WO2017047753A1 - スパッタリングターゲット材 - Google Patents
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- WO2017047753A1 WO2017047753A1 PCT/JP2016/077457 JP2016077457W WO2017047753A1 WO 2017047753 A1 WO2017047753 A1 WO 2017047753A1 JP 2016077457 W JP2016077457 W JP 2016077457W WO 2017047753 A1 WO2017047753 A1 WO 2017047753A1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/07—Alloys based on nickel or cobalt based on cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
- H01F41/18—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates by cathode sputtering
- H01F41/183—Sputtering targets therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
- H01J37/3411—Constructional aspects of the reactor
- H01J37/3414—Targets
- H01J37/3426—Material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
- H01J37/3411—Constructional aspects of the reactor
- H01J37/3414—Targets
- H01J37/3426—Material
- H01J37/3429—Plural materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/15—Nickel or cobalt
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/35—Iron
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2304/00—Physical aspects of the powder
- B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
Definitions
- the present invention relates to a sputtering target material useful for the production of alloy thin films in magnetic tunnel junction (MTJ) elements, HDDs, magnetic recording media and the like.
- MTJ magnetic tunnel junction
- Magnetic random access memory has a magnetic tunnel junction (MTJ) element.
- the magnetic tunnel junction (MTJ) element has a structure such as CoFeB / MgO / CoFeB and exhibits characteristics such as a high tunneling magnetoresistance (TMR) signal and a low switching current density (Jc).
- TMR tunneling magnetoresistance
- Jc switching current density
- a CoFeB thin film of a magnetic tunnel junction (MTJ) element is formed by sputtering a CoFeB target.
- a CoFeB sputtering target material for example, as disclosed in JP-A-2004-346423 (Patent Document 1), a sputtering target material having a fine structure utilizing a rapidly solidified structure of atomized powder that has been rapidly solidified. It has been known.
- the sputtering target material having a fine structure utilizing the rapidly solidified structure of Patent Document 1 has a problem that particles are generated during sputtering.
- the present inventors have made extensive developments.
- the rapid solidification structure of atomized powder produced by rapid solidification of gas atomization has few primary crystals without a boride phase.
- (CoFe) 3 B, Co 3 B, or Fe 3 B are formed, and it has been found that particles during sputtering can be reduced by removing them from the atomized powder used as a raw material of the sputtering target material.
- the present invention includes the following inventions. [1] at. %, A sputtering target material containing 10 to 50% of B, the balance consisting of at least one of Co and Fe and inevitable impurities, Intensity ratio of (CoFe) 3 B (121) X-ray diffraction intensity [I [(CoFe) 3 B]] to (CoFe) 2 B (200) X-ray diffraction intensity [I [(CoFe) 2 B]] X-ray diffraction of Co 3 B (121) with respect to [I [(CoFe) 3 B] / I [(CoFe) 2 B]], Co 2 B (200) X-ray diffraction intensity [I (Co 2 B)] The intensity ratio [I (Co 3 B)] to the intensity ratio [I (Co 3 B) / I (Co 2 B)] or the X-ray diffraction intensity [I (Fe 2 B)] of Fe 2 B (200) The sputtering target material whose intensity ratio [
- [I (Co 3 B)] is a sputtering target material according to the above [1], wherein the intensity ratio [I (Co 3 B) / I (Co 2 B)] is 1.50 or less.
- [I (Fe 3 B)] is a sputtering target material according to the above [1], wherein the intensity ratio [I (Fe 3 B) / I (Fe 2 B)] is 1.50 or less.
- (CoFe) 3 B, Co 3 B or Fe 3 B is small, the sputtering target material is provided which can suppress the generation of particles during sputtering.
- the sputtering target material of the present invention has an extremely excellent effect that the product yield of the sputtered film can be improved.
- the B content is 10 to 50%. If the B content is less than 10%, the alloy thin film formed during sputtering is not sufficiently amorphous, and if the B content exceeds 50%, particles generated during sputtering cannot be reduced. Therefore, the B content is adjusted to 10 to 50%.
- the content of B is preferably 20 to 50%.
- the balance consists of at least one of Co and Fe and inevitable impurities.
- Co and Fe are elements that impart magnetism, and the total content of Co and Fe is 50% or more.
