WO2015170534A1 - スパッタリングターゲット材 - Google Patents

スパッタリングターゲット材 Download PDF

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Publication number
WO2015170534A1
WO2015170534A1 PCT/JP2015/060441 JP2015060441W WO2015170534A1 WO 2015170534 A1 WO2015170534 A1 WO 2015170534A1 JP 2015060441 W JP2015060441 W JP 2015060441W WO 2015170534 A1 WO2015170534 A1 WO 2015170534A1
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Prior art keywords
copper
sputtering target
target material
powder
phase
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PCT/JP2015/060441
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English (en)
French (fr)
Japanese (ja)
Inventor
池田　真
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三井金属鉱業株式会社
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Application filed by 三井金属鉱業株式会社 filed Critical 三井金属鉱業株式会社
Priority to CN201580001209.2A priority Critical patent/CN105358734B/zh
Priority to KR1020167001775A priority patent/KR20160017101A/ko
Priority to JP2015533359A priority patent/JP5808513B1/ja
Publication of WO2015170534A1 publication Critical patent/WO2015170534A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • 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

  • the present invention relates to a sputtering target material containing copper or a copper alloy and an oxide, and more particularly to a sputtering target material suitable for forming a blackened layer of a touch panel sensor film employing a copper mesh.
  • a PET film-based transparent electrode film (ITO film: resistance value of about 100 ⁇ / ⁇ ) is used.
  • ITO film resistance value of about 100 ⁇ / ⁇
  • the sensor film for a touch panel using this ITO film is considered difficult to produce a large-area touch panel due to the problem of the resistance value of the ITO film. Therefore, development of a sensor film for a touch panel using a copper mesh capable of realizing a low resistance value is underway.
  • the sensor film for touch panel using this copper mesh is a film formed on a PET film base by a vapor deposition method, and the copper film is processed into a lattice mesh.
  • the sensor film employing the copper mesh can sufficiently cope with a large area touch panel because the resistance value of the copper mesh is about 1 ⁇ / ⁇ .
  • a copper film is formed by vapor deposition on a PET film base, and the brightness of the sensor film called a blackened layer is further formed on the surface of the copper film.
  • a thin film for adjusting the thickness is formed.
  • the surface treatment method is not suitable for thinning the copper mesh.
  • the film formation rate is affected by the supply of oxygen or the like.
  • the discharge has become unstable. Therefore, in the reactive sputtering method, in order to be able to form a blackened layer only with Ar gas, it is also considered to increase the oxygen content of a sputtering target material such as copper, but the oxygen content of the target material Increases, the bulk resistance of the target material itself increases, making it difficult to discharge (sputtering) the DC power supply.
  • JP2013-129183A Japanese Patent No. 3969743 JP 2008-311565 A
  • the present invention has been made in the background as described above, and provides a sputtering target material containing copper or a copper alloy and an oxide, which can be discharged by a DC power source, and statically. It is an object of the present invention to provide a sputtering target material suitable for forming a blackened layer of a capacitive touch panel sensor film.
  • the present invention has a mixed structure of a copper-based metal phase and an oxide phase, an oxygen content of 5 to 30 atom%, a relative density of 85% or more, and a bulk resistance value of 1.0 ⁇ 10 ⁇ 2.
  • the present invention relates to a sputtering target material that is ⁇ cm or less.
  • the sputtering target material of the present invention since the bulk resistance value of the target material itself is low, discharge by an inexpensive DC power source is possible, and the film formation rate can be improved. Further, since the sputtering target material contains a high concentration of oxygen, the amount of oxygen in the sputtering gas can be reduced to perform sputtering, and a stable blackened layer can be formed.
  • the copper-based metal phase in the sputtering target material of the present invention refers to a single phase of copper only or a copper alloy phase. Examples of the copper alloy phase include a copper-nickel alloy phase and a copper-titanium alloy phase.
  • the oxide phase refers to an oxide phase containing only copper (copper oxide phase) or an oxide phase containing a copper alloy as a component (copper alloy oxide phase).
  • the metal component may be the same as or different from the copper alloy phase.
  • examples of such an oxide phase include a copper oxide phase, a copper alloy oxide phase of a copper-nickel alloy, a copper alloy oxide phase of a copper-titanium alloy, and the like.
  • the oxygen content of the sputtering target material according to the present invention is 5 atom% to 30 atom%, preferably 10 atom% to 25 atom%, more preferably 10 atom% to 20 atom%.
  • the oxygen content is less than 5 atomic%, it becomes necessary to introduce a large amount of oxygen into the sputtering gas.
  • the oxygen content exceeds 30 atomic%, it is difficult to discharge with a DC power source.
  • the nickel content is preferably 61.0 atomic% or less, and more preferably 57.0 atomic% or less.
  • the nickel content exceeds 61.0 atomic%, the copper-nickel alloy phase becomes ferromagnetic, leading to a decrease in the film formation rate during sputtering.
  • the titanium content is preferably 7.50 atomic% or less, and more preferably 6.25 atomic% or less. If the titanium content exceeds 7.50 atomic%, a titanium oxide phase is formed, and cracking is likely to occur during sintering.
  • the relative density of the sputtering target material according to the present invention is 85% or more, preferably 90%, more preferably 95% or more. The closer the relative density is to 100%, the better. When the relative density is less than 85%, voids increase in the sputtering target material, and it becomes easy to take in gas components in the atmosphere. Further, abnormal discharge starting from the voids and cracking of the sputtering target material are likely to occur.
  • the sputtering target material according to the present invention has a bulk resistance value of 1.0 ⁇ 10 ⁇ 2 ⁇ cm or less in order to stably discharge by a DC power source. More preferably, it is 1.0 ⁇ 10 ⁇ 3 ⁇ cm or less, and further preferably 5.0 ⁇ 10 ⁇ 4 ⁇ cm or less.
