KR101475133B1 - Sb-Te ALLOY POWDER FOR SINTERING, PROCESS FOR PRODUCTION OF THE POWDER, AND SINTERED TARGET - Google Patents

Abstract

A sintered body target comprising an Sb-Te-based alloy powder for sintering and an Sb-Te-based alloy, wherein the sintered body is composed of a powder having an average particle diameter of 0.1 to 200 탆 and an oxygen content of not more than 1000 wtppm. Wherein the Sb-Te based alloy is characterized in that the resistance of the sintered body is 50 MPa or more and the relative density is 99% or more. Sb-Te-based alloy sputtering target structure is made uniform and finer, cracks are prevented from being generated in the sintered target, and arcing is prevented from occurring at the time of sputtering. Further, the unevenness of the surface due to the sputter erosion is reduced, and a Sb-Te alloy sputtering target of good quality is obtained.

Description

{Sb-Te ALLOY POWDER FOR SINTERING, PROCESS FOR PRODUCTION OF THE POWER, AND SINTERED TARGET}

The present invention relates to an Sb-Te alloy sputtering target for forming a phase change recording layer made of an Sb-Te alloy powder for sintering, for example, an Ag-In-Sb-Te alloy or a Ge-Sb- Te-based alloy powder for sintering and a method for producing an Sb-Te-based alloy powder for sintering for producing a target.

In recent years, a thin film made of an Sb-Te-based material has been used as a phase change recording material, that is, a medium for recording information by using a phase change. As a method for forming the thin film made of the Sb-Te alloy material, it is usually carried out by means known as a physical vapor deposition method such as a vacuum evaporation method or a sputtering method. In particular, in many cases, magnetron sputtering is used in terms of operability and film stability.

The formation of the film by the sputtering method is carried out by physically colliding the target provided on the cathode with a static ion such as Ar ions and discharging the material constituting the target with the collision energy so that the target material And then laminating films having the same composition.

The coating method by the sputtering method is characterized in that it is possible to form a film from a thin film of angstrom to a thick film of several tens of microns at a stable film forming speed by controlling the processing time and the supply power.

Particularly troublesome in the case of forming a film made of an Sb-Te alloy material for a phase-change recording film are problems in that particles are generated at the time of sputtering, or when abnormal discharge (micro arcing) or formation of a thin film of clusters Cracks or cracks occur in the target during the generation of nodules (protrusions) that cause the sputtering, and in the sputtering, and furthermore, a large amount of oxygen is absorbed in the production process of the target sintered powder.

Such a problem in the case of the target or the sputtering is a major cause of deteriorating the quality of the thin film as the recording medium.

It can be seen that the above problem is greatly affected by the particle diameter of the powder for sintering or the structure and properties of the target. However, conventionally, when a Sb-Te based alloy sputtering target for forming a phase change recording layer is manufactured, a suitable powder can not be produced, and a target obtained by sintering does not have sufficient characteristics, Generation of particles, abnormal discharge, generation of nodules, occurrence of cracks or cracks in the target, and even a large amount of oxygen contained in the target when sputtering could not be avoided.

As a method for producing a conventional Sb-Te alloy sputtering target, a method of producing a Ge-Sb-Te sputtering target is exemplified by the inert gas atomization method to quench the Ge-Te alloy and the Sb-Te alloy (See, for example, Patent Document 1) a method of producing a Ge-Sb-Te-based sputtering target by preparing a powder of a Ge-Sb-Te alloy powder, uniformly mixing the alloy powder, and then performing pressure sintering.

Further, a powder having a tap density (relative density) of 50% or more among the alloy powders containing Ge, Sb and Te is poured into the die and pressed at a cold or warm temperature to form a molding material having a density of 95% Or the sintered body is heat-treated in a vacuum atmosphere to have an oxygen content of 700 ppm or less, and a method of producing a Ge-Sb-Te-based sputtering target and a powder for use in these methods by atomization (See, for example, Patent Document 2).

The raw material containing Ge, Sb and Te is quenched by an inert gas atomization method to obtain a powder having a particle size distribution of 20 mu m or more and a specific surface area per unit weight of 300 mm < 2 > / g or less (Refer to, for example, Patent Document 3) a method of producing a Ge-Sb-Te-based sputtering target material by sintering a compact that has been subjected to pressure molding in cold or warm conditions using a powder having a high thermal conductivity.

Other techniques for producing a target using an atomized powder include the following Patent Documents 4, 5, and 6.