- the “total content of Co and Fe” means the one content.
- the sputtering target material according to the present invention may contain unavoidable impurities up to 1000 ppm.
- the intensity ratio [I [(CoFe) 3 B] / I [(CoFe) 2 B]] is, for example, 1.4 or less, 1.3 or less, 1.2 or less, 1.1 or less, 1.0 or less, 0.9 or less, 0.8 or less, 0.7 or less, 0.6 or less, or 0.5 or less.
- the lower limit value of the intensity ratio [I [(CoFe) 3 B] / I [(CoFe) 2 B]] is 0.0.
- (CoFe) X-ray diffraction intensity of 2 B (200) [I [(CoFe) 2 B]], among the X-ray diffraction peaks were measured using a Cu-K [alpha line, (CoFe) of 2 B This means the intensity of the peak attributed to the (200) plane, and the X-ray diffraction intensity [I [(CoFe) 3 B]] of (CoFe) 3 B (121) is measured by using Cu—K ⁇ rays. Of the line diffraction peaks, it means the intensity of the peak attributed to the (121) plane of (CoFe) 3 B.
- the intensity ratio [I (Co 3 B) / I (Co 2 B)] of the diffraction intensity [I (Co 3 B)] is 1.50 or less.
- the intensity ratio [I (Co 3 B) / I (Co 2 B)] is, for example, 1.4 or less, 1.3 or less, 1.2 or less, 1.1 or less, 1.0 or less, 0.9 or less. 0.8 or less, 0.7 or less, 0.6 or less, or 0.5 or less.
- the lower limit value of the intensity ratio [I (Co 3 B) / I (Co 2 B)] is 0.0.
- X-ray diffraction intensities of Co 2 B (200) [I (Co 2 B)] were measured using a Cu-K [alpha line, belonging to the (200) plane of Co 2 B to mean intensities of the peaks
- Co 3 B X-ray diffraction intensity [I (Co 3 B)] of the (121) among the X-ray diffraction peaks were measured using a Cu-K [alpha line, of Co 3 B It means the intensity of the peak attributed to the (121) plane.
- the intensity ratio [I (Fe 3 B) / I (Fe 2 B)] of the diffraction intensity [I (Fe 3 B)] is 1.50 or less.
- the intensity ratio [I (Fe 3 B) / I (Fe 2 B)] is, for example, 1.4 or less, 1.3 or less, 1.2 or less, 1.1 or less, 1.0 or less, 0.9 or less. 0.8 or less, 0.7 or less, 0.6 or less, or 0.5 or less.
- the lower limit value of the intensity ratio [I (Fe 3 B) / I (Fe 2 B)] is 0.0.
- X-ray diffraction intensity of Fe 2 B (200) [I (Fe 2 B)] of the X-ray diffraction peaks were measured using a Cu-K [alpha line, belonging to the (200) plane of Fe 2 B to mean intensities of the peaks, Fe 3 B X-ray diffraction intensity [I (Fe 3 B)] of the (121), among the X-ray diffraction peaks were measured using a Cu-K [alpha line, the Fe 3 B It means the intensity of the peak attributed to the (121) plane.
- (CoFe) 3 B, Co 3 B, and Fe 3 B are not stable as compounds, if they are present in the sputtering target material, they cause particles during sputtering.
- (CoFe) 2 B, (Co 2 B), (CoFe) with respect to Fe 2 B which is constantly formed as a stable compound when the B content is in the range of 10 to 50%.
- the ratio of 3 B, Co 3 B, and Fe 3 B is determined by the X-ray diffraction intensity ratio [I [(CoFe) 3 B] / I [(CoFe) 2 B]], [I (Co 3 B) / I (Co 2 B)], can be reduced [I (Fe 3 B) / I ((Fe 2 B)] by is adjusted to 1.50 or less, particles during sputtering.
- (CoFe) 3 B and (CoFe) 2 B are obtained by replacing part of Co in Co 3 B and (Co 2 B) with Fe, respectively.
- the raw materials to be melted are weighed so as to have the component compositions shown in Tables 1 and 2 and melted by induction heating in a refractory crucible in a reduced pressure Ar gas atmosphere or vacuum atmosphere.
