CN118077006A - Sputtering target member, sputtering target assembly, and film forming method - Google Patents
Sputtering target member, sputtering target assembly, and film forming method Download PDFInfo
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- CN118077006A CN118077006A CN202280068236.1A CN202280068236A CN118077006A CN 118077006 A CN118077006 A CN 118077006A CN 202280068236 A CN202280068236 A CN 202280068236A CN 118077006 A CN118077006 A CN 118077006A
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- sputtering target
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- recording layer
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- 238000005477 sputtering target Methods 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims description 21
- 230000005291 magnetic effect Effects 0.000 claims abstract description 46
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 150000004767 nitrides Chemical class 0.000 claims abstract description 10
- 239000000696 magnetic material Substances 0.000 claims abstract description 8
- 229910052751 metal Inorganic materials 0.000 claims description 18
- 238000004544 sputter deposition Methods 0.000 claims description 17
- 229910052796 boron Inorganic materials 0.000 claims description 10
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 229910003470 tongbaite Inorganic materials 0.000 claims description 6
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 abstract description 32
- 239000000843 powder Substances 0.000 description 40
- 239000010410 layer Substances 0.000 description 23
- 239000002994 raw material Substances 0.000 description 19
- 239000002184 metal Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 239000010408 film Substances 0.000 description 11
- 238000005245 sintering Methods 0.000 description 10
- 239000011812 mixed powder Substances 0.000 description 8
- 239000000470 constituent Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000007731 hot pressing Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000001513 hot isostatic pressing Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 150000002739 metals Chemical class 0.000 description 5
- 239000011241 protective layer Substances 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000010419 fine particle Substances 0.000 description 4
- 239000006249 magnetic particle Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 229910052726 zirconium Inorganic materials 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000003302 ferromagnetic material Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- -1 hydrocarbon ions Chemical class 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910005335 FePt Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005294 ferromagnetic effect Effects 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/64—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent
- G11B5/65—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
- G11B5/851—Coating a support with a magnetic layer by sputtering
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
Abstract
The invention provides a sputtering target component for a magnetic recording layer, which can inhibit generation of particles. The sputtering target member for a magnetic recording layer comprises: 10 to 70mol% of Co,5 to 30mol% of Pt,1.5 to 10mol% of carbide, and 0 to 30mol% of one or more non-magnetic materials selected from carbon, oxide, nitride and carbonitride.
Description
Technical Field
In one embodiment, the present invention relates to a sputtering target member for a magnetic recording layer. In another embodiment, the present invention relates to a sputtering target assembly including such a sputtering target member. In yet another embodiment, the present invention relates to a film forming method using such a sputtering target member.
Background
In the field of magnetic recording typified by hard disk drives, as a material of a magnetic thin film that plays a recording role, a material using Co, fe, or Ni of a ferromagnetic metal as a base has been used. For example, in a recording layer of a hard disk employing a perpendicular magnetic recording system, which has been practically used in recent years, a composite material in which non-magnetic particles such as oxide particles and carbon particles are dispersed in a co—pt-based ferromagnetic alloy containing Co as a main component is generally used. The recording layer is miniaturized by such a granular structure that the nonmagnetic particles magnetically separate the magnetic particles, and thus the recording amount per unit area increases.
The magnetic thin film is generally produced by sputtering a sputtering target composed of the above-mentioned materials using a magnetron sputtering apparatus from the viewpoint of high productivity. Therefore, conventionally, a sputtering target for forming a magnetic thin film has been developed from various viewpoints.
Patent document 1 (japanese patent application laid-open No. 2013-37730) discloses a sputtering target in which metals (magnetic metals, noble metals) and carbon constituting an L1 0 -type ordered alloy of FePt are mixed.
In order to suppress the expansion of the head pitch of a magnetic recording medium and to improve the recording density, this document discloses a method for manufacturing a perpendicular magnetic recording medium, comprising:
(1) Forming a magnetic recording layer including crystalline particles of an organic alloy and an interface layer composed of carbon on a nonmagnetic substrate, and forming a protective layer precursor composed of carbon and present on the magnetic recording layer,
(2) Irradiating the protective layer precursor with hydrocarbon ions generated by plasma discharge of a hydrocarbon gas to change the protective layer precursor into a protective layer,
The hydrocarbon ion has an energy of 300eV or more when reaching the protective layer precursor.