However, with respect to the above patent documents, it is difficult to say that sufficient strength of the target can not be obtained by using the atomized powder as it is, and that the fineness and homogenization of the target structure are achieved. In addition, there is a problem that the allowable oxygen content is large and it can not be said to be sufficient for an Sb-Te-based sputtering target for forming a phase change recording layer.

In this respect, the Applicant first proposed an Sb-Te-based sputtering target and a powder used therefor (see Patent Documents 7, 8 and 9). These are for solving the above problem.

Patent Document 1: JP-A-2000-265262

Patent Document 2: JP-A-2001-98366

Patent Document 3: JP-A-2001-123266

Patent Document 4: JP-A-10-81962

Patent Document 5: JP-A-2001-123267

Patent Document 6: Japanese Patent Application Laid-Open No. 2000-129316

Patent Document 7: JP-A-2004-162109

Patent Document 8: WO2006 / 077692

Patent Document 9: WO2006 / 067937

An object of the present invention is to optimize the crystallization rate, improve the resistance to repeated transformation of amorphous and crystalline phases, and further optimize the film resistivity. In addition, Sb-Te for target sintering, which can effectively suppress the generation of particles, an abnormal discharge, generation of nodules, occurrence of cracks or cracks of the target, and impurities such as oxygen contained in the target during sputtering, Te-based alloy powder for sintering, which is preferable for producing an Sb-Te-based alloy sputtering target for forming a phase-change recording layer made of a base alloy powder, particularly a Ag-In-Sb-Te alloy or a Ge- And a method for producing an Sb-Te alloy powder for sintering, and a sintered body target obtained thereby.

The technical means for solving the above problem is that a stable and homogeneous phase change recording layer can be obtained by studying the properties of the powder and the structure and properties of the target.

On the basis of this finding,

1) An Sb-Te alloy powder for sintering, characterized in that it is made of a powder having an average particle diameter of 0.1 to 200 탆 and an oxygen content of 1000 wtppm or less.

As the additive element, Ag, Al, As, Au, B, C, Ga, Ge, In, P, Pd, Pt, S, Se, Si and Ti can be used as the Sb- , And 1 to 30 at% of at least one element selected from these can be contained. In general, these addition elements can optimize the crystallization rate and optimize the melting point and the crystallization temperature. In addition, it is possible to improve the resistance to cyclic repetition of amorphous and crystalline, and to further optimize the film resistivity.

The addition amount of the additional elements needs to be adjusted depending on the characteristics of the elements. Normally, the addition amount is less than 1 at%, and when the upper limit value is more than 30 at%, the original phase change recording As, Ag, Al, As, Au, B, C, Ga, Ge, In, P, or the like may be used in some cases, The addition amount of at least one element selected from Pd, Pt, S, Se, Si and Ti is preferably 1 to 30 at%.

The average particle size of the powder is in the range of 0.1 to 200 mu m. The particle size is preferably small, and preferably has an average particle diameter of 1 to 50 μm, and more preferably 1 to 20 μm. Since it is difficult to produce a uniform powder having a uniform particle diameter, a certain degree of deviation is unavoidable. However, in the case where powders exceeding 200 탆 are mixed, the uniformity of the sintered body is impaired, Of 3?) Within the range of 0.1 to 200 占 퐉.

The oxygen content is set to 1000 wtppm or less. When the oxygen content is high, an oxide insulating layer with a low sintering property is formed, the mechanical strength of the target is lowered, cracks and cracks are generated, and an abnormal discharge (arcing) occurs due to the insulating layer portion. In order to prevent such a drawback, it is necessary to set the upper limit to 1000 wtppm. The oxygen content is preferably not more than 500 wtppm, more preferably not more than 100 wtppm.

When a powder having a specific surface area (BET) of 0.15 to 0.25 m < 2 > / g is used, it is a more preferable Sb-Te alloy powder because a dense sintered body target can be produced at the time of sintering.

The present invention,

2) a raw material comprising an Sb-Te based alloy is dissolved and then processed to form a powder, and the powder thus obtained is reduced to have an oxygen content of not more than 1000 wtppm and an average grain size of 0.1 to 200 탆 The present invention also provides a method for producing an Sb-Te alloy powder for use in the present invention.

In this case, too, it is preferable that the average particle diameter be 1 to 50 mu m, and further the Sb-Te alloy powder for sintering having an average particle diameter of 1 to 20 mu m. This can be achieved by adjusting and classifying the processing method of the powder.