- the solidification rate can be controlled by adjusting the Ar gas injection pressure. The greater the injection pressure, the greater the coagulation rate.
- the particle size distribution of the gas atomized powder can be adjusted by controlling the solidification rate. The faster the solidification rate, the smaller the width of the particle size distribution.
- the structure After removing coarse particles not suitable for molding having a particle size of 500 ⁇ m or more from the obtained gas atomized powder, the structure is rapidly solidified due to the influence of rapid cooling by atomization from the powder from which coarse particles have been removed. Fine particles were removed to prepare a powder satisfying any of the particle size conditions A, B, and C described later.
- the particle size conditions A, B, and C are defined as follows.
- the particle size condition A is that, in the particle size distribution of the powder (particle group), the cumulative volume of particles having a particle size of 5 ⁇ m or less is 10% or less, and the cumulative volume of particles having a particle size of 30 ⁇ m or less is 40% or less.
- the particle size condition B in the particle size distribution of the powder (particle group), the cumulative volume of particles having a particle size of 5 ⁇ m or less is 8% or less, and the cumulative volume of particles having a particle size of 30 ⁇ m or less is 35% or less. Defined.
- the particle size condition C is that, in the particle size distribution of the powder (particle group), the cumulative volume of particles having a particle size of 5 ⁇ m or less is 5% or less and the cumulative volume of particles having a particle size of 30 ⁇ m or less is 30% or less.
- the powder that satisfies all the particle size conditions A, B, and C is a powder that satisfies the particle size condition C
- the powder that satisfies the particle size conditions A and B is a powder that satisfies the particle size condition B.
- Removal of coarse particles having a particle diameter of 500 ⁇ m or more can be performed by classification using a sieve having an opening of 500 ⁇ m or less, for example, an opening of 250 to 500 ⁇ m. Removal of fine particles for preparing a powder satisfying any of the particle size conditions A, B, and C can be performed by classification using a sieve having an opening of 5 ⁇ m or less and / or an opening of 30 ⁇ m or less. In this example, the removal of coarse particles not suitable for molding having a particle size of 500 ⁇ m or more is performed by classification using a sieve having an opening of 500 ⁇ m.
- Fine particles for preparing a powder satisfying the particle size condition C are classified by using a sieve having a mesh size of 30 ⁇ m to remove fine particles for preparing a powder satisfying the particle size condition B by classification using a 35 ⁇ m sieve.
- the particle size and particle size distribution were measured and confirmed with a laser diffraction / scattering particle size distribution measuring device (Microtrack).
- a powder satisfying any of particle size conditions A, B, and C prepared by removing coarse particles and fine particles was used as a raw material powder.
- the raw material powder was deaerated and charged into an SC can having an outer diameter of 220 mm, an inner diameter of 210 mm, and a length of 200 mm.
- the powder-filled billet was sintered under the conditions shown in Tables 1 and 2 to produce a sintered body.
- the solidified molded body produced by the above method was processed into a disk shape having a diameter of 180 mm and a thickness of 7 mm by wire cutting, lathe processing, and planar polishing to obtain a sputtering target material.
- molding method is HIP, hot press, SPS, hot extrusion etc., for example, and is not specifically limited.
- the melted raw material is weighed so as to have the component composition shown in the raw material powder column of Table 3, melted by induction heating in a refractory crucible in a reduced pressure Ar gas atmosphere or vacuum atmosphere, and then discharged from a nozzle having a diameter of 8 mm at the bottom of the crucible
- the gas was atomized with Ar gas.
- the structure is rapidly solidified due to the influence of rapid cooling by atomization from the powder from which coarse particles have been removed. Fine particles were removed to prepare a powder satisfying any one of the particle size conditions A, B, and C. Removal of coarse particles and fine particles was performed in the same manner as described above.
- the particle size distribution of the powder was confirmed by measuring with a laser diffraction / scattering particle size distribution measuring device (Microtrac).
- a powder satisfying any of particle size conditions A, B, and C prepared by removing coarse particles and fine particles was used as a raw material powder.
- the raw material powder was mixed in a V-type mixer at the mixing ratio shown in Table 3 for 30 minutes to obtain the component composition shown in Table 3, and then an SC can having an outer diameter of 220 mm, an inner diameter of 210 mm, and a length of 200 mm. Was deaerated and charged.
