sintered body sputtering target comprising a Fe-Pt alloy and a non-magnetic material as a main component, characterized in that at least C (carbon) is contained as a non-magnetic material, other than the above-mentioned main components. Further, a trace amount of the additive element is contained in a range of 50 ppm by mass to 5000 ppm by mass, and a standard production free energy ΔG° per 1 mol of carbon of the trace addition element carbide is -5000 [cal/mol] or less; 2) (1) The sintered body sputtering target according to any one of the above-mentioned 1 or 2), wherein the sintered body sputtering target is a non-magnetic material, in addition to the above-mentioned In addition to C (carbon), it may contain any one or more of an oxide, a nitride, and a carbide; The sintered body sputtering target according to any one of the above 1 to 3, further comprising, in addition to the main component and the trace addition element, Ag, Au, Co, Cu, Ga, Ge, Ir, One or more elements of Ni, Pd, Re, Rh, Ru, Sn, and Zn are used as the metal component.

Further, the present invention provides: 5) a method for producing a sintered body sputtering target comprising Fe-Pt alloy and a non-magnetic material as main components, wherein: the Fe powder and the Pt powder are prepared. In the case of C powder (graphite powder) and carbide, a standard amount of carbon having a standard free energy ΔG° of -5000 [cal/mol] or less is used as a raw material powder, and these powders are used in an Ar environment. After mixing and pulverizing, the mixed and pulverized powder is filled in a carbon mold, and the temperature increase rate is set to 200 to 600 ° C / hour, the temperature is maintained at 800 to 1400 ° C, and the holding time is 0 to 4 in a vacuum environment using a hot press device. In the method of producing a sintered body sputtering target according to the above 5), the method for producing a sintered body sputtering target according to the above 5), wherein the trace amount of the element is W or Cr The method for producing a sintered body sputtering target according to the above 5) or 6), wherein the raw material powder as the non-magnetic material contains an oxide, a nitride, and a carbide in addition to the C (carbon). Sintering according to any one of the above; 8) as in the above 5 to 7) A method for producing a sintered body sputtering target according to the invention, further comprising one or more selected from the group consisting of Ag, Au, Co, Cu, Ga, Ge, Ir, Ni, Pd, Re, Rh, Ru, Sn, and Zn. The element is sintered as a raw material of the metal component.

According to the present invention, it is possible to provide a sputtering target which greatly reduces the amount of particles generated during sputtering. Thereby, there is an excellent effect that the productivity at the time of film formation can be remarkably improved, and productivity can be improved.

A sintered body sputtering target having a Fe-Pt alloy and a non-magnetic material as a main component of the present invention, characterized in that it contains at least C (carbon) as a non-magnetic material, and further has a mass of 50 ppm by mass to 5,000 in addition to the above main component. The range of ppm contains a trace amount of an additive element, and the standard production free energy ΔG° per 1 mol of the carbon of the trace addition element is -5000 [cal/mol] or less.

The representative material of the above-mentioned trace addition element is W or Cr, and it is effective to add any one or more of them. However, as long as it is satisfied that the standard production free energy ΔG° per 1 mol of carbon of the carbide of the trace addition element is within the range of -5000 [cal/mol] in the temperature region satisfying the sintering, other elements are also used. There will be no special problems.

The composition of the Fe-Pt alloy can be generally used in a ratio of Pt of 35% or more and 55% or less in the atomic ratio, and the remainder is Fe. However, if it is a magnetic recording medium which can be effectively maintained There are no special restrictions within the scope. The Fe-Pt alloy in the sputtering target is usually composed of a L1 ₀ type regular lattice, but there is no limitation in this respect.

In the invention of the present invention, it is particularly important to use (add) a trace element as a sputtering target: the standard formation free energy ΔG° per 1 mol of carbon in the case of forming the carbide is -5000 [cal/mol] or less. Further, the content of C is not particularly limited as long as it is effective as a magnetic recording medium, but it is preferably set to be in the range of 20 to 45% by volume ratio in the sputtering target. .

That is to say, it is formed by adding an element which is easy to become a carbide A carbide having a better wettability than C, whereby the carbide can improve the adhesion of the Fe-Pt alloy to C.

As a result, the sintered body sputtering target can suppress the seizure of C during sputtering, and the amount of particles generated can be greatly reduced.

