WO2018096992A1 - 物理蒸着用ターゲット部材及びスパッタリングターゲット部材並びに物理蒸着膜及び層構造の製造方法 - Google Patents

物理蒸着用ターゲット部材及びスパッタリングターゲット部材並びに物理蒸着膜及び層構造の製造方法 Download PDF

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WO2018096992A1
WO2018096992A1 PCT/JP2017/041030 JP2017041030W WO2018096992A1 WO 2018096992 A1 WO2018096992 A1 WO 2018096992A1 JP 2017041030 W JP2017041030 W JP 2017041030W WO 2018096992 A1 WO2018096992 A1 WO 2018096992A1
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Prior art keywords
physical vapor
target member
vapor deposition
film
sputtering target
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PCT/JP2017/041030
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English (en)
French (fr)
Japanese (ja)
Inventor
寛明 久保
康平 川辺
敦志 三谷
宗佑 横山
正信 高巣
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宇部マテリアルズ株式会社
日本タングステン株式会社
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Application filed by 宇部マテリアルズ株式会社, 日本タングステン株式会社 filed Critical 宇部マテリアルズ株式会社
Priority to JP2018552520A priority Critical patent/JPWO2018096992A1/ja
Priority to KR1020197016195A priority patent/KR20190085948A/ko
Priority to DE112017005990.9T priority patent/DE112017005990T5/de
Priority to CN201780072744.6A priority patent/CN109996903A/zh
Publication of WO2018096992A1 publication Critical patent/WO2018096992A1/ja

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Definitions

  • the present invention relates to a physical vapor deposition target member, a sputtering target member, a physical vapor deposition film, and a method for producing a layer structure.
  • the MTJ element has a structure in which a tunnel barrier layer is sandwiched between two ferromagnetic layers, that is, a three-layer structure of a ferromagnetic layer / tunnel barrier layer / ferromagnetic layer.
  • a tunnel barrier layer an Al oxide film (amorphous AlO x film) having an amorphous structure or a crystalline MgO film oriented in (001) plane is used.
  • the amorphous AlO x film has a high junction resistance with the ferromagnetic layer, a large interface roughness with the ferromagnetic layer, a large variation in characteristics, and a small tunnel magnetoresistance ratio (TMR ratio). Therefore, it is not suitable for the tunnel barrier layer of the MTJ element.
  • a crystalline MgO film is suitable for a tunnel barrier layer of an MTJ element because it has a small tunnel resistance (TR) and a large TMR ratio with respect to a ferromagnetic material having a bcc crystal structure such as Fe or FeCo. .
  • the performance of the MTJ element is improved, the MTJ element is miniaturized, and the recording density of the magnetic recording apparatus including the MTJ element is further improved.
  • MgO is easily hydrated, it may react with moisture in the atmosphere to generate hydroxide on the surface, and there is concern about the alteration of the crystalline MgO film and the MgO sputtering target member for forming it. Is done.
  • Patent Document 1 describes a spinel structure MgAl 2 O 4 film in which Al is added to a crystalline MgO film.
  • the spinel structure MgAl 2 O 4 film has a TR lower than that of an amorphous AlO x film by an order of magnitude, a larger TMR ratio, a crystalline MgO compared to a ferromagnetic Co-based full Heusler alloy or CoFe alloy. Since the lattice matching is better than that of the film, it has been found that an epitaxial tunnel junction with few defects can be formed, and is highly expected as a tunnel barrier layer of an MTJ element.
  • the manufacturing method of the spinel structure MgAl 2 O 4 film described in Patent Document 1 is as follows. That is, after laminating by sputtering Mg film and an Al film on the base of the ferromagnetic layers, or subjected to plasma oxidation treatment, or, MgAl 2 by sputtering MgAl 2 alloy on the base of the ferromagnetic layer After forming the alloy film, plasma oxidation is performed to oxidize and crystallize the metal film or the alloy film, thereby forming a spinel structure MgAl 2 O 4 film.
  • An object of the present invention is to provide a physical vapor deposition target member and a sputtering target member that have good lattice matching, have low hydration properties themselves and the physical vapor deposition film to be formed, and have little alteration due to hydration.