- the powder-filled billet was sintered under the conditions shown in Table 3 to produce a sintered body.
- the solidified molded body produced by the above method was processed into a disk shape having a diameter of 180 mm and a thickness of 7 mm by wire cutting, lathe processing, and planar polishing to obtain a sputtering target material.
- molding method is HIP, hot press, SPS, hot extrusion etc., for example, and is not specifically limited.
- Table 4 shows a comparative example.
- the raw materials to be dissolved are weighed so as to have the component composition shown in Table 4, and melted by induction heating in a refractory crucible in a reduced pressure Ar gas atmosphere or vacuum atmosphere, and then discharged from a nozzle having a diameter of 8 mm at the bottom of the crucible, and gas atomized by Ar gas. did. From the obtained gas atomized powder, coarse particles having a particle diameter of 500 ⁇ m or more not suitable for molding were removed, and the powder from which the coarse particles were removed was used as a raw material powder without removing fine particles.
- the raw material powder was deaerated and charged into an SC can having an outer diameter of 220 mm, an inner diameter of 210 mm, and a length of 200 mm.
- the powder-filled billet was sintered under the conditions shown in Table 4 to produce a sintered body.
- the solidified molded body produced by the above method was processed into a disk shape having a diameter of 180 mm and a thickness of 7 mm by wire cutting, lathe processing, and planar polishing to obtain a sputtering target material.
- Nos. 1 to 32 are examples of the present invention.
- 33 to 39 are comparative examples.
- the intensity of the peak attributed to the (200) plane of (CoFe) 2 B among the measured X-ray diffraction peaks is the X of (CoFe) 2 B (200) a ray diffraction intensity [I [(CoFe) 2 B]], (CoFe) X-ray diffraction intensity of the intensity of a peak attributed to (121) plane of the 3 B (CoFe) 3 B (121) [I [(CoFe ) 3 B]] and (CoFe) 2 B (200) X-ray diffraction intensity [I [(CoFe) 2 B]] (CoFe) 3 B (121) X-ray diffraction intensity [I [(CoFe) 3 B]] intensity ratio [I [(CoFe) 3 B] / I [(CoFe) 2 B]] was calculated.
- the intensity of the peak attributed to the (200) plane of Co 2 B among the measured X-ray diffraction peaks is the X-ray diffraction intensity of Co 2 B (200).
- the intensity of the peak attributed to the (200) plane of Fe 2 B among the measured X-ray diffraction peaks is the X-ray diffraction intensity of Fe 2 B (200). and [I [Fe 2 B]], and Fe 3 X-ray diffraction intensity of B of (121) Fe 3 the intensity of a peak attributed to face B (121) [I [Fe 3 B]], Fe 2 B ( 200) X-ray diffraction intensity [I [Fe 2 B]] to Fe 3 B (121) X-ray diffraction intensity [I [Fe 3 B]] intensity ratio [I [Fe 3 B] / I [Fe 2 B]] was calculated.
- the present invention example No. 19 shows the XRD pattern of 70Co-5Fe-25B.
- the XRD pattern of 38 72Co-8Fe-20B is shown in FIG.
- Particles were evaluated as follows. Using the sputtering target material of the example of the present invention or the comparative example, a film was formed on an aluminum substrate having a diameter of 95 mm and a plate thickness of 1.75 mm by DC magnetron sputtering at an Ar gas pressure of 0.9 Pa, and an optical surface analyzer of 0. The number of particles having a size of 1 ⁇ m or more was evaluated. If the number of particles is 10 or less, it is expressed as “A”, 11 to 100 is determined as good and “B”, 101 to 200 is permitted as “C”, and 201 or more is disabled as “D”. "
- the content of B in the sputtering target material is 5%, and the raw material powder does not satisfy any of the particle size conditions A to C (in the particle size distribution of the raw material powder, the cumulative volume of particles having a particle size of 30 ⁇ m or less is 11%. Therefore, the X-ray diffraction intensity ratio exceeded 1.5, and as a result, the particle evaluation was extremely poor.