As described above, as a trace addition element, W and Cr are effective, and any one or more of them may be added. Hereinafter, the case of using W and Cr which are mainly representative of the trace addition elements will be described.

The content of W or Cr described above is set to 50 ppm by mass to 5000 ppm by mass. When the content is less than 50 ppm by mass, the formation of a carbide having good wettability is insufficient, and the adhesion between the Fe-Pt alloy and C cannot be expected to be improved. On the other hand, if the content exceeds 5,000 ppm by mass, the content may become impossible. A sufficient magnetic property as a magnetic film is obtained.

The same effect can be obtained by either or both of W or Cr. In the case where both are contained, the total content thereof is preferably 50 ppm by mass to 5000 ppm by mass based on the total content of the sputtering target.

Further, the sputtering target of the present invention may contain, as a nonmagnetic material, any one or more of an oxide, a nitride, and a carbide in addition to the above C (carbon). In this case, preferred oxides are selected from the group consisting of Al, B, Ba, Be, Ca, Ce, Cr, Dy, Er, Eu, Ga, Gd, Ho, Li, Mg, Mn, Nb, Nd, Pr. An oxide of one or more of Sc, Sm, Sr, Ta, Tb, Ti, V, Y, Zn, and Zr. Moreover, as a preferable nitride, a nitride of an element selected from one or more of Al, B, Ca, Nb, Si, Ta, Ti, and Zr may be mentioned. Further, as a preferred carbide, a carbide selected from one or more of B, Ca, Nb, Si, Ta, Ti, W, and Zr may be mentioned. The magnetic film produced by such a sputtering target, due to carbon, carbide, and nitriding Since the substance and the oxide have a structure in which the magnetic particles are magnetically insulated from each other, good magnetic properties can be expected.

Further, the sputtering target of the present invention may further contain, in addition to the main component and the trace addition element, Ag, Au, Co, Cu, Ga, Ge, Ir, Ni, Pd, Re, Rh, Ru, Sn. One or more elements of Zn are used as the metal component.

These metal elements are incorporated into the sputtered film and are primarily added to reduce the heat treatment temperature used to characterize the L1 ₀ structure. The blending ratio is not particularly limited as long as it is within a range in which the characteristics of the magnetic recording medium can be maintained effectively.

The sputtering target of the present invention is produced by a powder sintering method, for example, by the following method.

First, Fe powder, Pt powder, Cr powder, Cu powder, W powder, or the like is prepared as a metal powder. As the metal powder, not only a single element metal powder but also an alloy powder can be used. These metal powders should preferably be used in a particle size range of 1 to 10 μm. When the particle diameter is 1 to 10 μm, it can be more uniformly mixed, and segregation and coarse crystallization can be prevented.

When the particle diameter of the metal powder is larger than 10 μm, sometimes the non-magnetic material may not be uniformly dispersed, and when it is less than 1 μm, the following problem sometimes occurs: the target is caused by the oxidation of the metal powder. Composition is not the desired composition. In addition, the particle size range is only a preferred range, and it should be understood that the scope of the invention is not negated.

Further, in addition to the above C (carbon), an oxide powder, a nitride powder, a carbide powder or the like is prepared as a nonmagnetic material powder. These non-magnetic material powders are preferably used in a particle size range of 1 to 30 μm. When the particle diameter is 1 to 30 μm, the non-magnetic material powders are less likely to aggregate with each other when mixed with the metal powder described above, and can be uniformly dispersed.

As the C powder in the non-magnetic material, those having a crystal structure such as graphite or a nanotube and amorphous ones represented by carbon black may be used.

In the production of the sintered body sputtering target, Fe powder, Pt powder, C powder (graphite powder) as a raw material powder, and a standard generation free energy ΔG° per 1 mol of carbon in the case of forming a carbide are - The micro-added metal powder of 5000 [cal/mol] or less is weighed into a predetermined composition, and these powders are pulverized and mixed in a Ar environment using a known means such as a ball mill.

The mixed/pulverized powder is filled in a carbon mold, and the temperature increase rate is set to 200 to 600 ° C / hour, and the holding temperature is set to 800 to 1400 ° C in a vacuum environment or an inactive environment using a hot press device. The holding time is set to 0 to 4 hours, and pressurization is performed at 20 to 50 MPa from the start of the temperature rise to the end of the holding, thereby producing a sintered body.