Patent document 2 (international publication No. 2014/132746) discloses a FePt-C-based sputtering target containing Fe, pt, and C, which is characterized by having the following structure: the C particles of 1 st order particles including unavoidable impurities are dispersed in a FePt-based alloy phase containing 33at% to 60at% Pt, and the balance being Fe and unavoidable impurities so as not to contact each other. According to patent document 2, it is considered that the FePt-C-based sputtering target has fewer particles.
Patent document 3 (japanese patent publication No. 2018-172770) discloses a ferromagnetic material sputtering target comprising Co: pt=x: the total of the metal Co and the metal Pt is 70mol% or more and the metal Cr is 0mol% or more and 20mol% or less in terms of the molar ratio of 100-X (59.ltoreq.X < 100), and the catalyst comprises: a Co particle phase containing 90mol% or more of metallic Co and having an average particle diameter of 30 to 300 [ mu ] m; and, in terms of mole ratio, co: pt=y: 100-Y (20.ltoreq.Y.ltoreq.60.5) contains 70mol% or more of metallic Co and metallic Pt in total, and has an average particle diameter of 7 μm or less. Patent document 3 discloses a ferromagnetic material sputtering target that contains 25mol% or less of one or two or more kinds of non-magnetic materials selected from the group consisting of carbon, oxide, nitride, carbide and carbonitride in total, and it is considered that the ferromagnetic material sputtering target employs a method of making a co—pt alloy phase finer and making a Co phase coarsen, and therefore has a high leakage flux, and can suppress the generation of fine particles even during sputtering.
Patent document 4 (international publication No. 2012/081340) proposes a step of adding B (boron) of 10wtppm or more in addition to SiO 2 to a sputtering target for a magnetic recording film. It is considered that by suppressing the formation of cristobalite, which causes generation of particles during sputtering, microcracking of a target and generation of particles during sputtering can be suppressed, and burn-in time can be shortened.
Prior art literature
Patent literature
Patent document 1: japanese patent laid-open No. 2013-37730
Patent document 2: international publication No. 2014/132746
Patent document 3: japanese patent laid-open publication No. 2018-172770
Patent document 4: international publication No. 2012/081340
Disclosure of Invention
Technical problem to be solved by the invention
In recent years, when a magnetic recording layer is formed, a substrate is heated in advance (for example, at about 200 ℃). Although the main purpose is to improve the crystallinity of the magnetic particles, the oxide particles may diffuse to the magnetic particles under the secondary influence, and the magnetic properties after film formation may be degraded. Therefore, carbon is considered to be used as a grain boundary material that is stable even at high temperatures. However, if only carbon is added, the particles increase sharply, and the yield decreases significantly. Strategies to reduce particulates by employing the techniques described in the prior art documents described above are viable, but there are limits. Therefore, from the viewpoint that the options of the technology can be increased and the possibility of the development of the technology can be further expanded, it is useful if the fine particles can be reduced by a different route therefrom.
Accordingly, in one embodiment, the present invention has been made to solve the above-described problems, and an object of the present invention is to provide a sputtering target member for a magnetic recording layer capable of suppressing generation of fine particles from a point of view different from the conventional art described above. In another embodiment, the present invention provides a sputtering target assembly including such a sputtering target member. In another embodiment, the present invention provides a film forming method using such a sputtering target member.
Method for solving technical problems
The present inventors have conducted intensive studies to solve the above-mentioned problems, and as a result, have found that a co—pt-based sputtering target member having an increased carbide ratio is effective for suppressing particles. The present invention has been completed based on the above knowledge, and examples are hereinafter given.
[1]
The sputtering target member for a magnetic recording layer comprises: 10 to 70mol% of Co,5 to 30mol% of Pt,1.5 to 10mol% of carbide, and 0 to 30mol% of one or more non-magnetic materials selected from carbon, oxide, nitride and carbonitride.
[2]
The sputtering target member for a magnetic recording layer according to [1], wherein the molar ratio of carbide to the total of carbon and carbide is 0.25 or more.
[3]
The sputtering target member for a magnetic recording layer according to [1] or [2], wherein one or more selected from B 4C、Cr3C2 and TiC are contained as carbide.
[4]
The sputtering target member for a magnetic recording layer according to [3], wherein the total content of one or more selected from B 4C、Cr3C2 and TiC is 1.5 to 10 mol%.
[5]
The sputtering target member for a magnetic recording layer according to any one of [1] to [4], wherein the total content of one or more metal elements selected from Cr, ru, B, ti, si and Mn is 30mol% or less.
[6]
The sputtering target member for a magnetic recording layer according to any one of [1] to [5], wherein the relative density is 90% or more.