  • the third aspect of the present invention provides a physical vapor deposition film in which the deterioration of the base due to oxidation is small, the number of defects generated at the joint with the base is small, the lattice matching with the base is good, and the alteration due to hydration is low
  • the purpose is to do.
  • the deterioration of the base due to oxidation is small, the number of defects generated at the joint between the physical vapor deposition film and the base is small, the lattice matching between the physical vapor deposition film and the base is good, and further, due to hydration
  • An object of the present invention is to provide a layer structure in which the TMR ratio is improved and miniaturization is expected because of little alteration.
  • the first aspect of the present invention contains Mg, M (M is a trivalent metal element) and O as main components, and is converted into MgO and M 2 O 3 oxides of Mg and M, respectively. And a physical vapor deposition target member having a molar ratio of 70:30 to 10:90.
  • physical vapor deposition is performed on a base using a physical vapor deposition target member having a molar ratio of Mg and M converted to MgO and M 2 O 3 oxides of 70:30 to 10:90, respectively.
  • a physical vapor deposition film having good lattice matching with the base can be formed.
  • the physical vapor deposition target member and the physical vapor deposition film are not MgO, there is little alteration due to hydration and excellent stability such as hydration resistance.
  • a second aspect of the present invention is a physical vapor deposition target characterized in that it contains Mg, M (M is a trivalent metal element), and O as main components and includes a crystal phase having a spinel structure. It relates to members.
  • a physical vapor deposition film having good lattice matching with the base can be formed. Furthermore, since the physical vapor deposition target member and the physical vapor deposition film are not MgO, there is little alteration due to hydration and excellent stability such as hydration resistance.
  • M is 1 or 2 chosen from the group which consists of Al and Ga.
  • the light transmittance when thickness is 2 mm is 60% or less.
  • a window material of an electric device or a manufacturing container is well known. do not need. Therefore, by configuring the physical vapor deposition target member so that the light transmittance when the thickness is 2 mm is 60% or less, the physical vapor deposition target member can be more easily and inexpensively manufactured.
  • the dielectric loss at 10 GHz is preferably 45000 GHz or more in terms of the f ⁇ Q value.
  • the dielectric loss of the physical vapor deposition target member at 10 GHz of 45,000 GHz or more in terms of the f ⁇ Q value reflects the small number of defects and inevitable impurities in the physical vapor deposition target member.
  • the whiteness is preferably 30 or more.
  • a whiteness of 30 or more reflects that there are few inevitable impurities and defects in the target member for physical vapor deposition.
  • the target member for physical vapor deposition is suitable for a sputtering target member.
  • a physical vapor deposition film is physically vapor-deposited on a base using the physical vapor deposition target member of the first or second aspect. About.
  • the physical vapor deposition film physically deposited on the base using the physical vapor deposition target member of the first or second aspect is supplied with necessary oxygen (O) from the physical vapor deposition target member. No oxidation treatment is required. For this reason, there is little deterioration of the foundation
  • a physical vapor deposition film having good lattice matching with the base can be formed. Furthermore, since the physical vapor deposition film is not MgO, it is hardly altered by hydration and has excellent stability such as hydration resistance.
  • a physical vapor deposition film is physically vapor-deposited on a base using the physical vapor deposition target member of the first or second aspect of the present invention, and the physical vapor deposition film is strongly
  • the present invention relates to a method for manufacturing a layer structure, wherein a magnetic layer is formed, a base is a ferromagnetic layer, and a physical vapor deposition film is a tunnel barrier layer.
  • the physical vapor deposition film physically deposited on the base using the physical vapor deposition target member of the first or second aspect is supplied with necessary oxygen (O) from the physical vapor deposition target member. No oxidation treatment is required. For this reason, the base is less degraded by oxidation. In addition, since oxidation or crystallization of the metal film or alloy film is unnecessary, defects generated at the joint between the physical vapor deposition film and the base can be reduced. Further, a physical vapor deposition target member containing a crystal phase having a spinel structure, wherein the molar ratio of Mg and M, converted into oxides of MgO and M 2 O 3 , is 70:30 to 10:90, respectively.
  • a physical vapor deposition film having good lattice matching with the base can be formed.
