WO2019097959A1 - 酸化物焼結体およびスパッタリングターゲット - Google Patents

酸化物焼結体およびスパッタリングターゲット Download PDF

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Publication number
WO2019097959A1
WO2019097959A1 PCT/JP2018/039241 JP2018039241W WO2019097959A1 WO 2019097959 A1 WO2019097959 A1 WO 2019097959A1 JP 2018039241 W JP2018039241 W JP 2018039241W WO 2019097959 A1 WO2019097959 A1 WO 2019097959A1
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oxide
sintered body
sno
oxide sintered
mol
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PCT/JP2018/039241
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English (en)
French (fr)
Japanese (ja)
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俊亮 竹谷
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三井金属鉱業株式会社
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
    • C04B35/457—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates based on tin oxides or stannates
    • 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

Definitions

  • Embodiments of the disclosure relate to an oxide sintered body and a sputtering target.
  • GTO Gallium Tin Oxide
  • tin oxide SnO 2
  • gallium oxide Ga 2 O 3
  • One aspect of the embodiment is made in view of the above, and it is an object of the present invention to provide an oxide sintered body for a GTO sputtering target that can perform DC sputtering even if the concentration of gallium oxide is higher than 20 mol%. I assume.
  • the oxide sintered body according to one aspect of the embodiment is an oxide sintered body containing tin oxide and gallium oxide, and the content of gallium oxide is 20 mol% ⁇ Ga 2 O 3 ⁇ 90 mol%.
  • the specific resistance is 1 ⁇ 10 3 ⁇ ⁇ cm or less.
  • an oxide sintered body for a GTO sputtering target which can perform DC sputtering even when the concentration of gallium oxide is higher than 20 mol%.
  • FIG. 1 is a SEM observation photograph of the oxide sintered body in Example 4.
  • FIG. 2 is a schematic diagram showing the measurement location of the bulk resistance of oxide sinter.
  • FIG. 3 is an X-ray diffraction chart of the oxide sintered body in Examples 4 to 8.
  • FIG. 4 is an X-ray diffraction chart of the oxide sintered body in Comparative Example 1.
  • Oxide sinter 1 of an embodiment contains tin oxide and gallium oxide, and can be used as a sputtering target.
  • Oxide sinter 1 of an embodiment consists of tin oxide, gallium oxide, and an unavoidable impurity, for example, and can be used as a GTO target.
  • the GTO target of the embodiment is allowed to contain a small amount of other elements as long as the advantageous effects of the embodiment are not impaired.
  • the content of gallium oxide is 20 mol% ⁇ Ga 2 O 3 ⁇ 90 mol%, and the specific resistance is 1 ⁇ 10 3 ⁇ ⁇ cm or less.
  • the oxide sinter 1 of the embodiment preferably has a gallium oxide content of more than 20 mol% (typically 20.5 mol% or more) and 90 mol% or less.
  • the content of gallium oxide is 90 mol% or less, the contribution of Ga 2 O 3 having a large specific resistance is smaller than that of SnO 2 , which is preferable because the specific resistance of the sputtering target is low.
  • the content of gallium oxide is preferably 85 mol% or less, more preferably 75 mol% or less, still more preferably 65 mol% or less, and still more preferably 50 mol% or less.
  • the content of gallium oxide is preferably 45 mol% or less, more preferably 40 mol% or less.
  • the oxide sintered body 1 of the embodiment has a specific resistance of 1 ⁇ 10 3 ⁇ ⁇ cm or less. Therefore, when this oxide sinter 1 is used as a sputtering target, sputtering using an inexpensive DC power supply becomes possible, and the film forming rate can be improved.
  • the oxide sintered body 1 of the embodiment preferably has a specific resistance of 5 ⁇ 10 2 ⁇ ⁇ cm or less, and more preferably 1 ⁇ 10 2 ⁇ ⁇ cm or less.