  • the sputtering target material according to the present invention preferably has an average particle size of the copper-based metal phase of 0.5 ⁇ m to 10.0 ⁇ m and an average particle size of the oxide phase of 0.05 ⁇ m to 7.0 ⁇ m. More preferably, the average particle size of the copper-based metal phase is 1.0 ⁇ m to 8.0 ⁇ m, and the average particle size of the oxide phase is 0.5 ⁇ m to 6.0 ⁇ m. In order to make the average particle size of the copper-based metal phase less than 0.5 ⁇ m, it is necessary to reduce the diameter of copper or copper alloy used as a raw material of the sputtering target material, or a metal raw material powder capable of forming an alloy with copper.
  • the oxide powder used as the raw material of the sputtering target material small in diameter, but the oxide powder of the average particle size of too small diameter Since aggregation tends to occur, it becomes difficult to produce a sputtering target material. If the average particle size of the oxide phase exceeds 7.0 ⁇ m, abnormal discharge is likely to occur during sputtering.
  • a sputtering target material having a bulk resistance value of 1.0 ⁇ 10 ⁇ 2 ⁇ cm or less can be stably realized.
  • the area ratio of the copper-based metal phase in the range of 60 ⁇ m ⁇ 60 ⁇ m is preferably 0.32 or more in the cross-sectional observation of the sputtering target material. More preferably, it is 0.44 or more. When the area ratio is less than 0.32, it is difficult to form a network structure of a copper-based metal phase.
  • the oxide phase is preferably a copper oxide phase or a copper alloy oxide phase.
  • the sputtering target material according to the present invention is a mixture of copper powder and / or copper alloy powder or metal powder other than copper for forming copper powder and copper alloy, and oxide powder. It can be produced by sintering at a sintering temperature within a temperature range 450 ° C. to 200 ° C. lower than the melting point of the copper alloy. When the sintering temperature is lower than the melting point of 450 ° C. below the melting point of copper or copper alloy, sintering becomes insufficient, and when the sintering temperature is lower than 200 ° C. lower than the melting point of copper or copper alloy, the melting point of copper or copper alloy is reached. Therefore, it becomes difficult to form a mixed structure of the copper-based metal phase and the oxide phase.
  • the method for producing a sputtering target material according to the present invention only copper powder and oxide powder are mixed, or only copper alloy powder and oxide powder are mixed, and copper powder, copper alloy powder and oxide powder are mixed. It can be manufactured by mixing and further mixing metal powder and oxide powder other than copper for forming copper powder and copper alloy. And the sputtering target material of predetermined oxygen content can be manufactured by adjusting the mixing amount of metal powder other than copper for forming copper powder and / or copper alloy powder or copper alloy, and oxide powder.
  • the copper alloy powder include copper-nickel alloy powder and copper-titanium alloy powder.
  • the oxide powder include copper oxide powder, copper-nickel alloy oxide powder, and copper-titanium alloy oxide powder.
  • metal powder other than copper for forming a copper alloy include nickel powder and titanium powder.
  • a powder metallurgy method using copper powder and / or copper alloy powder and oxide powder as raw materials can be applied.
  • the powder metallurgy method a method of firing a molded body after uniaxial pressing, a hot press method, an electric current sintering method, and the like can be applied, and an electric current sintering method is particularly preferable.
  • the electric current sintering method current flows preferentially to the conductive part in the mixed raw material powder and the sintering proceeds, that is, the copper powder or copper alloy powder part, or both parts Current flows preferentially, and the copper particles or copper alloy particles forming the copper-based metal phase preferentially grow easily.
  • the connection of the copper particles or copper alloy particles forming the copper-based metal phase is ensured, and the bulk resistance value of the sputtering target material itself Can be reliably reduced.
  • a sputtering target material having copper or a copper alloy and an oxide that can be discharged by a direct current power source can be realized, and a blackening layer for forming a capacitive touch panel sensor film, It can be formed stably and easily.
  • sputtering target materials (Examples 1 to 3) having respective oxygen contents were prepared.
  • Comparative Examples 1 to 3 were also produced.
  • Table 1 shows data of each sputtering target material. Below, the manufacturing conditions of each sputtering target material are demonstrated.
  • the oxygen content was weighed so as to be 20 atomic%.
  • Weighed raw material powder and zirconia grinding media were put into a pot and mixed for 3 hours in a ball mill. Thereafter, the mixed powder was sieved and filled into a graphite mold having a diameter of 174 mm.
  • the graphite mold filled with the mixed powder was set in an electric current sintering apparatus (DR.
  • Example 2 The raw material powder was weighed so that the oxygen content was 15 atomic%. The other production conditions were the same as in Example 1.
  • Example 3 The raw material powder was weighed so that the oxygen content was 10 atomic%. The other production conditions were the same as in Example 1.
  • the other production conditions were the same as in Example 1.
  • Comparative Example 1 The same procedure as in Example 1 was performed until mixing by a ball mill, and a compact having a diameter of 140 mm was produced by uniaxial pressure molding (press pressure: 500 kgf / cm 2 ). And it baked on the following conditions using the baking furnace.
  • Comparative example 2 It was made to be the same as that of the comparative example 1 except having made the baking atmosphere into vacuum (pressure: 40 Pa).
  • Oxygen content The surface of the sintered body was shaved by machining, and the oxygen content was measured from the obtained chips using an oxygen nitrogen analyzer (EMGA-550 / manufactured by Horiba, Ltd.).
  • Relative density The weight (g) of the sputtering target material is divided by its volume (cm 3 ), and the percentage of the theoretical density ⁇ (g / cm 3 ) based on the following theoretical formula (Equation 1) is calculated. %).
  • C (Cu) and C (Cu 2 O) indicate the contents (% by weight) of the copper-based metal phase and the oxide phase in the sputtering target material, respectively, and ⁇ (Cu) and ⁇ (Cu 2 O) indicates the density of copper or copper alloy and the density of oxide, respectively.
  • the content (% by weight) of the copper-based metal phase and the oxide phase was calculated on the assumption that all the oxygen in the measured sintered body forms copper oxide (I) or a copper alloy oxide. .
  • the volume resistance value of the processed sputtering target material was measured using a low resistivity meter (Loresta-HP / Mitsubishi Chemical Analytech Co., Ltd.) and a four-point probe.