[7]
A sputtering target assembly comprising the sputtering target member for a magnetic recording layer according to any one of [1] to [6], and a backing tube or backing plate bonded to the sputtering target member.
[8]
A film forming method comprising sputtering the sputtering target member for a magnetic recording layer as described in any one of [1] to [6 ].
ADVANTAGEOUS EFFECTS OF INVENTION
According to an embodiment of the present invention, since carbide is stable even at high temperature, it is possible to suppress the influence on the magnetic characteristics after film formation and to obtain a special effect of reducing particles at the time of sputtering.
Detailed Description
(1. Sputtering target member)
(1-1. Components)
In one embodiment, the sputtering target member of the present invention comprises: 10 to 70mol% of Co, 5 to 30mol% of Pt, and 1.5 to 10mol% of carbide, and one or more non-magnetic materials selected from carbon, oxide, nitride and carbonitride are contained in total at 0 to 30mol%. Among these components, the high proportion of carbide in the whole sputtering target member is advantageous in suppressing particles at the time of sputtering.
The concentration of Co in the sputtering target member is preferably 10 to 70mol% from the viewpoint of forming the magnetic recording layer. The concentration of Co can be appropriately adjusted according to the magnetic characteristics of the magnetic recording layer required, and typically 20 to 70mol%, more typically 30 to 70mol%, and still more typically 40 to 60mol% can be selected. Here, co is considered to be metal Co existing as a simple substance or metal Co alloyed with other metals such as Pt.
The concentration of Pt in the sputtering target member is preferably 5 to 30mol% from the viewpoint of forming the magnetic recording layer. The concentration of Pt can be appropriately adjusted according to the magnetic characteristics of the magnetic recording layer required, and typically, 5 to 25mol%, more typically 10 to 25mol%, and still more typically 10 to 20mol% can be selected. Here, pt is considered to be metallic Pt existing as a simple substance or metallic Pt alloyed with another metal such as Co.
The concentration of carbide in the sputtering target member is preferably 1.5 to 10mol%. The lower limit of the concentration of carbide is 1.5mol% or more, preferably 1.8mol% or more, and more preferably 2.0mol% or more, from the viewpoint of improving the effect of suppressing particles during sputtering. However, if the concentration of the carbide is too high, the effect of suppressing particles is also reduced, and therefore the upper limit of the concentration of the carbide is 10mol% or less, preferably 8.0mol% or less, and more preferably 6.0mol% or less.
The sputtering target member may contain one kind of carbide or two or more kinds of carbide. As the carbide, for example, one or two or more kinds of carbide of an element selected from B, ca, cr, nb, si, ta, ti, W and Zr are exemplified, among which one or two or more kinds selected from B 4C、Cr3C2 and TiC are preferable, one or two kinds selected from B 4 C and Cr 3C2 are more preferable, and B 4 C is still more preferable.
Accordingly, in a preferred embodiment, the sputtering target member contains 1.5 to 10mol%, preferably 1.8 to 8.0mol%, more preferably 2.0 to 6.0mol% of one or two or more selected from B 4C、Cr3C2 and TiC in total.
In a more preferred embodiment, the sputtering target member contains 1.5 to 10mol%, preferably 1.8 to 8.0mol%, and more preferably 2.0 to 6.0mol% of one or two or more selected from B 4 C and Cr 3C2.
In still more preferred embodiments, the sputtering target member contains 1.5 to 10mol% of B 4 C, preferably 1.8 to 8.0mol%, and more preferably 2.0 to 6.0mol%.
In the above sputtering target member, a nonmagnetic material other than carbide may be added from the viewpoint of adjusting the magnetic characteristics of the magnetic recording layer. Specifically, the non-magnetic material selected from one or more of carbon, oxide, nitride, and carbonitride may contain 0 to 30mol%, preferably 0 to 25mol%, and more preferably 0 to 20mol% in total.
As examples of the oxide, one or two or more oxides of elements selected from Al, B, ba, be, ca, ce, co, cr, dy, er, eu, ga, gd, ho, li, mg, mn, nb, nd, pr, sc, si, sm, sr, ta, tb, ti, V, Y, zn and Zr can be cited. Among the oxides, one or two or more oxides of the elements selected from B, co, cr, si and Ti are preferable.
As examples of the nitride, one or two or more kinds of nitrides of elements selected from Al, B, ca, nb, si, ta, ti and Zr can be cited.
As examples of carbonitrides, there may be mentioned carbonitrides of one or two or more elements selected from Ti, cr, V and Zr.
