TWI768149B - Oxide sintered body, sputtering target and transparent conductive film - Google Patents
Oxide sintered body, sputtering target and transparent conductive film Download PDFInfo
- Publication number
- TWI768149B TWI768149B TW107139172A TW107139172A TWI768149B TW I768149 B TWI768149 B TW I768149B TW 107139172 A TW107139172 A TW 107139172A TW 107139172 A TW107139172 A TW 107139172A TW I768149 B TWI768149 B TW I768149B
- Authority
- TW
- Taiwan
- Prior art keywords
- mass
- sintered body
- terms
- oxide sintered
- transparent conductive
- Prior art date
Links
- 238000005477 sputtering target Methods 0.000 title claims description 25
- 239000010955 niobium Substances 0.000 claims abstract description 41
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 38
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 38
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000011135 tin Substances 0.000 claims abstract description 34
- 229910052718 tin Inorganic materials 0.000 claims abstract description 34
- 229910052738 indium Inorganic materials 0.000 claims abstract description 33
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 33
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 26
- 238000002834 transmittance Methods 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000013077 target material Substances 0.000 claims 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 abstract 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 abstract 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 abstract 1
- 239000010408 film Substances 0.000 description 50
- 239000000843 powder Substances 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 16
- 239000002994 raw material Substances 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 11
- 238000005259 measurement Methods 0.000 description 11
- 238000004544 sputter deposition Methods 0.000 description 11
- 239000002245 particle Substances 0.000 description 10
- 239000011812 mixed powder Substances 0.000 description 9
- 239000000758 substrate Substances 0.000 description 8
- 238000005520 cutting process Methods 0.000 description 6
- 238000010304 firing Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 4
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000009694 cold isostatic pressing Methods 0.000 description 3
- 239000000306 component Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 238000010248 power generation Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005401 electroluminescence Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000001392 ultraviolet--visible--near infrared spectroscopy Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Structural Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Physical Vapour Deposition (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Laminated Bodies (AREA)
- Manufacturing Of Electric Cables (AREA)
Abstract
Description
本發明所揭示之實施形態係關於氧化物燒結體、濺鍍膜及透明導電膜。 Embodiments disclosed in the present invention relate to an oxide sintered body, a sputtered film, and a transparent conductive film.
以往,已知一種透明導電膜的濺鍍靶,係於ITO(Indium Tin Oxide,氧化銦錫)添加鈮等,且用以使在紫色區域(例如,波長400nm)之穿透率得到改善之透明導電膜成膜者(例如,參照專利文獻1)。
Conventionally, a sputtering target for a transparent conductive film has been known, which is a transparent target for improving the transmittance in the purple region (for example,
專利文獻1:國際公開第2011/052375號公報 Patent Document 1: International Publication No. 2011/052375
然而,藉由以往之濺鍍靶所成膜之透明導電膜,於紫外光區域(例如,波長300nm)或紫色區域(例如,波長400nm)等短波長區域下的穿透率仍有改善的空間。
However, there is still room for improvement in the transmittance of transparent conductive films formed by conventional sputtering targets in short wavelength regions such as ultraviolet light region (eg,
本實施形態之一樣態,係有鑑於上述情事 所研創者,其目的在於提供一種氧化物燒結體,其係在使用濺鍍靶所成膜之透明導電膜中,可提升紫外光區域或紫色區域等短波長區域的穿透率。 A state of the present embodiment is based on the above-mentioned circumstances The purpose of the inventors is to provide an oxide sintered body, which can improve the transmittance of short wavelength regions such as ultraviolet light region and violet region in a transparent conductive film formed by using a sputtering target.
本實施形態之一樣態的氧化物燒結體,係含有銦、鈮、錫及氧,且以In2O3換算的話含有90.0質量%以上之前述銦,以Nb2O5換算的話含有3.5至6.5質量%之前述鈮,以SnO2換算的話含有0.5至2質量%之前述錫。 The oxide sintered body in one form of the present embodiment contains indium, niobium, tin and oxygen, and contains 90.0 mass % or more of the aforementioned indium in terms of In 2 O 3 and 3.5 to 6.5 in Nb 2 O 5 conversion. The aforementioned niobium in mass % contains 0.5 to 2 mass % of the aforementioned tin in terms of SnO 2 .
藉由本實施形態之一樣態,可提升所成膜之透明導電膜之紫外光區域或紫色區域等短波長區域的穿透率。 According to the state of the present embodiment, the transmittance of the formed transparent conductive film in the short wavelength region such as the ultraviolet light region and the purple region can be improved.
第1圖係顯示實施例2及比較例1、4之透明導電膜之熱處理前之穿透率的波長相依性之圖表。 FIG. 1 is a graph showing the wavelength dependence of transmittance before heat treatment of the transparent conductive films of Example 2 and Comparative Examples 1 and 4. FIG.
第2圖係顯示實施例2及比較例1、4之透明導電膜之熱處理後之穿透率的波長相依性之圖表。 FIG. 2 is a graph showing the wavelength dependence of the transmittance of the transparent conductive films of Example 2 and Comparative Examples 1 and 4 after heat treatment.