  • a gallium stannate compound (Ga 4 SnO 8 ) is not generated as much as possible. Although the specific resistance becomes reason is not clear low by stannate gallium compound (Ga 4 SnO 8) is not generated, the resistivity of stannate gallium compound (Ga 4 SnO 8) is considered or not for high.
  • the oxide sintered body 1 of the embodiment is the (111) of the gallium stannate compound (Ga 4 SnO 8 ) phase with respect to the peak of the (110) plane of the tin oxide (SnO 2 ) phase in the X-ray diffraction measurement.
  • the peak intensity ratio I of the surface is preferably 0.15 or less. That is, in the oxide sintered body 1 of the embodiment, the ratio of the gallium stannate compound (Ga 4 SnO 8 ) phase to the tin oxide (SnO 2 ) phase is a predetermined ratio defined by the above peak intensity ratio I. It is preferable to be small.
  • oxide sinter 1 with a small specific resistance can be formed. Therefore, according to the embodiment, DC sputtering is facilitated when the oxide sintered body 1 is used as a sputtering target.
  • the above-mentioned peak intensity ratio I is preferably 0.10 or less, more preferably 0.05 or less, and still more preferably 0.03 or less. Preferably, it is more preferably 0.01 or less.
  • the oxide sintered body 1 of the embodiment preferably has a relative density of 90% or more. Thereby, when this oxide sinter 1 is used as a sputtering target, the discharge state of DC sputtering can be stabilized. From this viewpoint, the oxide sintered body 1 of the embodiment more preferably has a relative density of 95% or more.
  • the oxide sintered body 1 When the oxide sintered body 1 is used as a sputtering target, if the relative density is 90% or more, voids can be reduced in the sputtering target, and it is easy to prevent uptake of gas components in the atmosphere. In addition, abnormal discharge starting from the gap, cracking of the sputtering target, and the like are less likely to occur.
  • the oxide sintered body 1 of the embodiment can be manufactured, for example, by the following method.
  • the raw material powders are Ga 2 O 3 powder and SnO 2 powder.
  • the average particle size of each raw material powder is preferably 2 ⁇ m or less. If the average particle diameter of each raw material powder is 2 ⁇ m or less, a high density sintered body can be easily obtained even if the sintering temperature is lowered. From such a viewpoint, the average particle diameter of each raw material powder is more preferably 1.5 ⁇ m or less, and still more preferably 1 ⁇ m or less.
  • the lower limit value of the average particle diameter of each raw material powder is not particularly limited, but is preferably 0.1 ⁇ m or more from the viewpoint of preventing aggregation of the raw material.
  • the average particle size of the raw material powder is the volume cumulative particle diameter D 50 in the cumulative volume 50% by volume by laser diffraction scattering particle size distribution measuring method.
  • Various mixing means can be used for mixing of raw material powder.
  • media stirring type mills such as bead mills, sand mills, attritors (registered trademark) and ball mills can be used.
  • the obtained mixed powder may be sieved.
  • the oxide sintered body 1 of the embodiment is preferably sintered by a spark plasma sintering (SPS) method or a hot press (HP) method.
  • SPS spark plasma sintering
  • HP hot press
  • the mixed powder is filled in a sintering die having a shaped concave portion of a predetermined shape.
  • a sintering die for example, one made of graphite can be used.
  • the oxide sintered body 1 of the embodiment is preferably sintered at a relatively low temperature of 1200 ° C. or less. By sintering at a low temperature of 1200 ° C. or less, the formation of a gallium stannate compound (Ga 4 SnO 8 ) can be suppressed, and the specific resistance of the oxide sintered body 1 can be lowered.
  • a gallium stannate compound Ga 4 SnO 8
  • the sintering temperature of the embodiment is preferably 1100 ° C. or less, more preferably 1000 ° C. or less, and still more preferably 950 ° C. or less.
  • the lower limit value of the firing temperature is preferably 500 ° C. or more from the viewpoint of sufficient sintering.