- the raw material powder does not satisfy any of the particle size conditions A to C (in the particle size distribution of the raw material powder, the cumulative volume of particles having a particle size of 5 ⁇ m or less and the cumulative volume of particles having a particle size of 30 ⁇ m or less are 14% and 45%, respectively. Therefore, the X-ray diffraction intensity ratio exceeded 1.5, and as a result, the particle evaluation was extremely poor.
- each of 1 to 32 contains 10 to 50% of B, and the balance is composed of at least one of Co and Fe and inevitable impurities, and the intensity ratio [I [(CoFe) 3 B] / I [(CoFe ) 2 B], since the intensity ratio [I (Co 3 B) / I (Co 2 B)] or the intensity ratio [I (Fe 3 B) / it (Fe 2 B)] is 1.50 or less
- the particle evaluation was excellent.
- the stable phase in the rapidly solidified structure is removed from the atomized powder produced by the rapid solidification of gas atomization by removing the fine particles whose structure is a rapidly solidified structure under the influence of rapid cooling due to atomization.
- (CoFe) 3 B to remove the Co 3 B or Fe 3 B, by using a (CoFe) 3 B, the raw material powder of Co 3 B or Fe 3 B atomized powder has been removed, a sputtering target material, The amount of (CoFe) 3 B, Co 3 B, or Fe 3 B in the sputtering target material can be reduced.
- the X-ray diffraction intensity [I (Fe 3 B)] of (121) can be reduced, and (CoFe) with respect to the X-ray diffraction intensity [I [(CoFe) 2 B]] of (CoFe) 2 B (200) 3 B (121) X-ray diffraction intensity [I [(CoFe) 3 B]] intensity ratio [I [(CoFe) 3 B] / I [(CoFe) 2 B]], Co 2 B (200) X-ray diffraction intensity [I (Co 2 B)] Co 3 X -ray diffraction intensity of the B (121) for [I (Co 3 B)] intensity ratio [I (Co 3 B) / I (Co 2 B)] or, Fe 2 X-ray
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Abstract
Description
[1]at.%で、Bを10~50%含有し、残部がCoおよびFeの少なくとも1種と不可避的不純物とからなるスパッタリングターゲット材であって、
(CoFe)2B(200)のX線回折強度[I〔(CoFe)2B〕]に対する(CoFe)3B(121)のX線回折強度[I〔(CoFe)3B〕]の強度比[I〔(CoFe)3B〕/I〔(CoFe)2B〕]、Co2B(200)のX線回折強度[I(Co2B)]に対するCo3B(121)のX線回折強度[I(Co3B)]の強度比[I(Co3B)/I(Co2B)]、または、Fe2B(200)のX線回折強度[I(Fe2B)]に対するFe3B(121)のX線回折強度[I(Fe3B)]の強度比[I(Fe3B)/I(Fe2B)]が1.50以下である、スパッタリングターゲット材。
[2]残部がCoおよびFeと不可避的不純物とからなり、(CoFe)2B(200)のX線回折強度[I〔(CoFe)2B〕]に対する(CoFe)3B(121)のX線回折強度[I〔(CoFe)3B〕]の強度比[I〔(CoFe)3B〕/I〔(CoFe)2B〕]が1.50以下である、前記[1]に記載のスパッタリングターゲット材。
[3]残部がCoと不可避的不純物とからなり、Co2B(200)のX線回折強度[I(Co2B)]に対するCo3B(121)のX線回折強度[I(Co3B)]の強度比[I(Co3B)/I(Co2B)]が1.50以下である、前記[1]に記載のスパッタリングターゲット材。
[4]残部がFeと不可避的不純物とからなり、Fe2B(200)のX線回折強度[I(Fe2B)]に対するFe3B(121)のX線回折強度[I(Fe3B)]の強度比[I(Fe3B)/I(Fe2B)]が1.50以下である、前記[1]に記載のスパッタリングターゲット材。