In addition to the above-described hot pressing, various pressure sintering methods such as a plasma discharge sintering method can also be used. In particular, the hot hydrostatic sintering method is effective for increasing the density of the sintered body. The holding temperature at the time of sintering depends on the constituent components of the target, but most of the cases are in the temperature range of 800 ° C to 1400 ° C. Then, the sintered body obtained is processed into a desired shape by a lathe, whereby the sputtering target of the present invention can be produced.

The sputtering target of the present invention can be produced by the above method. The sputtering target produced in this manner has an excellent effect of reducing the amount of particles generated at the time of sputtering and improving the yield at the time of film formation.

Example

Hereinafter, it demonstrates based on an Example and a comparative example. In addition, this embodiment is merely an example and is not limited by this illustration. That is, the present invention is limited only by the scope of the patent application, and includes various modifications other than the embodiments included in the invention.

(Example 1)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, W powder having an average particle diameter of 3 μm, and C powder (graphite powder) having an average particle diameter of 10 μm were prepared as raw material powders.

The basic component was set to a weighing composition (molar ratio): 30Fe-30Pt-40C, and the total weight of the above-mentioned weighing amount was 2600 g.

Further weigh 5.2 g of W as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill pot having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1400 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and W were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result, the W content in the sputtering target was 1990 mass ppm. Further, regarding the basic component, the result of calculating the molar ratio based on the weight ratio obtained by the analysis, the composition of the sputtering target was an analysis composition (molar ratio): 30.09Fe-30.04Pt-39.87C.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. This target was mounted on a magnetron sputtering apparatus (CON-10 AN-C-3010 sputtering system) for sputtering. The sputtering conditions were as follows: input electric power 1 kW, Ar gas pressure 1.7 Pa, and 2 kWhr pre-sputtering, after 4 吋 diameter ruthenium base The film was formed on the plate for 20 seconds. The number of particles attached to the substrate is then measured with a particle counter. The number of particles at this time was 185.

(Comparative Example 1)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, W powder having an average particle diameter of 3 μm, and C powder (graphite powder) having an average particle diameter of 10 μm were prepared as raw material powders.

The basic component was set to a weighing composition (molar ratio): 30Fe-30Pt-40C, and the total weight of the above-mentioned weighing amount was 2600 g.

Further, 0.13 g of W was weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1400 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and W were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result, the W content in the sputtering target was 40 ppm by mass. Further, as a result of calculating the molar ratio based on the weight ratio obtained by the analysis on the basic component, the composition of the sputtering target was an analysis composition (molar ratio): 30.20Fe-30.08 Pt-39.72C.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, the same conditions as in Example 1 were carried out. The sputtering is performed, and the number of particles attached to the substrate is measured by a particle counter. The number of particles at this time was 498, which was larger than that of Example 1.

(Comparative Example 2)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, W powder having an average particle diameter of 3 μm, and C powder (graphite powder) having an average particle diameter of 10 μm were prepared as raw material powders.

The basic component was set to a weighing composition (molar ratio): 30Fe-30Pt-40C, and the total weight of the above-mentioned weighing amount was 2600 g.

Further, 52.0 g of W was weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1400 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and W were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result, the W content in the sputtering target was 20100 ppm by mass. Further, as a result of calculating the molar ratio based on the weight ratio by analysis, the composition of the sputtering target was an analysis composition (molar ratio): 30.07Fe-30.01 Pt-39.92C.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, the same conditions as in Example 1 were carried out. The sputtering is performed, and the number of particles attached to the substrate is measured by a particle counter. The number of particles at this time was 354, which was larger than that of Example 1.

On the other hand, when compared with Example 1, sufficient magnetic characteristics could not be obtained. It is considered that since the content of W is too large, the saturation magnetization or the crystal magnetic anisotropy energy is lowered.

(Example 2)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, C powder (graphite powder) having an average particle diameter of 10 μm, and Cr powder having an average particle diameter of 3 μm were prepared as raw material powders.

The basic component was set to a weighing composition (molar ratio): 30Fe-30Pt-40C, and the total weight of the above-mentioned weighing amount was 2600 g.

Further, 2.6 g of Cr was weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1300 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and Cr were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result, the Cr content in the sputtering target was 990 ppm by mass. Further, as a result of calculating the molar ratio based on the weight ratio obtained by the analysis on the basic component, the composition of the sputtering target was an analysis composition (molar ratio): 29.85Fe-30.10 Pt-40.05C.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time is 255.

