CN111712587A - Sputtering target material - Google Patents

Sputtering target material Download PDF

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CN111712587A
CN111712587A CN201980013051.9A CN201980013051A CN111712587A CN 111712587 A CN111712587 A CN 111712587A CN 201980013051 A CN201980013051 A CN 201980013051A CN 111712587 A CN111712587 A CN 111712587A
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sputtering target
phase
sputtering
less
powder
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新村梦树
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Sanyo Special Steel Co Ltd
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Sanyo Special Steel Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/02—Alloys based on vanadium, niobium, or tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/06—Alloys based on chromium
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • 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
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Vapour Deposition (AREA)
  • Powder Metallurgy (AREA)

Abstract

The present invention addresses the problem of providing a target (2) that is less likely to crack during sputtering, and in order to solve the problem, provides a sputtering target (2) that is a sputtering target (2) that includes an alloy that contains Ta and Cr, and the balance being unavoidable impurities, and that has a flexural strength of 400MPa or more as measured by a three-point bending test.

Description

Sputtering target material
Technical Field
The present invention relates to a sputtering target used for sputtering for forming a thin film of metal.
Background
Hard disks are used as external recording devices such as computers and digital home appliances. In general, a hard disk employs either an in-plane recording method or a perpendicular magnetic recording method. In recent years, there is a demand for a hard disk having an improved recording density. From this viewpoint, the perpendicular magnetic recording system is the mainstream. In a hard disk of a perpendicular magnetic recording system, both densification and stabilization of recording magnetization can be achieved.
Japanese patent No. 4499044 discloses a magnetic recording medium having a laminate and a recording film formed on the laminate. The laminate is formed on a substrate made of glass, aluminum alloy, or the like. The laminate has an adhesion layer, a soft magnetic underlayer, a seed layer, and an intermediate layer. The bonding layer is a film made of Ni-Ta alloy. The film can be formed by sputtering.
A target is used for sputtering. As a method for producing a sputtering target, a casting method such as vacuum melting or electron beam melting, a sintering method using a mixed powder obtained by mixing a plurality of kinds of powders, and a sintering method using an alloy powder are known. Japanese patent laid-open publication No. 2000-206314 discloses a sintering method based on a hot isostatic press.
Documents of the prior art
Patent document
Patent document 1: japanese patent No. 4499044
Patent document 2: japanese patent laid-open No. 2000-206314
Disclosure of Invention
Problems to be solved by the invention
The conventional sputtering target has poor strength. The adhesion layer is thick and thus requires time for sputtering. In order to shorten the time for forming the adhesion layer, a large power is sometimes used. In sputtering at high power, thermal stress strain occurs in the sputtering target. Due to this strain, the sputtering target is sometimes cracked. Further, due to the large power, particles are sometimes generated in the sputtering target.
The invention aims to provide a target material which is difficult to crack during sputtering.
Means for solving the problems
According to an aspect of the present invention, the following sputtering target is provided.
[1] A sputtering target material comprising an alloy containing Ta and Cr with the balance being unavoidable impurities, the sputtering target material having a flexural strength of 400MPa or more as measured by a three-point bending test.
[2] The sputtering target according to [1], having a relative density of 97% or more.
[3]According to [1]Or [2]]The sputtering target material comprises a Cr phase, a Ta phase and Cr2A Ta phase.