In the production process of the powder, the reduction treatment may be a vacuum drying treatment after the pickling (for example, after immersion in a 50% nitric acid aqueous solution for 10 minutes and a vacuum degree of 100 mTorr (13 Pa) (For example, 500 占 폚 for 2 hours), a reducing material (Mg, Fe) in an inert gas (Ar) atmosphere, By carrying out the treatment, the powder can be reduced.

The selection of these treatments is optional, and the reduction of the target powder can be achieved according to the degree of reduction, the amount of the powder, and the degree of oxidation, and there is no particular limitation. Thus, the present invention may achieve an oxygen content of less than 500 wtppm, less than 100 wtppm, and even less than 300 wtppm. The present invention can accomplish these.

Further, it is possible to provide a method for producing an Sb-Te alloy powder for sintering in which the specific surface area (BET) is adjusted to a powder of 0.15 to 0.25 m 2 / g. In the same way, the specific surface area can be adjusted by adjusting the processing method of the powder such as the degree of grinding.

3) A sintered body target made of an Sb-Te-based alloy having an oxygen content of 1000 wtppm or less, an uncut force of 50 MPa or more, and a relative density of 99% or more by sintering the powder obtained by the above- You can get the target.

Further, the present invention can provide a sintered body target made of an Sb-Te alloy, characterized in that the oxygen content is 500 wtppm or less, the uncut force is 60 MPa or more, and the relative density is 99.5% or more. The oxygen content can be set to 500 wtppm or less.

It is preferable that the sintered Sb-Te alloy sputtering target has a surface roughness Ra of the target erosion surface of 0.5 m or less. The present invention can accomplish this, and hence the generation of particles is less, and more uniform film formation becomes possible.

1 to 30 at% of one or more elements selected from Ag, Al, As, Au, B, C, Ga, Ge, In, P, Pd, Pt, S, Se, .

As described above, these added elements make it easy to optimize the crystallization rate and optimize the melting point and the crystallization temperature. In addition, it is possible to improve the resistance to cyclic repetition of amorphous and crystalline, and to easily optimize the film resistivity.

As described above, it is possible to make the Sb-Te alloy sputtering target structure uniform and finer, to prevent occurrence of cracks in the sintered target, and to suppress arcing at the time of sputtering. In addition, there is an effect that the unevenness of the surface due to the sputter erosion is reduced, and the generation of particles due to the peeling of the redistribution film to the upper surface of the target is reduced. As described above, by making the target structure finer and homogenized, fluctuations in composition between the in-plane and the lot of the thin film to be produced are suppressed, and the quality of the recording layer on the phase-change image is stabilized.

In addition, there is an effect that a material having a low oxygen concentration and a low carbon concentration can be obtained by reducing the powder during the manufacturing process of the powder. Further, the Sb-Te-based sputtering target sintered body of the present invention has an excellent resistance of 60 MPa or more and high strength, and cracks and cracks do not occur at the time of sputtering, and the material has excellent properties. By using the Sb-Te alloy powder of the present invention, the crystallization rate can be optimized, and the melting point and the crystallization temperature can be optimized.

In addition, it is possible to improve the resistance to cyclic repetition of amorphous and crystalline and to further optimize the film resistivity.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is an SEM photograph (image) of a powder obtained by reducing a gas atomized powder of a Ge _{22 .2} Sb _{22 .2} Te _{55 .6} (at%) alloy raw material.
2 is an SEM photograph (image) of a gas atomized powder of Ge _{22 .2} Sb _{22 .2} Te _{55 .6} (at%) alloy raw material.

The present invention provides a sintered body sputtering target obtained by sintering powder of an Sb-Te alloy powder for sintering which has an average particle diameter of 0.1 to 200 탆 and an oxygen content of not more than 1000 wtppm, .

In general, the gas atomized powder can obtain a very fine powder as compared with the mechanical powder and can further prevent the contamination due to the use of the pulverizing machine, so that it can be used as the sintered powder as it is. However, it is not necessary to be limited to this gas atomization method, and any known grinding process can be employed as long as the alloy powder of the present invention can be obtained.

However, in the actually prepared pulverized powders, the particle size varies, and there are particles exceeding 200 탆 in diameter. When sintering, these coarse grains become the starting point, and cracks sometimes occur in the sintered body target. When such a target is used for sputtering, it is likely to become a starting point of arcing. Therefore, in order to avoid such a problem, it is preferable to adjust the particle size according to classification.