(Comparative Example 3)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, C powder (graphite powder) having an average particle diameter of 10 μm, and Cr powder having an average particle diameter of 3 μm were prepared as raw material powders.

The basic component was set to a weighing composition (molar ratio): 30Fe-30Pt-40C, and the total weight of the above-mentioned weighing amount was 2600 g.

Further, 0.13 g of Cr was weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1300 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and Cr were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result, the Cr content in the sputtering target was 30 ppm by mass. Further, as a result of calculating the molar ratio based on the weight ratio obtained by the analysis on the basic component, the composition of the sputtering target was an analytical composition (molar ratio): 30.23Fe-29.85 Pt-39.92C.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, it was mounted on a magnetron sputtering apparatus, and sputtering was performed under the same conditions as in Example 1, and the number of particles attached to the substrate was measured by a particle counter. The number of particles at this time was 658, which was larger than that of Example 2.

(Comparative Example 4)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, C powder (graphite powder) having an average particle diameter of 10 μm, and Cr powder having an average particle diameter of 3 μm were prepared as raw material powders.

The basic component was set to a weighing composition (molar ratio): 30Fe-30Pt-40C, and the total weight of the above-mentioned weighing amount was 2600 g.

Further, 26 g of Cr was weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1300 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and Cr were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result, the Cr content in the sputtering target was 10,200 ppm by mass. Further, regarding the basic component, the result of calculating the molar ratio based on the weight ratio obtained by the analysis, the composition of the sputtering target was an analysis composition (molar ratio): 30.05Fe-30.10 Pt-39.85C.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 325, which was almost the same as in Example 2. On the other hand, when compared with Example 2, sufficient magnetic characteristics could not be obtained. It is considered that since the content of Cr is large, the saturation magnetization or the crystal magnetic anisotropy energy is lowered.

(Example 3)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, W powder having an average particle diameter of 3 μm, Cr powder having an average particle diameter of 3 μm, C powder (graphite powder) having an average particle diameter of 10 μm, and an average particle diameter of 10 μm were prepared. BN powder is used as a raw material powder.

The basic component was set to a weighing composition (molar ratio): 35Fe-35Pt-20C-10BN, and the total weight was 2600 g in terms of the above-mentioned weighing composition.

Further, 5.2 g of W and 5.2 g of Cr were weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1200 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, B, W, and Cr were measured using an ICP-AES apparatus. The content of BN is calculated based on the measured value of B using a stoichiometric ratio. In addition, the C system uses a high-frequency induction heating furnace to burn The carbon analyzer of the burn-infrared absorption method was measured. As a result, the W content in the sputtering target was 2000 ppm by mass, and the Cr content in the sputtering target was 2050 ppm by mass. Further, as a result of calculating the molar ratio based on the weight ratio obtained by analysis regarding the basic component, the composition of the sputtering target was an analytical composition (molar ratio): 34.91Fe-35.35Pt-20.04C-9.70BN.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, it was mounted on a magnetron sputtering device for sputtering, and the particle counter was used to measure the number of particles attached to the substrate. The number of particles at this time was 211.

(Comparative Example 5)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, W powder having an average particle diameter of 3 μm, Cr powder having an average particle diameter of 3 μm, C powder (graphite powder) having an average particle diameter of 10 μm, and an average particle diameter of 10 μm were prepared. BN powder is used as a raw material powder.

The basic component was set to a weighing composition (molar ratio): 35Fe-35Pt-20C-10BN, and the total weight was 2600 g in terms of the above-mentioned weighing composition.

Further, 0.06 g of W and 0.06 g of Cr were weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1200 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, using a sintered body produced from the obtained body, a part is obtained, and the component is implemented. Analysis. Fe, Pt, B, W, and Cr were measured using an ICP-AES apparatus. The content of BN is calculated based on the measured value of B using a stoichiometric ratio. Further, the C system is measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result, the W content in the sputtering target was 20 ppm by mass, and the Cr content in the sputtering target was 20 ppm by mass. Further, as a result of calculating the molar ratio based on the weight ratio by analysis, the composition of the sputtering target is the analysis composition (molar ratio): 35.09Fe-35.11Pt-19.87C-9.93BN.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, it was mounted on a magnetron sputtering apparatus, and sputtering was performed under the same conditions as in Example 1, and the number of particles attached to the substrate was measured by a particle counter. The number of particles at this time was 375, which was increased compared with Example 3.