[4]According to [3]The sputtering target material contains Cr in an X-ray diffraction (XRD) pattern2The ratio Px of the strength of Ta (220) to the strength of Ta (110) is 10% or less.
[5]According to [3]Or [4 ]]The sputtering target according to the present invention, wherein the Cr phase is present on the surface of the Cr phase2Ta phase of the above Cr2The thickness Tave of the Ta phase is 30 μm or less.
[6] The sputtering target according to any one of [1] to [5], wherein the Ta content is 20 at% or more and 90 at% or less, and the Cr content is 10 at% or more and 80 at% or less.
According to another aspect of the present invention, there is provided a method for manufacturing a sputtering target according to the present invention, including the steps of:
mixing a powder made of Cr with a powder made of Ta to obtain a mixed powder; and
and a step of pressurizing the mixed powder at a temperature of 1000 ℃ to 1350 ℃.
Effects of the invention
The target material according to the present invention is less likely to crack during sputtering.
Drawings
Fig. 1 is an enlarged photograph showing a part of a sputtering target according to an embodiment of the present invention.
Detailed Description
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings as appropriate.
The sputtering target material according to the present invention comprises or is composed of the alloy according to the present invention. The alloy according to the present invention contains Ta and Cr. The balance of the alloy according to the present invention is inevitable impurities. As inevitable impurities, O, S, C and N can be exemplified. In one embodiment, the alloy according to the present invention contains 1 or 2 or more types of unavoidable impurities. In a preferred embodiment, the content of O is 5000ppm or less, the content of S is 200ppm or less, the content of C is 300ppm or less, and the content of N is 300ppm or less. The lower limit of the content of O, S, C and N is zero.
The sputtering target according to the present invention can be manufactured by so-called powder metallurgy. In the method for producing a sputtering target, a powder made of Cr (i.e., an aggregate of Cr particles containing Cr and the balance being unavoidable impurities) and a powder made of Ta (i.e., an aggregate of Ta particles containing Ta and the balance being unavoidable impurities) are mixed to obtain a mixed powder. The mixed powder is composed of a plurality of particles. The mixed powder is pressurized at a high temperature. By this pressurization, the particles and other particles are sintered to obtain a sputtering target.
The sputtering target material according to the present invention preferably has a Cr phase, a Ta phase and Cr2A Ta phase. The Cr phase is derived from particles made of Cr. The Ta phase is derived from particles made of Ta. Cr (chromium) component2Ta is an intermetallic compound. The intermetallic compound is generated by a reaction of Cr and Ta.
Comprising Cr phase, Ta phase and Cr2A sputtering target of Ta phase can obtain a film having excellent characteristics. Further, has a Cr phase, a Ta phase and Cr2In the sputtering target material of the Ta phase, the Ta phase relaxes the stress during sputtering. From these viewpoints, the content of Ta in the sputtering target according to the present invention is preferably 20 at% or more and 90 at% or less, and more preferably 30 at% or more and 80 at% or less. The content of Cr in the sputtering target according to the present invention is preferably 10 at% or more and 80 at% or less, and more preferably 20 at% or more and 70 at% or less.
Fig. 1 is an enlarged photograph showing a part of a sputtering target 2 according to an embodiment of the present invention. The photograph shown in fig. 1 was obtained by energy dispersive X-ray analysis (EDX). In EDXA reflected electron image is observed. As shown in FIG. 1, the sputtering target 2 has a Cr phase 4, a Ta phase 6 and Cr2 A Ta phase 8.