  • Average particle diameter The surface of the sputtering target material was polished and smoothed. About this smooth surface, an FE gun type scanning electron microscope (SUPRA55VP / Carl) equipped with an energy dispersive X-ray analysis (EDS) / electron beam backscatter diffraction analysis (EBSD) apparatus (Pegasus System / Ametech Co., Ltd.). EDS spectra and EBSD patterns of copper, nickel and oxygen were measured by Zeiss. The measurement conditions were an acceleration voltage of 20 kV, an observation visual field of 60 ⁇ 60 ⁇ m, and a measurement interval of 0.5 ⁇ m.
  • EDS energy dispersive X-ray analysis
  • EBSD electron beam backscatter diffraction analysis
  • the indexed crystal phases were a copper-based metal phase (copper phase or copper alloy phase) and an oxide phase, and both were distinguished from the EDS spectrum.
  • the analysis menu “Grain Size” of the EBSD analysis program OIM Analysis / manufactured by TSL Solutions
  • the area-weighted average crystal grain size of each of the copper-based metal phase and the oxide phase was calculated.
  • the grain boundary is identified as a general grain boundary.
  • a twin grain boundary having an orientation relationship of 60 ° rotation around the ⁇ 111> axis is regarded as a general grain boundary. I went there.
  • the area ratio of the copper-based metal phase was calculated as follows.
  • Examples 4 and 5 containing nickel the oxygen content of the produced sputtering target material was almost at the target level. However, compared with Examples 1 to 3, the oxygen content in the raw material powder was slightly lower. This is considered because the nickel oxide phase formed by reaction of nickel powder and copper (II) oxide powder has oxygen deficiency. On the other hand, relative density was 85% or more in Examples 4 and 5.
  • the bulk resistance value was in the range of 1.0 ⁇ 10 ⁇ 2 ⁇ cm or less, and it was found that discharge by a DC power source was possible.
  • Comparative Examples 1 and 3 were insulators, and measurement of the bulk resistance value was impossible. Also in Comparative Example 2, the resistance value could not be specified because the bulk resistance value was very large and the measured value was unstable. Further, although Comparative Example 2 has a certain conductivity, it was difficult to stably discharge with a DC power source.
  • FIG. 1 shows the result of observing the cross section of the sputtering target material of Example 1 with an electron beam backscatter diffraction analyzer (EBSD device).
  • the portion that appears black in FIG. 1 is the copper phase, and the other portion is the oxide phase. Since the copper phase is in a state of being connected in a network, it is considered that a conductive path is formed inside the material. Therefore, in the case of the example, it is considered that the bulk resistance value is lowered.
  • the area ratio of the copper phase in the field of view (60 ⁇ m ⁇ 60 ⁇ m) in FIG. 1 was calculated to be 0.48.
  • the oxygen content is large, it is considered that the entire target material is composed of an oxide phase and becomes an insulator.
  • the comparative example 2 it was a state with low crystallinity, and it was a structure state in which the distinction with a copper phase and an oxide phase was unclear. Therefore, it is considered that the bulk resistance value is very high.
  • tissue which can hardly confirm a copper alloy phase, Therefore It is thought that it was in the state close
  • Example 4 the result of having observed the cross section of the sputtering target material of Example 4 in FIG. 2 is shown.
  • the portion that appears black in FIG. 2 is an alloy phase (copper metal phase) of copper and nickel, and the other portion is an oxide phase.
  • This oxide phase was found to contain a nickel oxide phase from the results of the EDS spectrum and the EBSD pattern. It was found that part of the nickel powder as a raw material formed a copper-based metal phase and the other part formed a copper alloy oxide phase.
  • the copper-type metal phase in Example 4 was the state connected in network form. In addition, it was 0.70 when the area ratio of the copper-type metal phase in the visual field (60 micrometers x 60 micrometers) of FIG. 2 was computed.
  • the evaluation of the blackened layer was performed by forming an evaluation sample in which a copper wiring layer made of copper was formed on a glass substrate and the blackened layer was formed on the surface of the copper layer.
  • the film thickness of the blackened layer is not particularly limited, but can be, for example, 5 nm to 100 nm.
  • Sputtering can be performed only with argon gas, but oxygen and / or nitrogen can be added as a sputtering gas for the purpose of adjusting the optical characteristics of the blackening layer to be formed.
  • the ratio of the added gas flow rate to the argon gas flow rate is preferably 20% or less, more preferably 15% or less. If too much oxygen and / or nitrogen is added, the film formation rate tends to decrease and the discharge becomes unstable.
  • a copper layer using pure copper is formed.
  • pure copper is used for the requirement of low resistance, and adhesion to the substrate.
  • a copper alloy can also be used.
  • an adhesion layer such as titanium or molybdenum can be formed on the base of the copper wiring.
  • the film thickness of the copper wiring is not particularly limited, but can be, for example, 50 nm to 10,000 nm.
  • the production conditions of the evaluation sample are as follows. First, each produced sputtering target material was bonded to a copper backing plate to obtain a sputtering target. The sputtering target and the pure copper sputtering target for wiring were mounted on a sputtering apparatus equipped with a DC power source to form a film.
  • the film forming conditions are as follows. ⁇ Film formation conditions> ⁇ Laminated film configuration: blackened layer / copper wiring film / glass substrate.
  • Blackened layer thickness 20 nm -Copper wiring layer thickness: 200nm ⁇ Glass substrate: 40mm x 40mm x 0.7mmt ⁇ Achieved pressure: less than 5 ⁇ 10 ⁇ 6 Torr ⁇
  • the value of the lightness L * targeted for suppressing the decrease in contrast of the display device was in the range of 40 or less. Further, it has been found that as the oxygen content in the sputtering target material increases, the value of the lightness L * decreases even with a small oxygen flow rate. On the other hand, in the case of Comparative Example 4, although the blackening layer was formed with the maximum oxygen flow rate of 10 sccm, the brightness L * could not be reduced to 40 or less.
  • the present invention it becomes possible to perform a sputtering process for discharging with a direct current power source, and to efficiently manufacture a sensor film for a touch panel provided with a blackened layer without reducing the contrast of the display device.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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PCT/JP2015/060441 2014-05-08 2015-04-02 スパッタリングターゲット材 WO2015170534A1 (ja)