In the sputtering target member, the molar ratio of carbide to the total of carbon and carbide is preferably 0.25 or more, more preferably 0.4 or more, still more preferably 0.6 or more, still more preferably 0.8 or more, and most preferably 1.0, from the viewpoint of effectively suppressing particles during sputtering.
The sputtering target may contain, as a third element, 30mol% or less, for example, 0.01 to 20mol%, and typically 0.05 to 10mol% of one or more metal elements selected from Cr, ru, B, ti, si and Mn. These are metals added as needed to improve the characteristics of the magnetic recording layer. The blending ratio can be variously adjusted within the above-described range, and the properties effective as the magnetic recording layer can be maintained. In the present invention, B is also used as a metal treatment. In the case where the above-described third elements are not elemental metals or alloys, but are present in the form of carbides, oxides, nitrides or carbonitrides, they are not the third elements specified herein but are treated as the non-magnetic material described above.
(1-2. Relative Density)
In one embodiment, the sputtering target member of the present invention preferably has a relative density of 90% or more, more preferably 95% or more. The relative density can be, for example, 90% to 100%. This reduces the occurrence of abnormal discharge (arcing) during film formation, and enables the production of a uniform thin film. In the present specification, the relative density is a value obtained by dividing the actual measured density of the sputtering target member by the calculated density (also referred to as the theoretical density). The measured density was determined by archimedes method. The calculated density is calculated by the following formula assuming that the constituent components of the raw material powder of the target member are mixed and present without being diffused or reacted with each other.
The formula: calculate density = Σ (molecular weight of constituent components of raw material powder x molar concentration of constituent components of raw material powder)/Σ (molecular weight of constituent components of raw material powder x molar concentration of constituent components of raw material powder/literature value density of constituent components of raw material powder)
Here, Σ means that all the constituent components of the target member except for the impurity are summed.
The sputtering target member can be bonded to a base material such as a backing plate or a backing tube, if necessary, and mounted as a sputtering target assembly in a sputtering apparatus. Instead of using a base material, a sputtering target member may be directly mounted as a sputtering target in a sputtering apparatus.
(2. Preparation method)
The sputtering target member of the present invention can be produced by a powder sintering method, for example, by the following method.
First, a raw material powder is prepared according to the composition of a target sputtering target member. Examples of the raw material powder include powder of one or more non-magnetic materials selected from carbon powder, oxide powder, nitride powder, and carbonitride powder, in addition to Co powder, pt powder, and carbide powder. In addition, one or two or more kinds of metal powders selected from Cr, ru, B, ti, si and Mn may be prepared.
The purity of the raw material powder is preferably 90mol% or more, more preferably 95mol% or more, and still more preferably 99.9mol% or more. In typical embodiments, the raw material powder contains no other components than the indicated components and unavoidable impurities.
The upper limit of the median diameter (D50) of the raw material powder is preferably 200 μm or less, more preferably 100 μm or less, still more preferably 50 μm or less, and still more preferably 10 μm or less, respectively, in order to achieve a uniform structure. The lower limit of the median diameter of the raw material powder is preferably 0.1 μm or more, more preferably 0.3 μm or more, and still more preferably 0.5 μm or more, for the reason of preventing oxidation of the raw material powder. The median diameter can be adjusted by comminution or screening.
Next, the prepared raw material powder is weighed to obtain a desired component, and the mixture is pulverized and mixed by a known method such as ball milling to obtain a mixed powder. In this case, it is preferable to seal an inert gas in the pulverizing container to suppress oxidation of the raw material powder as much as possible. As the inert gas, ar and N 2 gas are mentioned.
The upper limit of the median diameter (D50) of the mixed powder is preferably 20 μm or less, more preferably 10 μm or less, still more preferably 5 μm or less, in order to achieve a uniform structure. The lower limit of the median diameter of the mixed powder is preferably 0.1 μm or more, more preferably 0.3 μm or more, still more preferably 0.5 μm or more, for the reason of preventing oxidation of the mixed powder.
In the present invention, the median diameter of each raw material powder and mixed powder means the particle diameter (D50) at which the cumulative value of the particle size distribution calculated by the laser diffraction/scattering method on a volume basis is 50%. In the examples, powder was dispersed in an ethanol solvent and measured using a particle size distribution measuring apparatus of model LA-920 manufactured by horiba, ltd. The refractive index was a value of cobalt metal.