Cr2 The Ta phase 8 is present at the interface between the Cr phase 4 and the Ta phase 6. Cr (chromium) component2The Ta phase 8 is present on the surface of the Cr phase and adheres to the surface of the Cr phase 4. Cr (chromium) component2The Ta phase 8 is brittle. The sputtering target 2 is produced by sintering a mixed powder of a Cr powder (i.e., an aggregate of Cr particles containing Cr and the balance being unavoidable impurities) and a Ta powder (i.e., an aggregate of Ta particles containing Ta and the balance being unavoidable impurities). Therefore, the sputtering target 2 can suppress Cr as compared with a sputtering target obtained by a casting method2Formation of Ta phase 8. Cr (chromium) component2The sputtering target 2 having a small amount of Ta phase 8 has a high bending strength. From the viewpoint of flexural strength, Cr2The thickness Tave of the Ta phase 8 is preferably 30 μm or less, more preferably 25 μm or less, and still more preferably 20 μm or less. Although the thickness Tave is ideally zero, Cr having a thickness Tave of 5 μm or more is actually generated2A Ta phase 8.
In each of the 5-site photographs obtained by EDX, the thickness T was measured at 1 site randomly selected (see fig. 1). Cr (chromium) component2The thickness Tave of the Ta phase 8 is calculated as an average value of these thicknesses T.
As described above, Cr powder is used as the material of the sputtering target 2. The powder can be generally produced by a pulverization method. The average particle diameter D50 of the Cr powder is preferably 10 to 300 μm.
As described above, Ta powder is used as a material of the sputtering target 2. The powder can be generally produced by a chemical reduction method. The average particle diameter D50 of the Ta powder is preferably 1 μm or more and 100 μm or less.
D50 is the particle size at the point where the cumulative volume is 50% on the volume-based cumulative frequency distribution curve obtained by assuming the total volume of the powder as 100%. D50 can be measured by laser diffraction scattering. An apparatus suitable for this measurement is a laser diffraction scattering particle size distribution measuring apparatus "MICROTRAC MT 3000" available from japan electronics inc. In this apparatus, the powder flows into a measuring unit together with pure water, and the particle diameter of the powder is detected based on the light scattering information of the powder.
The Cr powder and the Ta powder were mixed to obtain a mixed powder. The mixed powder is subjected to forming, thereby obtaining a sputtering target 2. In the molding, the mixed powder is pressurized at a high temperature. A typical pressing process is Hot Isostatic Pressing (HIP). The pressure during molding is preferably 50MPa or more and 300MPa or less.
The temperature during sintering is preferably 1000 ℃ or higher and 1350 ℃ or lower. By pressurizing at a temperature of 1000 ℃ or higher, the sputtering target 2 having a large relative density can be obtained. From this viewpoint, the temperature is more preferably 1050 ℃ or higher, and still more preferably 1100 ℃ or higher. By pressurizing at 1350 deg.C or lower, Cr can be suppressed2Formation of Ta phase 8. From this viewpoint, the temperature is more preferably 1300 ℃ or lower, and still more preferably 1250 ℃ or lower.
The bending strength of the sputtering target (e.g., sputtering target 2) according to the present invention as measured by a three-point bending test is preferably 400MPa or more. When a target material having a flexural strength of 400MPa or more is subjected to sputtering, cracking due to thermal stress strain is less likely to occur. The target material with the breaking strength of more than 400MPa is suitable for sputtering under high power. From these viewpoints, the flexural strength is more preferably 450MPa or more, and particularly preferably 500MPa or more.
The flexural strength was measured in accordance with the regulations of "JIS Z2511". The test piece was cut out from the base material by wire cutting. The conditions of the test are as follows.
Size of test piece: 2mm (thickness) × 2mm (width) × 20mm (length)
Distance between fulcrums: 10mm
The load (kN) at the time of bending of the test piece was measured, and the breaking strength BS (MPa) was calculated by the following equation.
BS＝(3×P×L)/(2×t2×W)
t: thickness of test piece (mm)
W: width of test piece (mm)
L: distance between pivots (mm)
P: load at break (kN)
Sputtering target material according to the present inventionSuch as Cr in X-ray diffraction (XRD) pattern of the sputtering target 2)2The ratio Px of the intensity of Ta (220) to the intensity of Ta (110) is preferably 10% or less. The sputtering target having a Px ratio of 10% or less has a high flexural strength. When a sputtering target having a ratio Px of 10% or less is used for sputtering, cracking due to thermal stress strain is less likely to occur. A sputtering target having a ratio Px of 10% or less is suitable for sputtering at high power. From these viewpoints, the ratio Px is more preferably 7% or less, and still more preferably 5% or less. The ideal ratio Px is zero, but in reality, the sputtering target has a ratio Px of 1% or more.