以下,參照添附圖式,說明本發明所揭示之氧化物燒結體、濺鍍靶及透明導電膜的實施形態。又,本發明並不受限於以下所示之實施形態。 Hereinafter, embodiments of the oxide sintered body, the sputtering target, and the transparent conductive film disclosed in the present invention will be described with reference to the accompanying drawings. In addition, this invention is not limited to embodiment shown below.
實施形態之氧化物燒結體係含有銦(In)、鈮(Nb)、錫(Sn)及氧(O),可作為濺鍍靶使用。而實施形態之 氧化物燒結體,以In2O3換算的話含有90.0質量%以上之銦,以Nb2O5換算的話含有3.5至6.5質量%之鈮,以SnO2換算的話含有0.5至2質量%之錫。亦即,實施形態之氧化物燒結體係含有作為主成分之銦、與作為其他成分之鈮、錫及氧。 The oxide sintering system of the embodiment contains indium (In), niobium (Nb), tin (Sn) and oxygen (O), and can be used as a sputtering target. On the other hand, the oxide sintered body of the embodiment contains 90.0 mass % or more of indium in terms of In 2 O 3 , 3.5 to 6.5 mass % of niobium in terms of Nb 2 O 5 , and 0.5 to 2 mass % in terms of SnO 2 . % of tin. That is, the oxide sintering system of the embodiment contains indium as a main component, and niobium, tin, and oxygen as other components.
藉此,可提升將該氧化物燒結體用作為濺鍍靶所成膜之透明導電膜之在紫外光區域或紫色區域等短波長區域的穿透率。 Thereby, the transmittance of the transparent conductive film formed by using the oxide sintered body as a sputtering target in a short wavelength region such as an ultraviolet region or a violet region can be improved.
又,實施形態之透明導電膜係含有銦、鈮、錫及氧,且以In2O3換算的話含有90.0質量%以上之銦,以Nb2O5換算的話含有3.5至6.5質量%之鈮,以SnO2換算的話含有0.5至2質量%之錫。亦即,實施形態之透明導電膜係含有作為主成分之銦、與作為其他成分之鈮、錫及氧。 In addition, the transparent conductive film of the embodiment contains indium, niobium, tin and oxygen, and contains 90.0 mass % or more of indium in terms of In 2 O 3 conversion, and 3.5 to 6.5 mass % of niobium in terms of Nb 2 O 5 conversion. It contains 0.5 to 2 mass % of tin in terms of SnO 2 . That is, the transparent conductive film of the embodiment contains indium as a main component, and niobium, tin, and oxygen as other components.
藉此,可提升該透明導電膜之在紫外光區域或紫色區域等短波長區域的穿透率。因此,藉由實施形態,例如將該透明導電膜應用於太陽電池的透明電極時,射入於該太陽電池之紫外光區域的光(亦即,紫外線)亦能運用於發電,故能提升太陽電池的發光效率。 Thereby, the transmittance of the transparent conductive film in a short wavelength region such as an ultraviolet region or a violet region can be improved. Therefore, according to the embodiment, for example, when the transparent conductive film is applied to the transparent electrode of the solar cell, the light (that is, the ultraviolet light) incident in the ultraviolet region of the solar cell can also be used for power generation, so that the solar energy can be improved. The luminous efficiency of the battery.
實施形態之氧化物燒結體,以In2O3換算的話含有90.0質量%以上之銦。藉此,將該氧化物燒結體用作為濺鍍靶所成膜之透明導電膜時,可良好地維持導電性、穿透率。 The oxide sintered body of the embodiment contains 90.0 mass % or more of indium in terms of In 2 O 3 . Thereby, when the oxide sintered body is used as a transparent conductive film formed by a sputtering target, the conductivity and transmittance can be well maintained.
又,實施形態之氧化物燒結體,以In2O3換 算的話,以含有91.5至96.0質量%的銦為佳,更佳為含有92.5至95.0質量%,又更佳為含有93.6至94.4質量%。 In addition, the oxide sintered body of the embodiment preferably contains 91.5 to 96.0 mass % of indium in terms of In 2 O 3 , more preferably 92.5 to 95.0 mass %, and still more preferably 93.6 to 94.4 mass % .
又,實施形態之氧化物燒結體,較佳係以Nb2O5換算的話含有4.0至6.0質量%之鈮,以SnO2換算的話含有0.5至2質量%之錫。藉此,將該氧化物燒結體用作為濺鍍靶所成膜之透明導電膜時,可良好地維持導電性。 Further, the oxide sintered body of the embodiment preferably contains 4.0 to 6.0 mass % of niobium in terms of Nb 2 O 5 and 0.5 to 2 mass % of tin in terms of SnO 2 . Thereby, when the oxide sintered body is used as a transparent conductive film formed as a sputtering target, the conductivity can be maintained favorably.