It is possible to obtain an atomized powder having an appropriate particle size distribution (average particle diameter of 0.1 to 200 占 퐉). By reducing the atomized powder with this method, it is possible to make the particle size finer and adjust its particle size distribution. As a result of the reduction treatment, an oxide generated by the incorporation of oxygen, that is, an oxide of Sb or Te, that is, Ag, Al, As, Au, B, C, Ga, Ge, In, P, Pd, Pt, S, Se, Si, and Ti, so that occurrence of arcing originating from these oxides can be suppressed.

From the above, in the present invention, the Sb-Te alloy is dissolved and then pulverized and further reduced to obtain an alloy powder. As a result, a spherical powder having an average particle diameter of 0.1 to 200 μm with an oxygen content of 1000 wtppm or less can be produced. In the target obtained by sintering the spherical Sb-Te alloy powder obtained, And the occurrence of cracking can be reduced. More preferably, the oxygen content is not more than 500 wtppm, more preferably, the oxygen content is not more than 300 wtppm, and still more preferably, the oxygen content is not more than 100 wtppm.

In the reducing treatment by heat treatment in an inert gas, the heating time and time in the hydrogen reduction treatment, the acid concentration, the treatment time and the degree of vacuum in the acidic vacuum drying treatment, (Mg, Fe) can be achieved by adjusting the mixing throughput and the calcining temperature.

These conditions are not fixed because they need to be adjusted depending on the throughput of the Sb-Te alloy powder and the presence (content) of oxygen. Therefore, it is arbitrarily adjusted according to the target condition, that is, the target oxygen amount.

Generally, since the Sb-Te alloy has a high viscosity, a large amount of the Sb-Te alloy is adhered to the crushing jig at the time of machine crushing, and the powder particles contact with each other and the powder particles are rolled. Therefore, when the pulverization is performed for a long period of time, particles having a flattened shape (flat plate shape) are formed and fine particles having a particle size of less than 0.1 mu m are formed.

Such flat plate-shaped particles have a large particle shape and cause non-uniformity of the particles, and thus can not be used for a sintered body, resulting in deterioration of the yield of raw materials. In this sense, the atomization method in which spherical powders are well obtained is a recommended grinding method.

In the present invention, finally, a spherical powder having an average particle diameter of 0.1 to 200 탆 can be obtained. The overall shape of the Sb-Te alloy is a spherical powder having an average particle diameter of 0.1 to 200 占 퐉. The spherical powder having an average particle diameter of 10 to 50 占 퐉 and the spherical powder having an average particle diameter of 0.1 to 10 占 퐉 Or a mixture of small-diameter spherical powder. It is preferable that the volume ratio of the large-diameter spherical powder to the small-diameter spherical powder is in the range of 10 to 90%, respectively. This can be adjusted in the production step of the pulverized powder such as gas atomization.

When sintering, small diameter particles are inserted between large diameter particles to obtain a uniform and dense sintered body, which is an advantage. The volume ratio of 10 to 90% represents the optimum condition for this.

As the additive element, Ag, Al, As, Au, B, C, Ga, Ge, In, P, Pd, Pt, or the like is added to the sintered product sputtering target obtained by sintering the Sb- S, Se, Si, and Ti can be contained in an amount of at most 30 at%. This makes it possible to obtain a Sb-Te-based alloy sintered product sputtering target having fine crystal grains and high strength.

With this added element, the crystallization rate can be optimized, and the melting point and the crystallization temperature can be optimized. In addition, it is possible to improve the resistance to cyclic repetition of amorphous and crystalline, and to further optimize the film resistivity.

The addition amount of the additional elements is adjusted depending on the characteristics of the elements. Al, As, Au, B, C, Ga, or the like is added to the phase change recording material because the effect of addition is not exhibited when the addition amount is less than 1 at% The addition amount of at least one element selected from Ge, In, P, Pd, Pt, S, Se, Si and Ti is preferably 1 to 30 at%. The selection and addition of such elements is arbitrary.

Generally, the erosion surface after sputtering tends to become a coarse surface with a surface roughness Ra of 1 占 퐉 or more and tends to be more coarse with the progress of sputtering. In the Sb-Te alloy sputtering target of the present invention, A very specific Sb-Te based alloy sputtering target is obtained in which the surface roughness Ra of the surface is 0.5 mu m or less.

As described above, in the target having a uniform fine crystal structure, the surface unevenness due to the sputter erosion is reduced, and generation of particles due to the redisposition (reattachment) film peeling to the upper surface of the target can be suppressed.