The test piece for XRD had dimensions of 10 mm. times.20 mm. times.5 mm. The test piece was cut out from the base material by wire cutting. The surface of the test piece was smoothed by grinding. The conditions of XRD were as follows.
Ray source: CuKa
2θ：20-80°
For the measurement, for example, a fully automatic multifunction X-ray diffraction apparatus "SmartLab SE" of japan society of japan is used. The ratio Px was calculated from the diffraction pattern obtained by XRD.
The intensity of Ta (110) means the intensity of a peak assigned to the (110) plane of Ta among X-ray diffraction peaks measured by Cu-K α radiation, Cr2The intensity of Ta (220) is attributed to Cr in the X-ray diffraction peak measured by Cu-K α radiation2Intensity of peak of (220) plane of Ta.
The relative density of the sputtering target (for example, sputtering target 2) according to the present invention is preferably 97% or more. A sputtering target having a relative density of 97% or more is less likely to crack during sputtering. In addition, a sputtering target having a relative density of 97% or more is less likely to generate particles during sputtering. From these viewpoints, the relative density is more preferably 98% or more, and still more preferably 99% or more. The desired relative density is 100%.
The relative density is a ratio (%) of the true density of the sputtering target to the theoretical density calculated from the densities of the respective components of the sputtering target. True density (g/cm)3) The test piece for the determination had a size of 10mm × 20mm × 5mm, which was determined by the Archimedes methodThe cut is cut from the parent material. The surface of the test piece was smoothed by grinding. The true density is calculated by dividing the weight in air of the test piece by the volume of the test piece (i.e., the weight in water of the test piece/specific gravity of water at the measurement temperature). Theoretical density ρ (g/cm)3) The following mathematical formula is used to calculate.
ρ(g/cm3)＝100/(CCr/ρCr+CTa/ρTa)
In the mathematical formula, CCrRepresents the content (% by mass) of Cr ρCrRepresents the density (g/cm) of Cr3)，CTaRepresents the content (% by mass) of Ta ρTaRepresents the density (g/cm) of Ta3)。
Examples
The effects of the present invention will be clarified by the following examples, but the present invention should not be construed as being limited to the descriptions of the examples.
[ example 1]
Cr powder and Ta powder were prepared. These powders were mixed in a V-type mixer to obtain a mixed powder having a Cr powder content of 10 at% and a Ta powder content of 90 at%. A pot having a diameter of 200mm and a length of 10mm and made of carbon steel was filled with the mixed powder. After vacuum degassing of the powder, a green body was produced by HIP. The HIP conditions are as follows.
Temperature: 1350 deg.C
Pressure: 120MPa
Retention time: 2 hours
From this green body, a sputtering target of example 1 was obtained. The sputtering target has a disk shape. The diameter of the sputtering target material is 95mm, and the thickness is 2 mm.
Examples 2 to 12 and comparative examples 1 to 2
Sputtering targets of examples 2 to 12 and comparative examples 1 to 2 were obtained in the same manner as in example 1, except that the composition and the HIP temperature were as shown in table 1 below.
Comparative example 3
The sputtering target material of comparative example 3 was obtained by a melting method.
[ characteristics of sputtering target ]
The flexural strength, relative density, and XRD intensity ratios Px and Cr of each sputtering target were measured by the following methods2Thickness Tave of the Ta phase. The test piece for measurement was cut out from the above green body by wire cutting.
The flexural strength was measured in accordance with the regulations of "JIS Z2511". The conditions of the test are as follows.
Size of test piece: 2mm (thickness) × 2mm (width) × 20mm (length)
Distance between fulcrums: 10mm