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CN201580001209.2A CN105358734B (zh) 2014-05-08 2015-04-02 溅镀靶材
KR1020167001775A KR20160017101A (ko) 2014-05-08 2015-04-02 스퍼터링 타깃재
JP2015533359A JP5808513B1 (ja) 2014-05-08 2015-04-02 スパッタリングターゲット材

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017164168A1 (ja) * 2016-03-22 2017-09-28 三菱マテリアル株式会社 スパッタリングターゲット
JP2018051784A (ja) * 2016-09-26 2018-04-05 住友金属鉱山株式会社 積層体基板、導電性基板、積層体基板の製造方法、導電性基板の製造方法
WO2018159753A1 (ja) * 2017-03-01 2018-09-07 三菱マテリアル株式会社 スパッタリングターゲット及びスパッタリングターゲットの製造方法
JP2018145523A (ja) * 2017-03-01 2018-09-20 三菱マテリアル株式会社 スパッタリングターゲット及びスパッタリングターゲットの製造方法
WO2019167564A1 (ja) * 2018-03-01 2019-09-06 三菱マテリアル株式会社 Ｃｕ－Ｎｉ合金スパッタリングターゲット
JP2019151916A (ja) * 2018-03-01 2019-09-12 三菱マテリアル株式会社 Ｃｕ−Ｎｉ合金スパッタリングターゲット
CN113365763A (zh) * 2019-03-11 2021-09-07 三菱综合材料株式会社 含金属铜-氧化铜的粉末、含金属铜-氧化铜的粉末的制造方法及溅射靶材、溅射靶材的制造方法