  • the underlying layer is a ferromagnetic layer and the physical vapor deposition film is a tunnel barrier layer, a layer structure in which the tunnel barrier layer is sandwiched between two ferromagnetic layers is formed. Since this layer structure improves the TMR ratio, it is possible to manufacture a magnetic tunnel junction element that is smaller than the conventional one. Furthermore, since the physical vapor deposition film is not MgO, it is hardly altered by hydration and has excellent stability such as hydration resistance.
  • the physical vapor deposition target member of the present invention can be used for known physical vapor deposition methods such as resistance heating vapor deposition, sputtering, electron beam vapor deposition, molecular beam epitaxy, ion plating vapor deposition, and laser ablation.
  • a sputtering target member used in the sputtering method will be described.
  • the present embodiment described below does not unduly limit the contents of the present invention described in the claims, and all the configurations described in the present embodiment are indispensable as means for solving the present invention. Not always.
  • the sputtering target member of this embodiment contains Mg, M (M is a trivalent metal element), and O as a main component.
  • the sputtering target member may contain a subcomponent in addition to the main component.
  • a sputtering film formed by sputtering a sputtering target member containing Mg, M (M is a trivalent metal element) and O as main components is supplied with necessary oxygen (O) from the sputtering target member.
  • the oxidation treatment after film formation is unnecessary. For this reason, there is little deterioration of the foundation
  • the molar ratio of Mg and M contained in the sputtering target member when converted to oxides of MgO and M 2 O 3 is preferably 70:30 to 10:90, more preferably 65:35 to 20:80. More preferably, it is 60:40 to 30:70, and particularly preferably 55:45 to 40:60.
  • the crystal phase and lattice constant of the sputtered film can be controlled by adjusting the molar ratio of Mg and M contained in the sputtering target member when converted to MgO and M 2 O 3 oxides, respectively. Therefore, it is possible to form a sputtered film having good lattice matching with the base.
  • the sputtering target member preferably contains a crystal phase having a spinel structure.
  • M contained in the sputtering target member is preferably 1 or 2 selected from the group consisting of Al and Ga.
  • the light transmittance of the sputtering target member when the thickness is 2 mm is preferably 60% or less, more preferably 45% or less.
  • a window material of an electric device or a manufacturing container is well known, but a sputtering target member needs light permeability as much as the window material. do not do.
  • the inevitable impurities of the sputtering target member are at least 0.5% by mass, preferably 0.1% by mass or less, more preferably 0.01% by mass or less.
  • the dielectric loss of the sputtering target member at 10 GHz is preferably 45000 GHz or more, more preferably 50000 GHz or more, still more preferably 70000 GHz or more, and particularly preferably 80000 GHz or more in terms of f ⁇ Q value.
  • a large f ⁇ Q value of dielectric loss reflects a small number of defects and inevitable impurities in the sputtering target member. By sputtering such a sputtering target member, a uniform sputtered film can be formed with fewer defects and inevitable impurities.
  • the whiteness of the sputtering target member is preferably 30 or more, more preferably 50 or more, still more preferably 60 or more, and particularly preferably 65 or more. High whiteness reflects that there are few inevitable impurities and defects in the sputtering target member. By sputtering such a sputtering target member, a uniform sputtered film can be formed with fewer defects and inevitable impurities.
  • the whiteness is L * of CIE 1976 (L *, a *, b *). The closer the whiteness is to 100, the closer to white.
  • the surface roughness of the sputtering target member is preferably 5 ⁇ m or less, more preferably 2 ⁇ m or less, and even more preferably 1 ⁇ m or less.
  • the thickness and diameter of the sputtering target member can be changed to a desired thickness and diameter according to the sputtering apparatus, and as an example, the thickness is 2.0 mm or less.
  • the material of the sputtering target member is not particularly limited as long as it is uniform and dense, but is preferably made of a sintered body.
  • a uniform and dense sputtering target member can be produced more easily and cheaply than other solid production methods such as melting and solidification.
  • the relative density of the sintered body is preferably 95% by mass or more, more preferably 98% by mass or more, further preferably 99% by mass or more, and particularly preferably 99.5% by mass or more.
  • the three-point bending strength of the sintered body is preferably 230 MPa or more, more preferably 250 MPa or more, still more preferably 300 MPa or more, and particularly preferably 320 MPa or more.