(Comparative Example 6)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, W powder having an average particle diameter of 3 μm, Cr powder having an average particle diameter of 3 μm, C powder (graphite powder) having an average particle diameter of 10 μm, and an average particle diameter of 10 μm were prepared. BN powder is used as a raw material powder.

The basic component was set to a weighing composition (molar ratio): 35Fe-35Pt-20C-10BN, and the total weight was 2600 g in terms of the above-mentioned weighing composition.

Further, 5.2 g of W and 13.0 g of Cr were weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1200 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. Directly after the end Cool naturally in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, B, W, and Cr were measured using an ICP-AES apparatus. The content of BN is calculated based on the measured value of B using a stoichiometric ratio. Further, the C system is measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result, the W content in the sputtering target was 1980 ppm by mass, and the Cr content in the sputtering target was 5030 ppm by mass. Further, as a result of calculating the molar ratio based on the weight ratio by analysis, the composition of the sputtering target was an analytical composition (molar ratio): 34.94Fe-35.26Pt-19.97C-9.83BN.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, it was mounted on a magnetron sputtering device for sputtering, and the particle counter was used to measure the number of particles attached to the substrate. The number of particles at this time was 208, which was almost the same as in Example 3. On the other hand, when compared with Example 3, sufficient magnetic characteristics could not be obtained. It is considered that since the content of W and Cr is large, the saturation magnetization or the crystal magnetic anisotropy energy is lowered.

(Example 4)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, B powder having an average particle diameter of 10 μm, C powder (graphite powder) having an average particle diameter of 10 μm, and SiO ₂ powder having an average particle diameter of 5 μm were prepared as raw material powders.

The basic component was set to a weighing composition (molar ratio): 35Fe-35Pt-25C-5SiO ₂ , and the total weight was 2500 g in terms of the above-mentioned weighing composition.

Further, 0.25 g of B was weighed as a trace addition component.

Then, we put all the powder weighed together with the SUS grinding ball of the pulverizing medium. A 10 liter ball mill was mixed and pulverized in an Ar environment for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1150 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Si, and B were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. The content of SiO ₂ was calculated from the measured value of Si using a stoichiometric ratio. As a result, the B content in the sputtering target was 110 ppm by mass. Further, regarding the basic component, the result of calculating the molar ratio based on the weight ratio obtained by the analysis, the composition of the sputtering target is the analytical composition (molar ratio): 34.95Fe-35.02Pt-24.90C-5.13SiO ₂ .

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 108.

(Comparative Example 7)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, B powder having an average particle diameter of 10 μm, C powder (graphite powder) having an average particle diameter of 10 μm, and SiO ₂ powder having an average particle diameter of 5 μm were prepared as raw material powders.

The basic component was set to a weighing composition (molar ratio): 35Fe-35Pt-25C-5SiO ₂ , and the total weight was 2500 g in terms of the above-mentioned weighing composition.

Further weigh 0.07g of B as a trace additive

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1150 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Si, and B were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. The content of SiO ₂ was calculated from the measured value of Si using a stoichiometric ratio. As a result, the B content in the sputtering target was 20 ppm by mass. Further, regarding the basic component, the result of calculating the molar ratio based on the weight ratio obtained by the analysis, the composition of the sputtering target is the analysis composition (molar ratio): 34.77Fe-35.02Pt-25.07C-5.14SiO ₂ .

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, it was mounted on a magnetron sputtering apparatus, and sputtering was performed under the same conditions as in Example 1, and the number of particles attached to the substrate was measured by a particle counter. The number of particles at this time was 245, which was larger than that of Example 4.

(Comparative Example 8)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, B powder having an average particle diameter of 10 μm, C powder (graphite powder) having an average particle diameter of 10 μm, and SiO ₂ powder having an average particle diameter of 5 μm were prepared as raw material powders.

The basic component was set to a weighing composition (molar ratio): 35Fe-35Pt-25C-5SiO ₂ , and the total weight was 2500 g in terms of the above-mentioned weighing composition.

Further, 17.5 g of B was weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1150 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Si, and B were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. The content of SiO ₂ was calculated from the measured value of Si using a stoichiometric ratio. As a result, the B content in the sputtering target was 6950 ppm by mass. Further, regarding the basic component, the result of calculating the molar ratio based on the weight ratio obtained by the analysis, the composition of the sputtering target is the analytical composition (molar ratio): 35.03Fe-34.87Pt-25.05C-5.05SiO ₂ .