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JP6876268B2 (ja) * 2016-03-22 2021-05-26 三菱マテリアル株式会社 スパッタリングターゲット
JP6533805B2 (ja) * 2017-03-31 2019-06-19 Ｊｘ金属株式会社 スパッタリングターゲット、スパッタリングターゲットの製造方法、非晶質膜、非晶質膜の製造方法、結晶質膜及び結晶質膜の製造方法

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JP2001295034A (ja) * 2000-04-10 2001-10-26 Nikko Materials Co Ltd 光ディスク保護膜形成用スパッタリングターゲット
JP2010077530A (ja) * 2008-08-26 2010-04-08 Hitachi Metals Ltd スパッタリングターゲットの製造方法及びスパタリングターゲット
JP2011084754A (ja) * 2009-10-13 2011-04-28 Hitachi Metals Ltd スパッタリングターゲットの製造方法
JP2011174167A (ja) * 2010-02-01 2011-09-08 Ryukoku Univ 酸化物膜及びその製造方法、並びにターゲット及び酸化物焼結体の製造方法

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017164168A1 (ja) * 2016-03-22 2017-09-28 三菱マテリアル株式会社 スパッタリングターゲット
JP2018051784A (ja) * 2016-09-26 2018-04-05 住友金属鉱山株式会社 積層体基板、導電性基板、積層体基板の製造方法、導電性基板の製造方法
WO2018159753A1 (ja) * 2017-03-01 2018-09-07 三菱マテリアル株式会社 スパッタリングターゲット及びスパッタリングターゲットの製造方法
JP2018145523A (ja) * 2017-03-01 2018-09-20 三菱マテリアル株式会社 スパッタリングターゲット及びスパッタリングターゲットの製造方法
WO2019167564A1 (ja) * 2018-03-01 2019-09-06 三菱マテリアル株式会社 Ｃｕ－Ｎｉ合金スパッタリングターゲット
JP2019151916A (ja) * 2018-03-01 2019-09-12 三菱マテリアル株式会社 Ｃｕ−Ｎｉ合金スパッタリングターゲット
CN113365763A (zh) * 2019-03-11 2021-09-07 三菱综合材料株式会社 含金属铜-氧化铜的粉末、含金属铜-氧化铜的粉末的制造方法及溅射靶材、溅射靶材的制造方法

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TW201542849A (zh) 2015-11-16
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CN105358734B (zh) 2017-03-29
JP5808513B1 (ja) 2015-11-10
JPWO2015170534A1 (ja) 2017-04-20
KR20160017101A (ko) 2016-02-15

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