The mixed powder thus obtained is molded and sintered in a vacuum atmosphere or an inert gas atmosphere by a hot pressing method. In addition to the hot pressing method, various pressure sintering methods such as a plasma discharge sintering method can be used. In particular, hot Isostatic Pressing (HIP) is effective for increasing the density of the sintered body, and from the viewpoint of increasing the density of the sintered body, it is preferable to sequentially perform the hot pressing method and the Hot Isostatic Pressing (HIP).
The upper limit of the holding temperature at the time of sintering varies depending on the target composition, but is preferably 1500 ℃ or lower, more preferably 1400 ℃ or lower, still more preferably 1200 ℃ or lower, in order to prevent coarsening of crystal grains. In order to avoid a decrease in the density of the sintered body, the lower limit of the holding temperature during sintering is preferably 600 ℃ or higher, more preferably 650 ℃ or higher, and still more preferably 700 ℃ or higher.
The lower limit of the pressing pressure at the time of sintering is preferably 10MPa or more, more preferably 15MPa or more, and still more preferably 20MPa or more, in order to promote sintering. The upper limit of the pressing pressure at the time of sintering is preferably 70MPa or less, more preferably 50MPa or less, and still more preferably 40MPa or less, in view of the strength of the die.
In order to increase the density of the sintered body, the lower limit of the sintering time is preferably 0.1 hour or more, more preferably 0.2 hour or more, and still more preferably 0.5 hour or more. In order to prevent coarsening of the crystal grains, the upper limit of the sintering time is preferably 10 hours or less, more preferably 5 hours or less, and still more preferably 2 hours or less.
The obtained sintered body is formed into a desired shape by using a lathe, whereby a sputtering target member according to an embodiment of the present invention can be produced. The target shape is not particularly limited, and examples thereof include a flat plate shape (including a disk shape and a rectangular plate shape) and a cylindrical shape. In one embodiment, the sputtering target member of the present invention is particularly useful as a sputtering target member for forming a magnetic thin film having a granular structure.
(3. Film Forming method)
In one embodiment, the present invention provides a film forming method including a step of sputtering using the sputtering target member. The sputtering conditions can be appropriately set.
[ Example ]
Examples of the present invention are shown below together with comparative examples, but the examples and comparative examples are provided for better understanding of the present invention and its advantages, and are not intended to limit the present invention.
(1. Production of sputtering target Member)
As raw material powders, the following powders were prepared. The high purity products each being 99.9 mass% or more contain no other components except the indicated components and unavoidable impurities. Screening can be performed to properly adjust the median diameter of these powders.
Co powder: median diameter (D50) =3.3 μm
Pt powder: median diameter (D50) =21.8 μm
Cr powder: median diameter (D50) =2.7 μm
Powder B: median diameter (D50) =3.9 μm
Powder C: median diameter (D50) =25.5 μm
B 4 C powder: median diameter (D50) =0.5 μm
Cr 3C2 powder: median diameter (D50) =1.2 μm
TiC powder: median diameter (D50) =5.1 μm
B 2O3 powder: median diameter (D50) =0.5 μm
TiO 2 powder: median diameter (D50) =0.9 μm
CoO powder: median diameter (D50) =2.1 μm
Next, the above raw material powders were mixed and generally pulverized by using zirconia balls as a pulverizing medium and using a ball mill so that the molar ratios of the raw material components described in table 1 were set according to the test numbers. The median diameters (D50) of the obtained mixed powders were all about 0.5 to 5.0. Mu.m. Next, the obtained mixed powder was filled in a mold made of carbon, and sintered by hot pressing in a vacuum atmosphere and Hot Isostatic Pressing (HIP) in an Ar atmosphere. Hot pressing at 800-1100 deg.c and 20-30 MPa for 1-2 hr. For densification, hot Isostatic Pressing (HIP) after hot pressing is performed. Thereafter, the sintered body after HIP was ground using a general lathe and a surface milling machine to obtain a disk-shaped sputtering target member having a diameter of 180mm and a thickness of 5 mm.
(2. Relative Density)
For each sputtering target member obtained by the above procedure, the relative density was measured according to the method described above (relative density=measured density/theoretical density×100%). The results are shown in table 1.
[ Table 1-1 ]
(Table 11)
[ Table 1-2 ]
(Continuation of Table 1)
(3. Number of particles)
Each sputtering target member obtained by the above-described steps was mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by ANELVA, inc.). The sputtering conditions were that the sputtering was performed for a total of 2 hours at an input power of 1kw and an ar gas pressure of 1.7Pa, and then film formation was performed on a silicon substrate having a diameter of 4 feet for 20 seconds. Then, the number of fine particles having a particle diameter of 0.07 μm or more attached to the substrate was measured by a surface foreign matter inspection device (CANDELA CS and 920 manufactured by KLA-Tencor Co.). The results are shown in table 2.