  • JIS R1601 is used as a method for measuring the three-point bending strength.
  • the average particle diameter of the crystal particles constituting the sintered body is not particularly limited as long as the sintered body can be made uniform and dense.
  • the thickness is preferably 1 to 100 ⁇ m, more preferably 2 to 80 ⁇ m, still more preferably 2 to 60 ⁇ m, and particularly preferably 2 to 50 ⁇ m.
  • the D90 / D10 of the crystal particles constituting the sintered body is not particularly limited as long as the sintered body can be made uniform and dense, but is preferably 4 or less, more preferably 3 or less, and even more preferably 2.5 or less. Particularly preferably, it is 2.3 or less.
  • the average particle size is determined by obtaining the particle size of 200 crystal particles and using a value (D50) of 50% of the particle size distribution (number basis). Similarly, 10% and 90% of the particle size distribution (number basis) are used for D10 and D90.
  • the manufacturing method of the sputtering target member of this embodiment is the raw material mixing process which measures and mixes the raw material powder and obtains a slurry, and dry-granulates the slurry to obtain granulated powder.
  • the manufacturing method of a sputtering target member is demonstrated in more detail.
  • MgO, M 2 O 3 (M is a trivalent metal element) powder can be used as a raw material for the sputtering target member.
  • M is preferably 1 or 2 selected from the group consisting of Al and Ga.
  • the raw material contains MgO and M 2 O 3 as main components, and may further contain subcomponents as necessary.
  • the purity of the raw material powder is preferably higher, at least 99.5% by mass or more, preferably 99.9% by mass or more, more preferably 99.99% by mass or more, and further preferably 99.999% by mass or more. is there.
  • a sputtering target member with few inevitable impurities can be obtained by using a raw material powder with high purity. By sputtering this sputtering target member, it is possible to form a uniform sputtered film with fewer inevitable impurities and defects.
  • D50 average particle diameter
  • it is preferably 1 ⁇ m or less, more preferably 0.5 ⁇ m or less.
  • the raw material of the sputtering target member is not limited to MgO and M 2 O 3 oxides, and compounds such as carbonates and nitrates that become oxides during the manufacturing process can also be used.
  • the raw material powder is weighed.
  • the molar ratio of Mg and M when converted to oxides of MgO and M 2 O 3 is preferably 70:30 to 10:90, more preferably 65:35 to 20:80, and still more preferably 60: 40 to 30:70, particularly preferably 55:45 to 40:60.
  • the crystal phase and lattice constant of the sputtered film can be controlled. Therefore, it is possible to form a sputtered film having good lattice matching with the base.
  • the mixing method is not particularly limited as long as the raw material powder can be uniformly mixed, but, for example, a wet ball mill is suitable.
  • a wet ball mill raw material powder, a dispersion medium, and balls are put in a container and mixed (wet mixing).
  • the dispersion medium water, or an organic solvent such as alcohol or methanol can be used.
  • the mass ratio of the raw material and the dispersion medium is not particularly limited as long as the raw material powder can be mixed uniformly, but is generally 15:85 to 75:25. In order to mix the raw material powder uniformly, a dispersant may be further added.
  • the dispersant is not particularly limited as long as it does not decompose and remain in the degreasing and sintering processes described later.
  • the mixing time is not particularly limited as long as the raw material powder can be uniformly mixed, but is preferably 10 hours or more. If the raw material powder is not uniformly mixed, composition and density unevenness occur in the sputtering target member, and the strength tends to decrease. Further, when such a sputtering target member is sputtered, abnormal discharge is likely to occur during sputtering, and a non-uniform sputtered film is likely to be formed with many defects.
  • the raw material powder is mixed and then the slurry is dried to obtain a dry powder, and the dry powder is heat-treated to obtain a heat-treated powder in which a part or all of the raw material is composed of a composite oxide.
  • the particle size of the heat-treated powder is preferably smaller because it facilitates the sintering in the subsequent sintering step. For this reason, the pulverization step may be further combined with dry pulverization before wet pulverization.
  • (2-2) Dry granulation step The slurry obtained in the raw material mixing step is dried and granulated to obtain a granulated powder suitable for molding.
  • a molding aid may be added to the slurry as needed before drying.