  • the mixed powder was sieved with a sieve having an opening of 710 ⁇ m to obtain a mixed powder having an average particle size (volume cumulative particle size D 50 ) of 0.8 ⁇ m.
  • the sieved mixed powder was filled into a graphite sintering die with an inner diameter of 120 mm.
  • the sintered die filled with the mixed powder was sintered by a spark plasma sintering (SPS) apparatus to produce a sintered body.
  • Sintering with this SPS device is performed under vacuum (15 Pa or less), pressure 20 MPa, sintering temperature 600 ° C., temperature rising rate 20 ° C./min, holding time at sintering temperature 30 min, temperature lowering is natural furnace cooling.
  • the obtained sintered body was cut to obtain an oxide sintered body 1 having a diameter of 101.6 mm and a thickness of 6 mm.
  • the ratio (mol%) of each oxide contained in the mixed powder of SnO 2 powder and Ga 2 O 3 powder is the oxide sintered body 1 finally obtained. It can be regarded as the ratio (mol%) of each oxide contained in.
  • the mixed powder was sieved with a sieve having an opening of 710 ⁇ m to obtain a mixed powder having an average particle size (volume cumulative particle size D 50 ) of 0.8 ⁇ m.
  • the sieved mixed powder was filled into a graphite sintering die with an inner diameter of 120 mm.
  • the sintered die filled with the mixed powder was sintered by a hot press (HP) device to produce a sintered body.
  • Sintering with this HP apparatus was carried out in an argon atmosphere at a pressure of 17 MPa, a sintering temperature of 920 ° C., a temperature rising rate of 60 ° C./min, a holding time of 180 minutes at the sintering temperature, and a temperature lowering by natural furnace cooling.
  • the obtained sintered body was cut to obtain an oxide sintered body 1 having a diameter of 101.6 mm and a thickness of 6 mm.
  • Ga 2 O 3 powder having an average particle diameter (volume cumulative particle diameter D 50) is 1 [mu] m, an average particle diameter (volume cumulative particle diameter D 50) is a SnO 2 powder is 0.5 ⁇ m, Ga 2 O 3: SnO 2 30.0: were weighed so as to 70.0 (mol%). Next, it mixed using a ball mill for 24 hours, and obtained mixed powder.
  • the mixed powder was sieved with a sieve having an opening of 710 ⁇ m to obtain a mixed powder having an average particle size (volume cumulative particle size D 50 ) of 0.8 ⁇ m.
  • the obtained mixed powder 6% by mass of polyvinyl alcohol diluted to 4% by mass was added with respect to the mixed powder, and the polyvinyl alcohol was made to conform well to the powder using a mortar. Then, the obtained powder was temporarily pressed under the condition of 200 kg / cm 2 , and the obtained temporary formed body was crushed in a mortar to obtain a crushed powder. Next, the obtained pulverized powder was filled in a press die, and molded for 60 seconds under a press pressure of 1 t / cm 2 to obtain a molded body.
  • the obtained compact is put into a sintering furnace, oxygen is allowed to flow in the furnace at 1 L / h, and the sintering atmosphere is made an oxygen flow atmosphere, and the temperature rising rate is 5.83 ° C./min (350 ° C./min. h)
  • the sintering temperature was 1500 ° C.
  • the holding time at the sintering temperature was set to 540 minutes (9 h).
  • the obtained sintered body was cooled at a temperature lowering rate of 100 ° C./h.
  • the cooled sintered body was cut to obtain an oxide sintered body 1 having a diameter of 101.6 mm and a thickness of 6 mm.
  • the air mass of the oxide sintered body 1 is divided by the volume (mass of the sintered body in water / specific gravity of water at the measurement temperature), and the percentage value relative to the theoretical density ⁇ (g / cm 3 ) is a relative density (Unit:%).
  • C 1 and C 2 and ⁇ ⁇ ⁇ 1 and ⁇ 2 in the above formula indicate the following values, respectively.