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 117, which was the same as in Example 4. On the other hand, when compared with Example 4, sufficient magnetic characteristics could not be obtained. It is considered that since the content of B is large, the saturation magnetization or the crystal magnetic anisotropy energy is lowered.

(Example 5)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Cu powder having an average particle diameter of 3 μm, W powder having an average particle diameter of 3 μm, C powder (graphite powder) having an average particle diameter of 10 μm, and an average particle diameter of 1 μm were prepared. TaC powder is used as a raw material powder. The basic composition was set to a weighing composition (molar ratio): 30Fe-30Pt-5Cu-20C-15TaC, and the total weight was 3000 g in terms of the above-mentioned weighing composition.

Further, 12.0 g of W was weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a nitrogen atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1100 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Cu, Ta, and W were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. The content of TaC is calculated from the measured value of Ta using a stoichiometric ratio. As a result, the W content in the sputtering target was 4000 ppm by mass. Further, regarding the basic component, the result of calculating the molar ratio based on the weight ratio obtained by the analysis, the composition of the sputtering target is the analytical composition (molar ratio): 29.92Fe-30.09Pt-5.04Cu-19.92C- 15.03TaC.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, the same conditions as in Example 1 were carried out. The sputtering is performed, and the number of particles attached to the substrate is measured by a particle counter. The number of particles at this time was 278.

(Comparative Example 9)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Cu powder having an average particle diameter of 3 μm, W powder having an average particle diameter of 3 μm, C powder (graphite powder) having an average particle diameter of 10 μm, and an average particle diameter of 1 μm were prepared. TaC powder is used as a raw material powder. The basic composition was set to a weighing composition (molar ratio): 30Fe-30Pt-5Cu-20C-15TaC, and the total weight was 3000 g in terms of the above-mentioned weighing composition.

Further, 0.1 g of W was weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a nitrogen atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1100 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Cu, Ta, and W were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. The content of TaC is calculated from the measured value of Ta using a stoichiometric ratio. As a result, the W content in the sputtering target was 30 ppm by mass. Further, regarding the basic component, the result of calculating the molar ratio based on the weight ratio obtained by the analysis, the composition of the sputtering target is the analytical composition (mole ratio): 29.92Fe-30.38Pt-5.18Cu-19.72C- 14.80TaC.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 590, which was larger than that of Example 5.

(Comparative Example 10)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Cu powder having an average particle diameter of 3 μm, W powder having an average particle diameter of 3 μm, C powder (graphite powder) having an average particle diameter of 10 μm, and an average particle diameter of 1 μm were prepared. TaC powder is used as a raw material powder. The basic composition was set to a weighing composition (molar ratio): 30Fe-30Pt-5Cu-20C-15TaC, and the total weight was 3000 g in terms of the above-mentioned weighing composition.

Further, 24.0 g of W was weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a nitrogen atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1100 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Cu, Ta, and W were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. The content of TaC is calculated from the measured value of Ta using a stoichiometric ratio. As a result, the W content in the sputtering target was 7980 ppm by mass. Also, regarding the basic component, it is calculated based on the weight ratio obtained by analysis. As a result of the molar ratio, the composition of this sputtering target was the analytical composition (mole ratio): 30.03Fe-30.00Pt-5.06Cu-19.98C-14.93 TaC.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 290, which was almost the same as in Example 5. On the other hand, when compared with Example 5, sufficient magnetic characteristics could not be obtained. It is considered that since the content of W is large, the saturation magnetization or the crystal magnetic anisotropy energy is lowered.

(Example 6)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, W powder having an average particle diameter of 3 μm, and C powder (graphite powder) having an average particle diameter of 10 μm were prepared as raw material powders.

The basic composition was set to a weighing composition (molar ratio): 45.5Fe-24.5Pt-30C, and the total weight was 2470 g in terms of the above-mentioned weighing composition.