The load (kN) at the time of bending of the test piece was measured, and the breaking strength BS (MPa) was calculated by the following equation.
BS＝(3×P×L)/(2×t2×W)
t: thickness of test piece (mm)
W: width of test piece (mm)
L: distance between pivots (mm)
P: load at break (kN)
The size of the test piece to be subjected to XRD was set to 10 mm. times.20 mm. times.5 mm. The surface of the test piece was smoothed by grinding. The conditions of XRD were as follows.
Ray source: CuKa
2θ：20-80°
For the measurement, a fully automatic multifunction X-ray diffraction apparatus "SmartLab SE" of Kabushiki Kaisha was used. The intensity of Ta (110) and Cr were determined from the diffraction pattern obtained by XRD2Ta (220) Strength, Cr2The intensity of Ta (110) is the intensity of the peak assigned to the (110) plane of Ta among the X-ray diffraction peaks measured by using Cu-K α radiation, and the ratio Px of the intensity of Ta (220) to the intensity of Ta (110) is the intensity of Cr2The intensity of Ta (220) is attributed to Cr in the X-ray diffraction peak measured by Cu-K α radiation2Intensity of peak of (220) plane of Ta.
The relative density is a ratio (%) of the true density of the sputtering target to the theoretical density calculated from the densities of the respective components of the sputtering target. True density (g/cm)3) The size of the test piece to be measured was set to 10mm × 20mm × 5mm, and the surface of the test piece was smoothed by polishing. The true density is calculated by dividing the weight in air of the test piece by the volume of the test piece (i.e., the weight in water of the test piece/specific gravity of water at the measurement temperature). Theoretical density ρ (g/cm)3) The following mathematical formula is used to calculate.
ρ(g/cm3)＝100/(CCr/ρCr+CTa/ρTa)
In the mathematical formula, CCrRepresents the content (% by mass) of Cr ρCrRepresents the density (g/cm) of Cr3)，CTaRepresents the content (% by mass) of Ta ρTaRepresents the density (g/cm) of Ta3)。
Energy dispersive X-ray analysis (EDX) was performed on 5 sites of each sputtering target, and Cr was measured at 1 site selected at random in each photograph (reflected electron image) of 5 sites obtained by EDX2Thickness T of Ta phase (see fig. 1). The average value of the thicknesses T was calculated and used as Cr of each sputtering target2Thickness Tave of the Ta phase.
[ sputtering ]
Sputtering was performed using each sputtering target, and an adhesion layer was formed on the glass substrate. The thickness of the adhesion layer was 20 nm. The sputtering conditions were as follows.
Vacuum-exhausting to 1 × 10-4After Pa or less, Ar gas with a purity of 99.99% is fed
The internal pressure of the cavity is as follows: 0.6Pa
Cracking of the sputtered target material was visually confirmed. The results are shown in table 1 below.
[ TABLE 1]
Table 1: evaluation results of sputtering target
Figure BDA0002629313550000091
As shown in table 1, the sputtering targets of the examples were excellent in strength. From the evaluation results, the superiority of the present invention is evident.
Industrial applicability
The sputtering target described above can be used for forming various thin films.
Description of the reference numerals
2. sputtering target material
4. Cr phase
6. Ta phase
8···Cr2Ta phase

Claims (6)

1. A sputtering target material is a sputtering target material containing the following alloy,
the alloy contains Ta and Cr, and the balance is inevitable impurities,
the bending strength of the sputtering target material measured by a three-point bending test is more than 400 MPa.
2. The sputtering target according to claim 1,
the relative density is more than 97%.
3. The sputtering target according to claim 1,
having a Cr phase, a Ta phase and Cr2A Ta phase.
4. The sputtering target according to claim 3,
cr in X-ray diffraction XRD patterns2The ratio Px of the strength of Ta (220) to the strength of Ta (110) is 10% or less.
5. The sputtering target according to claim 3,
the Cr is present on the surface of the Cr phase2A Ta phase of said Cr2The thickness Tave of the Ta phase is 30 μm or less.
6. The sputtering target according to claim 1,
the Ta content is 20 at% to 90 at%, and the Cr content is 10 at% to 80 at%.
CN201980013051.9A 2018-02-19 2019-02-08 Sputtering target material Pending CN111712587A (en)

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