CoおよびFeは、磁性を付与する元素であり、CoおよびFeの合計含有量は50%以上である。なお、本発明に係るスパッタリングターゲット材がCoおよびFeの一方のみを含有する場合、「CoおよびFeの合計含有量」は当該一方の含有量を意味する。本発明に係るスパッタリングターゲット材は、不可避的不純物を1000ppmまで含んでもよい。
表1および2に示す成分組成となるように溶解原料を秤量し、減圧Arガス雰囲気または真空雰囲気の耐火物坩堝内で誘導加熱溶解した後、坩堝下部の直径8mmのノズルより出湯し、Arガスによりガスアトマイズした。なお、Arガスの噴射圧を調整することにより、凝固速度をコントロールすることができる。噴射圧が大きいほど、凝固速度が大きい。凝固速度のコントロールにより、ガスアトマイズ粉末の粒度分布を調整することができる。凝固速度が速いほど、粒度分布の幅は小さい。
粒度条件Aは、粉末(粒子群)の粒度分布において、粒径5μm以下の粒子の累積体積が10%以下、かつ、粒径30μm以下の粒子の累積体積が40%以下となっていることと定義される。
粒度条件Bは、粉末(粒子群)の粒度分布において、粒径5μm以下の粒子の累積体積が8%以下、かつ、粒径30μm以下の粒子の累積体積が35%以下となっていることと定義される。
粒度条件Cは、粉末(粒子群)の粒度分布において、粒径5μm以下の粒子の累積体積が5%以下、かつ、粒径30μm以下の粒子の累積体積が30%以下となっていることと定義される。
なお、粒度条件A,B,Cの全てを満たす粉末は、粒度条件Cを満たす粉末とし、粒度条件A,Bを満たす粉末は、粒度条件Bを満たす粉末とする。
X線源としてCu-Kα線を用いて、スキャンスピード4°/minの条件で、2θ=20~80°におけるX線回折ピークの強度を測定した。
本発明例または比較例のスパッタリングターゲット材を用いて、直径95mm、板厚1.75mmのアルミ基板上にDCマグネトロンスパッタにてArガス圧力0.9Paで成膜し、Optical Surface Analyzerにて0.1μm以上の大きさのパーティクルの数を評価した。パーティクルの数が10個以下を優とし「A」で表し、11~100個を良とし「B」で表し、101~200個を可とし「C」で表し、201個以上を不可とし「D」で表した。
Claims (4)
- at.%で、Bを10~50%含有し、残部がCoおよびFeの少なくとも1種と不可避的不純物とからなるスパッタリングターゲット材であって、
(CoFe)2B(200)のX線回折強度[I〔(CoFe)2B〕]に対する(CoFe)3B(121)のX線回折強度[I〔(CoFe)3B〕]の強度比[I〔(CoFe)3B〕/I〔(CoFe)2B〕]、Co2B(200)のX線回折強度[I(Co2B)]に対するCo3B(121)のX線回折強度[I(Co3B)]の強度比[I(Co3B)/I(Co2B)]、または、Fe2B(200)のX線回折強度[I(Fe2B)]に対するFe3B(121)のX線回折強度[I(Fe3B)]の強度比[I(Fe3B)/I(Fe2B)]が1.50以下である、スパッタリングターゲット材。 - 残部がCoおよびFeと不可避的不純物とからなり、(CoFe)2B(200)のX線回折強度[I〔(CoFe)2B〕]に対する(CoFe)3B(121)のX線回折強度[I〔(CoFe)3B〕]の強度比[I〔(CoFe)3B〕/I〔(CoFe)2B〕]が1.50以下である、請求項1に記載のスパッタリングターゲット材。
- 残部がCoと不可避的不純物とからなり、Co2B(200)のX線回折強度[I(Co2B)]に対するCo3B(121)のX線回折強度[I(Co3B)]の強度比[I(Co3B)/I(Co2B)]が1.50以下である、請求項1に記載のスパッタリングターゲット材。
- 残部がFeと不可避的不純物とからなり、Fe2B(200)のX線回折強度[I(Fe2B)]に対するFe3B(121)のX線回折強度[I(Fe3B)]の強度比[I(Fe3B)/I(Fe2B)]が1.50以下である、請求項1に記載のスパッタリングターゲット材。
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US15/760,421 US10844476B2 (en) | 2015-09-18 | 2016-09-16 | Sputtering target material |
| SG11201802202TA SG11201802202TA (en) | 2015-09-18 | 2016-09-16 | Sputtering target material |
| EP16846624.1A EP3351654A4 (en) | 2015-09-18 | 2016-09-16 | sputter target |
| KR1020187006796A KR102620685B1 (ko) | 2015-09-18 | 2016-09-16 | 스퍼터링 타겟재 |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2015184644A JP6660130B2 (ja) | 2015-09-18 | 2015-09-18 | CoFeB系合金ターゲット材 |
| JP2015-184644 | 2015-09-18 |
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| Publication Number | Publication Date |
|---|---|
| WO2017047753A1 true WO2017047753A1 (ja) | 2017-03-23 |
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| Application Number | Title | Priority Date | Filing Date |