  • C 1 :% by mass of SnO 2 powder used for the production of oxide sintered body 1 ⁇ ⁇ 1 density of SnO 2 (6.95 g / cm 3 )
  • C 2 :% by mass of Ga 2 O 3 powder used in the production of oxide sintered body 1 ⁇ ⁇ 2 density of Ga 2 O 3 (5.95 g / cm 3 )
  • FIG. 1 is a SEM observation photograph of the oxide sintered body 1 in Example 4.
  • a dark gallium oxide (Ga 2 O 3 ) phase is dispersed in a light tin oxide (SnO 2 ) phase.
  • a gallium stannate compound (Ga 4 SnO 8 ) phase which is a compound of tin oxide and gallium oxide, was not observed in the oxide sintered bodies 1 of Examples 1 to 8.
  • the concentration of Zr impurities contained in each of the oxide sintered bodies 1 of Examples 1 to 8 and Comparative Examples 1 and 2 obtained above was measured. Specifically, it was measured by an acid decomposition ICP-OES method using ICP emission spectrometer 720 ICP-OES manufactured by Agilent Technologies. As a result, in all the oxide sintered bodies 1, the Zr concentration was less than 50 ppm.
  • FIG. 2 is a schematic view showing measurement points of bulk resistance of the oxide sintered body 1.
  • the specific resistance was 1 ⁇ 10 3 ⁇ ⁇ cm or less, and it was possible to measure the specific resistance
  • Comparative Example 1 was an insulator (That is, the specific resistance was larger than 1 ⁇ 10 7 ⁇ ⁇ cm), and the measurement of the specific resistance (bulk resistance) could not be performed.
  • Comparative Example 2 has a specific resistance of 2.4 ⁇ 10 3 ⁇ ⁇ cm, which is higher than those of Examples 1 to 8. It is considered that this is because the proportion of tin oxide which is considered to be responsible for conductivity decreases and it becomes difficult to form a conductive path in the target.
  • sputtering targets of Examples 1 to 8 and Comparative Examples 1 and 2 were produced from the oxide sintered bodies 1 of Examples 1 to 8 and Comparative Examples 1 and 2 obtained above.
  • the sputtering target was manufactured by using indium as a low melting point solder as a bonding material, and bonding the oxide sintered body 1 obtained above to a copper base.
  • Film forming apparatus DC magnetron sputtering apparatus
  • Exhaust system cryopump
  • rotary pump Sputtering power 150 W (1.85 W / cm 2 )
  • the ultimate pressure 1.0 ⁇ 10-4 Pa
  • Sputtering pressure 0.4 Pa -Oxygen partial pressure: O 2 2.0%
  • the content of gallium oxide 90 mol% or less By making the content of gallium oxide 90 mol% or less according to the comparison between Examples 1 to 8 in which the content of gallium oxide is 90 mol% or less and the comparative example 2 in which the content of gallium oxide is 95 mol% or more.
  • the specific resistance can be reduced to 1 ⁇ 10 3 ⁇ ⁇ cm or less.
  • Examples 1-8 specific resistance 1 ⁇ 10 3 ⁇ ⁇ cm or less by comparison with Comparative Examples 1 and 2 the resistivity is 1 ⁇ 10 3 ⁇ ⁇ cm or more, the resistivity 1 ⁇ It is understood that a sputtering target capable of DC sputtering can be realized by reducing it to 10 3 ⁇ ⁇ cm or less.
  • the discharge state of DC sputtering can be stabilized. Furthermore, by making the relative density 95% or more, the discharge state of DC sputtering is made by comparing the examples 4 to 8 having a relative density of less than 95% and the examples 1 to 3 having a relative density of 95% or more. It turns out that it is stabilized further.
  • X-Ray Diffraction (XRD) measurement is performed on each of the oxide sintered bodies 1 of Examples 1 to 8 and Comparative Examples 1 and 2 obtained above, and X-ray diffraction charts Obtained. Then, the structures of oxide sintered bodies 1 of Examples 1 to 8 and Comparative Examples 1 and 2 were identified from the obtained X-ray diffraction chart.