  • molding adjuvant Generally polyvinyl alcohol (PVA), polyethyleneglycol (PEG), cellosol, paraffin, etc. are used in many cases.
  • the drying method is not particularly limited, and for example, a rotary evaporator and a spray dryer are suitable.
  • the higher purity of the granulated powder is suitable, and it is at least 99.5% by mass, more preferably 99.9% by mass, and further preferably 99.99% by mass or more.
  • the granulated powder is molded to obtain a molded body having a predetermined shape.
  • known molding methods such as uniaxial molding using a mold and CIP (cold isostatic pressing) molding can be used alone or in combination.
  • CIP cold isostatic pressing
  • molding pressure can obtain a favorable molded object Generally 100 Mpa or more is preferable.
  • HP hot uniaxial pressing
  • (2-4) Sintering step The compact is sintered to obtain a sintered body.
  • a uniform and dense sputtering target member can be produced more easily and cheaply than other solid production methods.
  • known sintering methods such as atmospheric pressure sintering, HP sintering, and HIP sintering can be used alone or in combination.
  • the sintering temperature is not particularly limited as long as a sintered body can be obtained, but is preferably 1800 ° C. or lower because normal pressure sintering can be performed in an air atmosphere.
  • HP sintering and HIP sintering a sintered body having a high density can be obtained at a sintering temperature lower than that of atmospheric pressure sintering.
  • a granulated powder contains a dispersing agent or a shaping
  • the degreasing temperature is not particularly limited, but a temperature at which the dispersant and the molding aid are completely decomposed and removed, and a temperature rising rate are preferable.
  • the manufacturing method of a sputtering target member may use other solid manufacturing methods, such as melt solidification, if the uniform and precise
  • the sintered body is processed into a desired shape to obtain a sputtering target member.
  • a known method such as cutting, grinding, polishing, or the like can be used as a method for the outer shape processing.
  • the sputtering target member is bonded to a backing plate and is used for sputtering as a sputtering target.
  • sputtering target member As an application example of the sputtering target member of this embodiment, a layer structure in which a tunnel barrier layer is sandwiched between two ferromagnetic layers, that is, a base ferromagnetic layer / tunnel barrier layer / upper strength.
  • An MTJ element having a three-layer structure of magnetic layers will be described.
  • the MTJ element is formed on the substrate.
  • the substrate for example, spinel MgAl 2 O 4 single crystal, Si single crystal, GaAs single crystal, or thermally oxidized Si can be used.
  • a buffer layer made of MgO may be formed on the surface of the substrate as necessary.
  • a base ferromagnetic layer (base), a tunnel barrier layer, and an upper ferromagnetic layer are sequentially formed on the substrate.
  • the underlying ferromagnetic layer, tunnel barrier layer, and upper ferromagnetic layer are, for example, a Co-based full Heusler alloy (for example, Co 2 FeAl 0.5 Si 0.5 ), the sputtering target member of this embodiment, and CoFe, respectively.
  • An alloy for example, Co 75 Fe 25 alloy
  • the tunnel barrier layer (sputtered film) formed by sputtering the sputtering target member of the present embodiment is supplied with necessary oxygen (O) from the sputtering target member, so that an oxidation treatment after film formation is unnecessary. .
  • the tunnel barrier layer does not need to be oxidized or crystallized, defects generated at the junction between the tunnel barrier layer and the underlying ferromagnetic layer can be reduced.
  • the tunnel barrier layer has good lattice matching with the base ferromagnetic layer made of a Co-based full Heusler alloy and the upper ferromagnetic layer made of a CoFe alloy. Therefore, the MTJ element having the underlying ferromagnetic layer / tunnel barrier layer / upper ferromagnetic layer has an improved TMR ratio, and thus a smaller MTJ element can be manufactured.
  • a magnetic recording apparatus provided with this MTJ element can further increase the recording density.
  • the tunnel barrier layer is not MgO, it is hardly altered by hydration and has excellent stability such as hydration resistance.
  • sputtering target member of the present embodiment is not limited to the sputtering method.
  • known physical properties such as resistance heating vapor deposition, electron beam vapor deposition, molecular beam epitaxy, ion plating vapor deposition, and laser ablation. Those skilled in the art will readily understand that they can be used in vapor deposition.