[ Table 2]
| Test number | Number of particles to be detected |
| Example 1 | 60 |
| Example 2 | 1500 |
| Comparative example 1 | 2100 |
| Example 3 | 300 |
| Example 4 | 4000 |
| Comparative example 2 | 15000 |
| Comparative example 3 | 20000 |
Example 1, example 2 and comparative example 1, which were identical in the molar concentration of the C source of 2mo1%, were compared with each other except for carbon and carbide. However, the number of particles was smaller in example 1 and example 2 using only carbide as the C source than in comparative example 1 using only carbon as the C source. Comparing example 1 with example 2, it is evident that the particle number is drastically reduced by using B 4 C as carbide.
Example 3, example 4, comparative example 2 and comparative example 3, which are identical in composition except for carbon and carbide, are compared, and they are identical in molar concentration of the C source of 5 mol%. However, the number of particles was smaller in comparative example 2, example 3 and example 4, in which carbide was used as the C source, than in comparative example 3, in which carbon was used only as the C source. Comparing comparative example 2, example 3 and example 4 shows that as the carbide content increases, the number of particles decreases. In addition, the reduction in the number of particles was more remarkable in example 3 and example 4 in which the carbide concentration was 1.5mol% or more, as compared with comparative example 2 in which the carbide concentration was less than 1.5 mol%.
Claims (8)
1. A sputtering target member for a magnetic recording layer, comprising: 10 to 70mol% of Co,5 to 30mol% of Pt,1.5 to 10mol% of carbide, and 0 to 30mol% of one or more non-magnetic materials selected from carbon, oxide, nitride and carbonitride.
2. The sputtering target member for a magnetic recording layer according to claim 1, wherein a molar ratio of carbide to a total of carbon and carbide is 0.25 or more.
3. The sputtering target member for a magnetic recording layer according to claim 1 or 2, wherein one or more kinds selected from the group consisting of B 4C、Cr3C2 and TiC are contained as carbide.
4. The sputtering target member for a magnetic recording layer according to claim 3, wherein the total content of one or more selected from B 4C、Cr3C2 and TiC is 1.5 to 10 mol%.
5. The sputtering target member for a magnetic recording layer according to any one of claims 1 to 4, wherein the total content of one or more metal elements selected from Cr, ru, B, ti, si and Mn is 30mol% or less.
6. The sputtering target member for a magnetic recording layer according to any one of claims 1to 5, wherein the relative density of the sputtering target member for a magnetic recording layer is 90% or more.
7. A sputtering target assembly comprising the sputtering target member for a magnetic recording layer according to any one of claims 1 to 6, and a backing tube or backing plate bonded to the sputtering target member.
8. A film forming method comprising sputtering the sputtering target member for a magnetic recording layer according to any one of claims 1 to 6.
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| Application Number | Priority Date | Filing Date | Title |
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| JP2021181296 | 2021-11-05 | ||
| JP2021-181296 | 2021-11-05 | ||
| PCT/JP2022/035488 WO2023079856A1 (en) | 2021-11-05 | 2022-09-22 | Sputtering target member, sputtering target assembly, and film forming method |
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| JP (1) | JP7412659B2 (en) |
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| US9103023B2 (en) * | 2009-03-27 | 2015-08-11 | Jx Nippon Mining & Metals Corporation | Nonmagnetic material particle-dispersed ferromagnetic material sputtering target |
| JP6728094B2 (en) * | 2017-03-31 | 2020-07-22 | Ｊｘ金属株式会社 | Ferromagnetic material sputtering target |
| JP7242652B2 (en) * | 2018-05-14 | 2023-03-20 | Ｊｘ金属株式会社 | Sputtering target and sputtering target manufacturing method |
| WO2021014760A1 (en) * | 2019-07-23 | 2021-01-28 | Ｊｘ金属株式会社 | Sputtering target member for non-magnetic layer formation |
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- 2022-09-22 CN CN202280068236.1A patent/CN118077006A/en active Pending
- 2022-09-22 WO PCT/JP2022/035488 patent/WO2023079856A1/en active Application Filing
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| WO2023079856A1 (en) | 2023-05-11 |
| TW202325873A (en) | 2023-07-01 |
| JPWO2023079856A1 (en) | 2023-05-11 |
| JP7412659B2 (en) | 2024-01-12 |
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