  • XRD X-Ray Diffraction
  • FIG. 3 is an X-ray diffraction chart of the oxide sintered body 1 in Examples 4 to 8.
  • FIG. 3 also shows the positions of peaks appearing due to various planes present in each oxide in the X-ray diffraction chart.
  • the peak of the (110) plane of tin oxide (SnO 2) phase is the main peak of the tin oxide (SnO 2) phases, the diffraction angle (2 [Theta]) appears to 26.58 ° It is a peak.
  • the peak of the (111) plane of stannate gallium compound (Ga 4 SnO 8) phase is the main peak of stannate gallium compound (Ga 4 SnO 8) phase, diffraction angle (2 [Theta]) is the 34.81 ° It is a peak that appears.
  • the peak intensity ratio I in Example 4 is 0.03, the peak intensity ratio I in Example 5 is 0.03, and the peak intensity ratio I in Example 6 is 0.04.
  • the peak intensity ratio I in Example 7 was 0.09, and the peak intensity ratio I in Example 8 was 0.13.
  • the peak intensity ratio I in Example 1 is 0.01
  • the peak intensity ratio I in Example 2 is 0.01
  • the peak intensity in Example 3 The ratio I was 0.01.
  • FIG. 4 is an X-ray diffraction chart of the oxide sintered body 1 in Comparative Example 1. As in FIG. 3, FIG. 4 also shows the positions of peaks appearing in the X-ray diffraction chart due to various planes present in each oxide.
  • Example 1 sintered at a relatively low temperature of 1200 ° C. or lower using the SPS method or the HP method, and Comparative Example 1 sintered at a temperature higher than 1200 ° C.
  • the peak intensity ratio I can be reduced to 0.05 or less by bonding. That is, in the embodiment, the formation of the gallium stannate compound (Ga 4 SnO 8 ) phase can be suppressed by sintering at a relatively low temperature.
  • the gallium stannate compound (Ga 4 SnO 8 ) phase has a high ratio It is considered to have resistance. That is, according to the embodiment, the specific resistance can be reduced to 1 ⁇ 10 3 ( ⁇ ⁇ cm) or less by suppressing the formation of the gallium stannate compound (Ga 4 SnO 8 ) phase by low temperature sintering. .
  • the SPS method and the HP method are used is described as a method capable of performing sintering at a relatively low temperature of 1200 ° C. or less.
  • the low temperature sintering method includes the SPS method and the HP method It is not limited to.
  • the shape of the oxide sintered body 1 is not limited to the disc shape, and may be cylindrical or the like. It may have any shape.

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  • Ceramic Engineering (AREA)
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PCT/JP2018/039241 2017-11-15 2018-10-22 酸化物焼結体およびスパッタリングターゲット WO2019097959A1 (ja)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000077358A (ja) * 1998-08-27 2000-03-14 Asahi Glass Co Ltd 透明導電膜、スパッタリングターゲットおよび透明導電膜付き基体
JP2015166305A (ja) * 2014-02-14 2015-09-24 株式会社コベルコ科研 酸化物焼結体およびスパッタリングターゲット
JP2016098396A (ja) * 2014-11-20 2016-05-30 Tdk株式会社 スパッタリングターゲット、透明導電性酸化物薄膜、及び導電性フィルム

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPWO2010018707A1 (ja) * 2008-08-11 2012-01-26 出光興産株式会社 酸化ガリウム−酸化スズ系酸化物焼結体及び酸化物膜

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000077358A (ja) * 1998-08-27 2000-03-14 Asahi Glass Co Ltd 透明導電膜、スパッタリングターゲットおよび透明導電膜付き基体
JP2015166305A (ja) * 2014-02-14 2015-09-24 株式会社コベルコ科研 酸化物焼結体およびスパッタリングターゲット
JP2016098396A (ja) * 2014-11-20 2016-05-30 Tdk株式会社 スパッタリングターゲット、透明導電性酸化物薄膜、及び導電性フィルム

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