In addition, there is an advantage that the compositional change between the in-plane and the lot of the sputter film is suppressed by the microstructure, and the quality of the phase change recording layer is stabilized. In addition, it is possible to effectively suppress the occurrence of the putty, the abnormal discharge, the nodule, and the like when the sputtering is performed in this way.

In the Sb-Te-based sputtering target of the present invention, it is important to improve the resistance force to 60 MPa or more. By significantly improving the mechanical strength as described above, it is possible to effectively reduce the occurrence of cracks or cracks in the target.

Further, the Sb-Te-based sputtering target of the present invention has an oxygen content of not more than 1000 wtppm to further reduce the generation of cracks or cracks in the target by further improving the mechanical strength, . Thus, reduction plays an important role.

Further, the present invention can provide an Sb-Te alloy powder for sinter added with 1 to 30 at% of any one or more components selected from among N, C, S, P, Si and B elements. As described above, by the addition of these light elements, the thin film enters between the lattices of the Sb-Te alloy, and the resistivity of the thin film can be optimized. In addition, the target has an effect of being able to increase the mechanical strength because it is precipitated at grain boundaries and functions as a buffer layer for internal stress.

Further, in this case, there are elements overlapping the additive element described in the paragraph <66>, and it should be easily understood that the selection and adjustment are arbitrary. In order to retain the effect of such addition, 1 at% or more is necessary, and the addition is arbitrary. When added, the content should be 30 at% or less. When the upper limit is exceeded, the target strength is lowered and the target is cracked during or during the production of the target, which is not preferable.

Powders to be used in the production of the Sb-Te-based sputtering target of the present invention having fine crystal grains and high strength can be powders having a specific surface area (BET) of 0.5 m 2 / g or more and 0.7 m 2 / g or more.

It should be understood that while the above describes the essential components, the additional and additional requirements are not necessarily incorporated into the essential components of the invention. That is, it is a requirement that can be arbitrarily adopted depending on the property or purpose required for the target.

Example

An embodiment of the present invention will be described. The present embodiment is merely an example, and the present invention is not limited to this example. That is, the present invention includes all aspects or modifications other than the embodiment within the scope of the technical idea of the present invention.

(Example 1)

Ge _{22 .2} Sb _{22 .2} Te _{55 .6} (at%) Atomization powder was prepared by using a gas atomization apparatus. The average particle diameter of the atomized powder was 15 mu m and the oxygen content was 1100 wtppm.

The gas atomization powder was further immersed in a 50% nitric acid aqueous solution for 10 minutes and subjected to a reduction treatment by drying in a vacuum at 10 Pa for 6 hours. By this reduction treatment, the oxygen content became 550 wt ppm. The average particle diameter was 14 mu m.

The powder thus obtained was subjected to hot pressing to obtain a high-density target having a relative density of 100%. The resistance of this target was 70 MPa, and a sintered body (target) having a very high strength was obtained. No cracks were observed.

Sputtering was performed using this target. As a result, arcing did not occur, the average number of particles generated after 10 kW · hr was 30, and the surface roughness Ra of the eroded surface after sputtering was 0.4 μm. The above results are shown in Table 1.

(Example 2)

The gas atomization powder of Example 1 was subjected to a reduction treatment by heat treatment at 500 DEG C for 2 hours in an Ar atmosphere. By this reduction treatment, the oxygen content was 290 wtppm. The average particle diameter was 13 mu m.

An SEM photograph (image) of the powder thus obtained is shown in Fig. The scale of FIG. 1 is as shown in the figure.

As shown in Fig. 1, a neat spherical powder having a particle diameter of 1 to 50 mu m was obtained. In this case, the spherical powder having a large diameter with an average particle diameter of 10 to 50 μm was about 80% by volume, and the spherical powder with a small diameter having an average particle diameter of 1 to 10 μm had a volume ratio of about 20%. In addition, the spherical powder having a large diameter was a spherical powder having a particle size of about 15 to 20 μm.

Fig. 2 is shown as a reference diagram. 2 is a gas atomized powder, which is a powder that does not control the particle diameter of the powder, that is, &quot; as it exits &quot;. This gas atomized powder having a particle diameter in the range of 60 to 70 탆 is placenta, and is not suitable for the purpose of the present invention.