  • Example 1 As raw materials, an MgO powder having an average particle size of 0.2 ⁇ m and a purity of 99.98% by mass and an Al 2 O 3 powder having an average particle size of 0.15 ⁇ m and a purity of 99.99% by mass were used. Weighing was performed so that the molar ratio of MgO to Al 2 O 3 was 50:50.
  • methanol as a dispersion medium, raw material powder, and nylon balls were placed and mixed (wet mixing) for 15 hours to obtain a slurry. The slurry was dried using a rotary evaporator (drying step), and the obtained dry powder was heat treated (heat treatment step) at 1000 ° C.
  • the heat-treated powder was dry pulverized, then placed in a resin ball mill container with methanol as a dispersion medium, the dry-ground pulverized heat-treated powder and alumina balls, and wet pulverized (pulverization step) to obtain a slurry ( Raw material mixing step).
  • the slurry was dried using a rotary evaporator, and the obtained dry powder was crushed and granulated to obtain granulated powder (dry granulation step).
  • the granulated powder was HP sintered in an Ar atmosphere at 1500 ° C. and a pressure of 20 MPa to obtain an HP sintered body.
  • the HP sintered body was further subjected to HIP sintering in an Ar atmosphere, a temperature range of 1400 ° C. to 1550 ° C. and a pressure of 100 MPa to obtain a HIP sintered body (sintering step). Since the HIP sintered body is reduced by sintering in an inert gas atmosphere, an oxidation treatment was performed for 5 hours at 1500 ° C. and normal pressure in an oxygen-containing atmosphere to obtain a sintered body. The sintered body was processed into a desired shape (outer shape processing step), and the obtained sample was used for evaluation.
  • Examples 2, 3 A sample was prepared in the same process as in Example 1 except that the molar ratio of MgO: Al 2 O 3 was 40:60 and 30:70, and was used for evaluation.
  • Example 4 The same raw material powder as in Example 1 was used and weighed so that the molar ratio of MgO: Al 2 O 3 was 20:80. The same wet mixing as in Example 1 was performed to obtain a slurry (raw material mixing step). The slurry was dried using a rotary evaporator to obtain a dry powder. The dried powder was crushed and granulated without heat treatment to obtain a granulated powder (dry granulation step). After the granulated powder was molded at a pressure of 100 MPa (molding process), it was sintered at 1750 ° C. and atmospheric pressure for 3 hours to obtain a sintered body (sintering process). The sintered body was processed into a desired shape (outer shape processing step), and the obtained sample was used for evaluation.
  • a slurry raw material mixing step
  • the slurry was dried using a rotary evaporator to obtain a dry powder.
  • the dried powder was crushed and granulated without heat treatment to obtain a granulated powder (dry
  • Examples 5 to 7 A sample was prepared in the same process as in Example 4 except that the molar ratio of MgO: Al 2 O 3 was set to 10:90, 60:40, and 70:30, and was used for evaluation.
  • Example 8 The same raw material powder as in Example 1 was used and weighed so that the molar ratio of MgO: Al 2 O 3 was 50:50. The same wet mixing as in Example 1 was performed to obtain a slurry. The slurry was dried using a rotary evaporator to obtain a dry powder. The dried powder was heat treated at 1000 ° C. in an air atmosphere to obtain heat treated powder. The heat-treated powder was directly granulated without being crushed. The granulated powder was subjected to HP sintering and HIP sintering similar to Example 1 to obtain a sintered body. The sintered body was processed into a desired shape, and the obtained sample was used for evaluation.
  • Example 9 A sample was prepared in the same process as in Example 4 except that the molar ratio of MgO: Al 2 O 3 was set to 30:70, and used for evaluation.
  • Example 10 The same raw material mixing step (including a drying step, a heat treatment step and a pulverization step) and a dry granulation step as in Example 1 were performed to obtain granulated powder.
  • the granulated powder was oxidized in an oxygen-containing atmosphere at 1700 ° C. and normal pressure for 5 hours.
  • the oxidized powder was directly granulated without being pulverized, and subjected to the same sintering process (HP sintering, HIP sintering and oxidation process) and outer shape processing process as in Example 1, and the obtained sample Was used for evaluation.
  • the density of a sample can be determined by, for example, the Archimedes method.