Further, 5.0 g of W was weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1300 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and W are measured using an ICP-AES device, and C is using a high frequency induction. The carbon analyzer of the hot-burning-infrared absorption method was measured. As a result, the W content in the sputtering target was 2010 mass ppm. Further, as a result of calculating the molar ratio based on the weight ratio obtained by the analysis on the basic component, the composition of the sputtering target was an analysis composition (molar ratio): 45.53Fe-24.50Pt-29.97C.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. This target was mounted on a magnetron sputtering device (C-3010 sputtering system manufactured by Canon Annehua) for sputtering. The sputtering conditions were 1 kW of input electric power and 1.7 Pa of Ar gas pressure, and after pre-sputtering of 2 kWhr, film formation was performed on a 4 吋 diameter ruthenium substrate for 20 seconds. The number of particles attached to the substrate is then measured with a particle counter. The number of particles at this time was 124.

(Comparative Example 11)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, W powder having an average particle diameter of 3 μm, and C powder (graphite powder) having an average particle diameter of 10 μm were prepared as raw material powders.

The basic composition was set to a weighing composition (molar ratio): 45.5Fe-24.5Pt-30C, and the total weight was 2470 g in terms of the above-mentioned weighing composition.

Further, 0.25 g of W was weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1300 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, using a sintered body produced from the obtained body, a part is obtained, and the component is implemented. Analysis. Fe, Pt, and W were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result, the W content in the sputtering target was 80 ppm by mass. Further, as a result of calculating the molar ratio based on the weight ratio obtained by analysis regarding the basic component, the composition of the sputtering target was an analytical composition (molar ratio): 45.40Fe-24.52 Pt-30.08C.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 354, which was larger than that of Example 6.

(Comparative Example 12)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, W powder having an average particle diameter of 3 μm, and C powder (graphite powder) having an average particle diameter of 10 μm were prepared as raw material powders.

The basic composition was set to a weighing composition (molar ratio): 45.5Fe-24.5Pt-30C, and the total weight was 2470 g in terms of the above-mentioned weighing composition.

Further, 50.0 g of W was weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1300 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

Then, using a sintered body produced from the obtained body, a part is obtained, and the component is implemented. Analysis. Fe, Pt, and W were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result, the W content in the sputtering target was 20100 ppm by mass. Further, as a result of calculating the molar ratio based on the weight ratio obtained by the analysis on the basic component, the composition of the sputtering target was an analytical composition (molar ratio): 45.47Fe-24.58 Pt-29.95C.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 163, which was larger than that of Example 6.

On the other hand, sufficient magnetic properties could not be obtained as compared with Example 6. It is considered that this is because the W content is too large, so the saturation magnetization or the crystal magnetic anisotropy energy is lowered.

(Example 7)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, C powder (graphite powder) having an average particle diameter of 10 μm, and Cr powder having an average particle diameter of 3 μm were prepared as raw material powders.

The basic component was set to a weighing composition (molar ratio): 20.25Fe-24.75 Pt-55C, and the total weight of the above-mentioned weighing amount was 2200 g.

Further, 2.2 g of Cr was weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1400 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. Directly after the end Cool naturally in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and Cr were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result, the Cr content in the sputtering target was 990 ppm by mass. Further, as a result of calculating the molar ratio based on the weight ratio obtained by the analysis on the basic component, the composition of the sputtering target was an analytical composition (molar ratio): 20.35Fe-24.78Pt-54.87C.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 356.

(Comparative Example 13)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, C powder (graphite powder) having an average particle diameter of 10 μm, and Cr powder having an average particle diameter of 3 μm were prepared as raw material powders.

The basic component was set to a weighing composition (molar ratio): 20.25Fe-24.75 Pt-55C, and the total weight of the above-mentioned weighing amount was 2200 g.

Further, 0.1 g of Cr was weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1400 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. Directly after the end Cool naturally in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and Cr were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result, the Cr content in the sputtering target was 30 ppm by mass. Further, as a result of calculating the molar ratio based on the weight ratio obtained by the analysis on the basic component, the composition of the sputtering target was an analytical composition (molar ratio): 20.23Fe-24.80Pt-54.97C.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, it was mounted on a magnetron sputtering apparatus, and sputtering was performed under the same conditions as in Example 1, and the number of particles attached to the substrate was measured by a particle counter. The number of particles at this time was 486, which was larger than that of Example 7.

(Comparative Example 14)

Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, C powder (graphite powder) having an average particle diameter of 10 μm, and Cr powder having an average particle diameter of 3 μm were prepared as raw material powders.

The basic component was set to a weighing composition (molar ratio): 20.25Fe-24.75 Pt-55C, and the total weight of the above-mentioned weighing amount was 2200 g.