The powder thus obtained was subjected to hot pressing to obtain a high-density target having a relative density of 100%. The resistance of this target was 70 MPa, and a sintered body (target) having a very high strength was obtained. Cracks were not observed at all.

Sputtering was performed using this target. As a result, arcing did not occur, the average number of particles generated after 10 kW · hr was 25, and the surface roughness Ra of the eroded surface after sputtering was 0.4 μm. The above results are shown in Table 1.

(Example 3)

The gas atomization powder of Example 1 was subjected to a reduction treatment by heat treatment at 500 DEG C for 2 hours in a hydrogen atmosphere. By this reduction treatment, the oxygen content was 90 wt ppm. The average particle diameter was 13 mu m.

The powder thus obtained was subjected to hot pressing to obtain a high-density target having a relative density of 100%. The resistance of this target was 80 MPa, and a sintered body (target) having a very high strength was obtained. No cracks were observed.

Sputtering was performed using this target. As a result, arcing did not occur, and the average number of particles generated after 10 kW · hr was 19, and the surface roughness Ra of the eroded surface after sputtering was 0.4 μm. The above results are shown in Table 1.

(Example 4)

The gas atomized powder of Example 1 was further mixed with the iron powder which had been subjected to reduction treatment in advance, calcined at 300 ° C for 24 hours, and then subjected to reduction treatment by removing iron powder. By this reduction treatment, the oxygen content became 600 wtppm. The average particle diameter was 14 mu m.

The powder thus obtained was subjected to hot pressing to obtain a high-density target having a relative density of 100%. The resistance force of this target was 60 MPa, and a sintered body (target) having a very high strength was obtained. No cracks were observed. Then, sputtering was performed using this target.

 As a result, arcing did not occur, the average number of particles generated after 10 kW · hr was 35, and the surface roughness Ra of the erosion surface after sputtering was 0.4 μm. Table 1 shows the above results.

(Example 5)

The gas atomization powder of Example 1 was subjected to a reduction treatment by heat treatment at 500 DEG C for 5 hours in an Ar atmosphere. By this reduction treatment, oxygen was further reduced, and the oxygen content became 200 wtppm.

The average particle diameter after the reduction treatment was 13 占 퐉. The characteristics of the other powders were not particularly changed, but the force of resistance was 72 MPa, and a sintered body (target) having higher strength was obtained as compared with Example 2. No cracks were observed.

From the above, it was confirmed that the reducing treatment contributes to the reduction of oxygen and the increase of the resistance force. This is not limited to the Ge _{22 .2} Sb _22.2 Te _{55 .6} (at%) alloying material although not specifically shown in the examples, and the same tendency is observed in all of the Sb-Te alloy powder for sintering of the present invention .

Sputtering was performed using this target. As a result, arcing did not occur, the average number of particles generated after 10 kW · hr was 15, and the surface roughness Ra of the eroded surface after sputtering was 0.4 μm. The above results are shown in Table 1.

(Example 6)

Ge _{22 .2} Sb _{22 .2} Te _{55 .6} (at%) The alloy raw material was introduced into a vibrating ball mill as a machine for crushing and subjected to mechanical pulverization using an inert gas of Ar as the atmospheric gas. The mechanical grinding time is 20 minutes. As a result, a powder having an average particle diameter of 20 mu m was obtained. Powders of more than 200 mu m of the pulverized powders were removed according to classification. The pulverized powder had an oxygen content of 2500 wtppm.

The pulverized powder was further immersed in a 50% aqueous solution of nitric acid for 10 minutes, and dried at 6 Pa for 10 minutes under vacuum to effect reduction treatment. By this reduction treatment, the oxygen content was 700 wt ppm. The average particle diameter after the reduction treatment was 19 占 퐉.

The powder thus obtained was subjected to hot pressing to obtain a high-density target having a relative density of 100%. The resistance of this target was 65 MPa, and a sintered body (target) having high strength was obtained. No cracks were observed. Then, sputtering was performed using this target.

As a result, arcing did not occur, the average number of particles generated after 10 kW · hr was 25, and the surface roughness Ra of the erosion surface after sputtering was 0.9 μm, and good results were obtained. The above results are shown in Table 1.

(Example 7)

Ge _{22 .2} Sb _{22 .2} Te _{55 .6} (at%) alloy raw material was jet mill pulverized to obtain powder having an average particle diameter of 2 탆. The pulverized powder had an oxygen content of 6000 wtppm. This pulverized powder was subjected to a reduction treatment by heat treatment at 500 DEG C for 12 hours in a hydrogen atmosphere. By this reduction treatment, the oxygen content was 900 wtppm. The average particle diameter after the reduction treatment was 2 占 퐉.