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| PCT/JP2016/077457 Ceased WO2017047753A1 (ja) | 2015-09-18 | 2016-09-16 | スパッタリングターゲット材 |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US10844476B2 (ja) |
| EP (1) | EP3351654A4 (ja) |
| JP (1) | JP6660130B2 (ja) |
| KR (1) | KR102620685B1 (ja) |
| SG (2) | SG10201913474RA (ja) |
| TW (1) | TWI715630B (ja) |
| WO (1) | WO2017047753A1 (ja) |
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| JP7682787B2 (ja) | 2019-03-20 | 2025-05-26 | Jx金属株式会社 | スパッタリングターゲット及び、スパッタリングターゲットの製造方法 |
| JP7506477B2 (ja) * | 2020-01-06 | 2024-06-26 | 山陽特殊製鋼株式会社 | スパッタリングターゲット材の製造方法 |
| JP7564626B2 (ja) | 2020-02-13 | 2024-10-09 | 山陽特殊製鋼株式会社 | スパッタリングターゲット材及びその製造方法 |
| TWI829184B (zh) * | 2022-06-07 | 2024-01-11 | 光洋應用材料科技股份有限公司 | 鐵磁性自由層、包含其的疊層結構、磁穿隧結接面結構、磁阻式隨機存取記憶體和鐵鈷基靶材 |
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| JP2004346423A (ja) * | 2003-04-30 | 2004-12-09 | Hitachi Metals Ltd | Fe−Co−B系合金ターゲット材、その製造方法、軟磁性膜および磁気記録媒体ならびにTMR素子 |
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| US6759005B2 (en) * | 2002-07-23 | 2004-07-06 | Heraeus, Inc. | Fabrication of B/C/N/O/Si doped sputtering targets |
| US7141208B2 (en) * | 2003-04-30 | 2006-11-28 | Hitachi Metals, Ltd. | Fe-Co-B alloy target and its production method, and soft magnetic film produced by using such target, and magnetic recording medium and TMR device |
| JP2005320627A (ja) * | 2004-04-07 | 2005-11-17 | Hitachi Metals Ltd | Co合金ターゲット材の製造方法、Co合金ターゲット材および垂直磁気記録用軟磁性膜ならびに垂直磁気記録媒体 |
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2015
- 2015-09-18 JP JP2015184644A patent/JP6660130B2/ja active Active
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2016
- 2016-09-16 KR KR1020187006796A patent/KR102620685B1/ko active Active
- 2016-09-16 SG SG10201913474RA patent/SG10201913474RA/en unknown
- 2016-09-16 EP EP16846624.1A patent/EP3351654A4/en not_active Ceased
- 2016-09-16 US US15/760,421 patent/US10844476B2/en active Active
- 2016-09-16 WO PCT/JP2016/077457 patent/WO2017047753A1/ja not_active Ceased
- 2016-09-16 SG SG11201802202TA patent/SG11201802202TA/en unknown
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Also Published As
| Publication number | Publication date |
|---|---|
| US20180245211A1 (en) | 2018-08-30 |
| JP6660130B2 (ja) | 2020-03-04 |
| TWI715630B (zh) | 2021-01-11 |
| KR102620685B1 (ko) | 2024-01-02 |
| TW201726955A (zh) | 2017-08-01 |
| EP3351654A4 (en) | 2019-04-17 |
| EP3351654A1 (en) | 2018-07-25 |
| JP2017057477A (ja) | 2017-03-23 |
| SG10201913474RA (en) | 2020-03-30 |
| KR20180054596A (ko) | 2018-05-24 |
| US10844476B2 (en) | 2020-11-24 |
| SG11201802202TA (en) | 2018-04-27 |
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