  • the relative density of the sample can be represented by the ratio of the actually measured sample density to the theoretical density in the sample composition (the product of the theoretical density and the volume ratio of the crystal phase constituting the sample).
  • the particle size of the crystal particles constituting the sample can be obtained by image analysis of the crystal particles on the mirror polished surface of the sample. That is, the Heywood equivalent diameter which converted the area of the crystal grain in the mirror polishing surface into a circle is used for the grain size of a crystal grain.
  • the average particle size the particle size of 200 crystal particles is obtained, and a value (D50) of 50% of the particle size distribution (number basis) is used. Similarly, 10% and 90% of the particle size distribution are used for D10 and D90.
  • the light transmittance of the sample is determined by measuring the total light transmittance of the sample having a thickness of 2 mm with an integrating sphere using a spectrophotometer (JASCO V-670), and a wavelength of 400 to 800 nm. The average light transmittance is used.
  • the dielectric loss of a sample can be determined by the waveguide method.
  • the quality factor Q value is measured at a measurement frequency of 10 GHz using a network analyzer (Agilent Technology 8720ES) by placing a sample in a waveguide.
  • f ⁇ Q value (GHz) which is the product of measurement frequency f (GHz) and Q value, is used as an index of dielectric loss. The larger the f ⁇ Q value, the smaller the dielectric loss.
  • ICP analysis is performed on the concentration of inevitable impurities contained in the sample.
  • Examples 1 to 3 the relative density was as high as 99.6 to 99.8% by mass.
  • the average particle size (D50) of the sintered body was 2.1 to 2.4 ⁇ m, and D90 / D10 was 2.4 to 3.6.
  • the whiteness was 66 to 75, and the light transmittance was 40 to 45%.
  • the f ⁇ Q value was as low as 74000 to 89000 GHz, and the bending strength was 320 to 345 MPa, which was a sufficient strength as a sputtering target member. There was little abnormal discharge during sputtering, and good film formation was possible.
  • Examples 4 to 7 In Examples 4 to 7, the relative density was as high as 99.5 to 100% by mass. In addition, the volume ratio of the spinel phase in the constituent phases was as low as 16 to 88%. In addition, in Examples 4 and 5, an Al 2 O 3 phase was observed, and in Examples 6 and 7, an MgO phase was observed.
  • the average particle diameter (D50) of the sintered body is 5.2 to 6.5 ⁇ m, which is larger than Examples 1 to 3. This is probably because the sintering temperature was high and the grains grew. D90 / D10 was 2.2 to 3.2.
  • the whiteness is 77 to 82, which is white, and the light transmittance is 27 to 36%, which is lower than those of Examples 1 to 3.
  • the f ⁇ Q value was as low as 88000 to 107000 GHz, and the bending strength was 340 to 385 MPa, which was sufficient for a sputtering target member. There was little abnormal discharge during sputtering, and good film formation was possible.
  • the average particle diameter (D50) of the sintered body was 1.6 ⁇ m, and D90 / D10 was 2.6.
  • the whiteness was 98 and white, the light transmittance was 1%, and the f ⁇ Q value was 48000 GHz.

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WO2019187324A1 (ja) * 2018-03-30 2019-10-03 Jx金属株式会社 MgAl2O4焼結体及び該焼結体を用いたスパッタリングターゲット、並びにMgAl2O4焼結体の製造方法
JPWO2019187324A1 (ja) * 2018-03-30 2020-04-30 Jx金属株式会社 MgAl2O4焼結体及び該焼結体を用いたスパッタリングターゲット、並びにMgAl2O4焼結体の製造方法
JP7110175B2 (ja) 2018-03-30 2022-08-01 Jx金属株式会社 MgAl2O4焼結体及び該焼結体を用いたスパッタリングターゲット、並びにMgAl2O4焼結体の製造方法
US11479509B2 (en) 2018-03-30 2022-10-25 Jx Nippon Mining & Metals Corporation MgAI2O4 sintered body, sputtering target using the sintered body and method of producing MgAI2O4 sintered body

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JPWO2018096992A1 (ja) 2019-10-17
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DE112017005990T5 (de) 2019-08-08
KR20190085948A (ko) 2019-07-19

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