The powder thus obtained was subjected to hot pressing to obtain a high-density target having a relative density of 100%. The resistance force of this target was 90 MPa, and a sintered body (target) having high strength was obtained. No cracks were observed. Then, sputtering was performed using this target.

As a result, arcing did not occur, the average number of particles generated after 10 kW · hr was 25, and the surface roughness Ra of the erosion surface after sputtering was 0.1 μm, and good results were obtained. The above results are shown in Table 1.

* (Comparative Example 1)

Ge _{22 .2} Sb _{22 .2} Te _{55 .6} (at%) The alloy raw material was introduced into a vibrating ball mill as a machine for crushing and subjected to mechanical pulverization using an inert gas of Ar as the atmospheric gas. The mechanical grinding time is 20 minutes. The oxygen content after the mechanical pulverization was 1500 wtppm. In addition, the maximum particle diameter was very large at 300 탆.

This was classified to obtain a powder having an average particle diameter of 30 mu m. Then, this powder was hot-pressed. As a result, a relative density of 97% and an elastic force of 50 MPa were obtained, and a sintered body (target) with low resistance was obtained. Then, occurrence of cracks was confirmed.

Sputtering was performed using this target. As a result, arcing occurred and the average particle generation number after 10 kW · hr increased to 140. The surface roughness Ra of the erosion surface after the sputtering was 0.9 占 퐉. The above results are shown in Table 1.

As shown above, it was confirmed that the increase of the oxygen content caused a large amount of particles.

(Comparative Example 2)

Ge _{22 .2} Sb _{22 .2} Te _{55 .6} (at%) Atomization powder was prepared by using a gas atomization apparatus. The average particle size of the atomized powder was 15 mu m and the oxygen content was 1100 wtppm.

This powder was hot-pressed. As a result, the relative density was 97% and the spring force was 52 MPa, and a sintered body (target) with low resistance was obtained. Then, occurrence of cracks was confirmed.

Sputtering was performed using this target. As a result, arcing occurred and the average number of particles generated after 10 kW · hr was 90. The surface roughness Ra of the erosion surface after the sputtering was 0.5 占 퐉. The above results are shown in Table 1.

As shown above, it was confirmed that the increase of the oxygen content caused a large amount of particles.

(Comparative Example 3)

The gas atomized powder of Comparative Example 2 was classified to have an average particle diameter of 7 탆. In this case, the oxygen content was 1500 wt ppm.

This powder was hot-pressed. As a result, the relative density was 97% and the spring force was 55 MPa, and a sintered body (target) with low resistance was obtained. Then, occurrence of cracks was confirmed.

Sputtering was performed using this target. As a result, arcing occurred, and the average number of particles generated after 10 kW · hr was 70. The surface roughness Ra of the erosion surface after the sputtering was 0.4 占 퐉. The above results are shown in Table 2.

As shown above, it was confirmed that the increase of the oxygen content caused a large amount of particles.

(Example 8)

The mechanical pulverized powder shown in Comparative Example 1 was classified to obtain an average particle size of 30 mu m and hydrogen reduced to give an average particle size of 26 mu m and an oxygen concentration of 550 ppm.

The powder thus obtained was subjected to hot pressing to obtain a high-density target having a relative density of 100%. The resistance of this target was 65 MPa, and a sintered body (target) having high strength was obtained. No cracks were observed.

Sputtering was performed using this target. As a result, arcing did not occur, the average number of particles generated after 10 kW · hr was 20, and the surface roughness Ra of the erosion surface after sputtering was 0.9 μm, and good results were obtained. Table 1 shows the above results.

(Example 9)

The _{Ag 5 .0 In 5 .0 Sb 70} .0 Te 20 .0 (at%) alloy raw material, the atomized powder was prepared using the gas atomization system. The average particle size of the atomized powder was 15 mu m and the oxygen content was 90 wt ppm.

 The gas atomization powder was subjected to a reduction treatment by heat treatment at 500 DEG C for 2 hours in a hydrogen atmosphere. By this reduction treatment, the oxygen content became 350 wt ppm. The average particle diameter was 13 mu m.

The powder thus obtained was subjected to hot pressing to obtain a high-density target having a relative density of 100%. The resistance of this target was 80 MPa, and a sintered body (target) having a very high strength was obtained. No cracks were observed.