Further, 20 g of Cr was weighed as a trace addition component.

Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1400 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. Directly after the end Cool naturally in the chamber.

Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and Cr were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result, the Cr content in the sputtering target was 10,600 ppm by mass. Further, as a result of calculating the molar ratio based on the weight ratio obtained by the analysis on the basic component, the composition of the sputtering target was an analytical composition (molar ratio): 20.24Fe-24.78Pt-54.98C.

Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 345. Almost the same as Example 7. On the other hand, when compared with Example 7, sufficient magnetic characteristics could not be obtained. It is considered that since the content of Cr is large, the saturation magnetization or the crystal magnetic anisotropy energy is lowered.

As described above, in any of the embodiments, by adding a predetermined amount of W or Cr, the amount of particles generated at the time of sputtering can be reduced, and the yield at the time of film formation can be improved. Therefore, it is understood that the inclusion of W or Cr has a very important effect on suppressing the generation of particles.

The results of the above examples and comparative examples are shown in Table 1.

[Table 1]

In the above-described examples and comparative examples, examples of BN, SiO ₂ , and TaC are listed as examples of the addition of an oxide, a nitride, or a carbide to the non-magnetic material in addition to the above-mentioned C (carbon). However, it is confirmed that other oxides, nitrides, and carbides also exhibit the same effect.

Further, an element containing one or more elements selected from the group consisting of Ag, Au, Co, Cu, Ga, Ge, Ir, Ni, Pd, Re, Rh, Ru, Sn, and Zn is used as a metal component, and Cu is added. In the same manner, it is confirmed that an element selected from one or more selected from the group consisting of Ag, Au, Co, Cu, Ga, Ge, Ir, Ni, Pd, Re, Rh, Ru, Sn, and Zn can be used. Get the same effect.

Industrial utilization

The sputtering target of the present invention has an excellent effect of reducing the amount of particles generated during sputtering and improving the yield at the time of film formation. Therefore, it is suitable as a sputtering target for forming a granular structure type magnetic thin film.

Claims (8)

A sintered body sputtering target comprising a Fe-Pt alloy and a non-magnetic material as a main component, characterized in that at least C (carbon) is contained as a non-magnetic material, and further 50 mass ppm to 5000 mass ppm is further contained outside the main component The range contains a trace amount of the additive element, and the standard production free energy ΔG° per 1 mol of the carbon of the trace addition element is -5000 [cal/mol] or less. The sintered body sputtering target according to the first aspect of the invention, wherein the trace addition element is one or more of W and Cr. The sintered body sputtering target according to claim 1 or 2, wherein the non-magnetic material contains at least one of an oxide, a nitride, and a carbide in addition to the C (carbon). The sintered body sputtering target according to any one of claims 1 to 3, which further comprises, in addition to the main component and the trace addition element, an element selected from the group consisting of Ag, Au, Co, Cu, Ga, Ge, Ir, One or more elements of Ni, Pd, Re, Rh, Ru, Sn, and Zn are used as the metal component. A method for producing a sintered body sputtering target, which comprises Fe-Pt alloy and a non-magnetic material as main components, and is characterized in that Fe powder, Pt powder, C powder (graphite powder) and carbonization are prepared. In the case of a substance, a standard amount of elemental powder having a free energy ΔG° of -5000 [cal/mol] or less is used as a raw material powder, and these powders are mixed and pulverized in an Ar environment, and mixed and pulverized. The powder after the filling is filled in a carbon mold, and the heating rate is set to 200 to 600 ° C / hour in a vacuum environment, the temperature is maintained at 800 to 1400 ° C, and the holding time is 0 to 4 hours. The sintered body was produced by pressurizing at 20 to 50 MPa. The method for producing a sintered body sputtering target according to the fifth aspect of the invention, wherein the trace addition element is one or more of W and Cr. A method of manufacturing a sintered body sputtering target according to claim 5 or 6, wherein The raw material powder of the non-magnetic material contains, in addition to the C (carbon), any one or more of an oxide, a nitride, and a carbide, and is sintered. The method for producing a sintered body sputtering target according to any one of claims 5 to 7, which further comprises a material selected from the group consisting of Ag, Au, Co, Cu, Ga, Ge, Ir, Ni, Pd, Re, Rh, One or more elements of Ru, Sn, and Zn are used as a raw material of the metal component to be sintered.