Sputtering was performed using this target. As a result, arcing did not occur, and the average number of particles generated after 10 kW 占 는 was 19, and the surface roughness Ra of the eroded surface after sputtering was 0.4 占 퐉. The above results are shown in Table 1.

(Example 10)

Ge _{21 .1} Sb _{21 .1} Te _{52 .8} B _5.0 (at%) Atomization powder was prepared by using the alloy raw material and the gas atomization apparatus. Thus, a powder having an average particle diameter of 15 mu m was obtained. The pulverized powder had an oxygen content of 1600 wtppm. Boron (B) was added to the pulverized powder in an amount of 5 at% and subjected to a reduction treatment by heat treatment at 500 DEG C for 2 hours in a hydrogen atmosphere. By this reduction treatment, the oxygen content was 85 wt ppm. The average particle diameter was 13 mu m.

 The powder thus obtained was subjected to hot pressing to obtain a high-density target having a relative density of 100%. The resistance of this target was 80 MPa, and a sintered body (target) having a very high strength was obtained. No cracks were observed.

Sputtering was performed using this target. As a result, arcing did not occur, the average number of particles generated after 10 kW 占 는 was 19, and the surface roughness Ra of the eroded surface after sputtering was 0.4 占 퐉. The above results are shown in Table 1.

As apparent from the above Examples and Comparative Examples, it can be seen that the oxygen content has a large influence. As the content of oxygen increases, voids remain in the sintered body and cracks occur. Therefore, the relative density can not be made sufficiently high, and therefore, the target strength after sintering is lowered and a large amount of particles are generated at the time of sputtering Lt; / RTI &gt;

The present invention can provide a Sb-Te alloy powder for sinter which can solve such a problem.

As described above, by using the powder of the present invention, uniformity and fineness of the Sb-Te alloy sputtering target structure can be made, cracks in the sintering target are eliminated, and occurrence of arcing during sputtering can be suppressed Effect is obtained. In addition, the irregularities of the surface due to the sputter erosion are reduced, and the generation of particles due to the peeling of the redistribution film to the upper surface of the target is reduced. In addition, by micronizing and homogenizing the target structure as described above, variations in the in-plane and composition between the in-plane and the lot of the thin film to be produced are suppressed and the quality of the recording layer on the phase change image is stabilized. As a result, the generation of particles is suppressed.

Therefore, an Sb-Te alloy sputtering target for forming a phase change recording layer made of an Sb-Te alloy powder for sintering, for example, an Ag-In-Sb-Te alloy or a Ge-Sb-Te alloy, The Sb-Te alloy powder for sintering, and the Sb-Te alloy powder for sintering.

Claims (7)

Characterized by comprising a mixture of a large diameter powder having an average particle diameter of 1 to 20 μm and an oxygen content of 100 wtppm or less and an average particle diameter of 10 to 50 μm and a small diameter powder having an average particle diameter of 0.1 to 10 μm Sb-Te alloy powder for sintering. Sb-Te-based alloy is dissolved and then processed into powder, and the powder thus obtained is further reduced to have an oxygen content of 100 wtppm or less and an average particle size of 1 to 20 mu m Wherein the Sb-Te-based alloy powder is sintered at a temperature of not less than &lt; RTI ID = 0.0 &gt; 3. The method of claim 2,
A method for producing an Sb-Te alloy powder for sintering according to claim 1, wherein the powder is a mixture of a large-diameter powder having an average particle diameter of 10 to 50 占 퐉 and a small-diameter powder having an average particle diameter of 0.1 to 10 占 퐉. A sintered body made of an Sb-Te-based alloy characterized in that an oxygen content of 100 wtppm or less, an abrupt force of 60 MPa or more, and a relative density of 99.5% or more is produced using the Sb-Te alloy powder for sinter according to claim 1, target. 5. The method of claim 4,
And the surface roughness Ra of the erosion surface of the target is not more than 0.5 占 퐉. The method according to claim 1,
A Sb-Te alloy powder for sintering characterized in that it is made of a mixture of a large diameter powder having an average particle diameter of 10 to 50 占 퐉 and a small diameter powder having an average particle diameter of 1 to 10 占 퐉. 3. The method of claim 2,
A method for producing an Sb-Te alloy powder for sintering according to claim 1, characterized in that it comprises a mixture of a large diameter powder having an average particle diameter of 10 to 50 占 퐉 and a small diameter powder having an average particle diameter of 1 to 10 占 퐉.

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