又,實施形態之氧化物燒結體,更佳係以Nb2O5換算的話含有4.5至5.5質量%之鈮,以SnO2換算的話含有0.5至2質量%之錫,又更佳為係以Nb2O5換算的話含有4.8至5.2質量%之鈮,以SnO2換算的話含有0.8至1.2質量%之錫。 Further, the oxide sintered body of the embodiment preferably contains 4.5 to 5.5 mass % of niobium in terms of Nb 2 O 5 and 0.5 to 2 mass % of tin in terms of SnO 2 , and more preferably contains Nb It contains 4.8 to 5.2 mass % of niobium in terms of 2 O 5 and 0.8 to 1.2 mass % of tin in terms of SnO 2 .
實施形態之透明導電膜,以In2O3換算的話含有90.0質量%以上之銦。藉此,可良好地維持透明導電膜的導電性、穿透率。 The transparent conductive film of the embodiment contains 90.0 mass % or more of indium in terms of In 2 O 3 . Thereby, the conductivity and transmittance of the transparent conductive film can be maintained favorably.
又,實施形態之透明導電膜,以In2O3換算的話,以含有91.5至96.0質量%的銦為佳,更佳為含有92.5至95.0質量%,又更佳為含有93.6至94.4質量%。 In addition, the transparent conductive film of the embodiment preferably contains 91.5 to 96.0 mass % of indium in terms of In 2 O 3 , more preferably 92.5 to 95.0 mass %, and still more preferably 93.6 to 94.4 mass %.
又,實施形態之透明導電膜,較佳係以Nb2O5換算的話含有4.0至6.0質量%之鈮,以SnO2換算的話含有0.5至2質量%之錫。藉此,可良好地維持該透明導電膜的導電性。 Further, the transparent conductive film of the embodiment preferably contains 4.0 to 6.0 mass % of niobium in terms of Nb 2 O 5 and 0.5 to 2 mass % of tin in terms of SnO 2 . Thereby, the conductivity of the transparent conductive film can be maintained favorably.
再者,實施形態之透明導電膜,更佳係以Nb2O5換算的話含有4.5至5.5質量%之鈮,以SnO2換算 的話含有0.5至2質量%之錫,又更佳係以Nb2O5換算的話含有4.8至5.2質量%之鈮,以SnO2換算的話含有0.8至1.2質量%之錫。 Furthermore, the transparent conductive film of the embodiment preferably contains 4.5 to 5.5 mass % of niobium in terms of Nb 2 O 5 , and 0.5 to 2 mass % of tin in terms of SnO 2 , and more preferably contains Nb 2 It contains 4.8 to 5.2 mass % of niobium in terms of O 5 , and 0.8 to 1.2 mass % of tin in terms of SnO 2 .
又,實施形態之氧化物燒結體及透明導電膜,更佳係由作為主成分之之銦、與作為其他成分之鈮、錫及氧所構成。 Furthermore, the oxide sintered body and the transparent conductive film of the embodiment are more preferably composed of indium as the main component, and niobium, tin, and oxygen as other components.
又,實施形態之氧化物燒結體及透明導電膜,可含有來自原料等之不可避免的雜質。實施形態之氧化物燒結體中之不可避免的雜質,可舉例如Fe、Cr、Ni、Si、W、Zr等,該等之含量通常各為100ppm以下。 In addition, the oxide sintered body and the transparent conductive film of the embodiment may contain unavoidable impurities derived from raw materials and the like. The unavoidable impurities in the oxide sintered body of the embodiment include, for example, Fe, Cr, Ni, Si, W, Zr, and the like, and the content of these is usually 100 ppm or less.
又,實施形態之氧化物燒結體之比電阻較佳為7.0×10-4Ω.cm以下。藉此,當使用該氧化物燒結體作為濺鍍靶時,可進行使用廉價之DC電源的濺鍍,而能提升成膜速度。 Furthermore, the specific resistance of the oxide sintered body of the embodiment is preferably 7.0×10 -4 Ω. cm below. Thereby, when this oxide sintered body is used as a sputtering target, sputtering using an inexpensive DC power supply can be performed, and the film-forming speed can be improved.
又,實施形態之氧化物燒結體之比電阻更佳為5.0×10-4Ω.cm以下,又更佳為4.0×10-4Ω.cm以下、再更佳為3.0×10-4Ω.cm以下。 In addition, the specific resistance of the oxide sintered body of the embodiment is more preferably 5.0×10 -4 Ω. cm or less, and more preferably 4.0×10 -4 Ω. cm or less, more preferably 3.0×10 -4 Ω. cm below.
又,實施形態之氧化物燒結體的相對密度為95%以上。藉此,當使用該氧化物燒結體作為濺鍍靶時,可使DC濺鍍的放電狀態安定。又,實施形態之氧化物燒結體,較佳係相對密度為97%以上,更佳係相對密度為99%以上。 In addition, the relative density of the oxide sintered body of the embodiment is 95% or more. Thereby, when this oxide sintered body is used as a sputtering target, the discharge state of DC sputtering can be stabilized. In addition, the oxide sintered body of the embodiment preferably has a relative density of 97% or more, and more preferably has a relative density of 99% or more.
相對密度若為95%以上,則當使用該氧化物燒結體作為濺鍍靶時,可減少濺鍍靶中的空隙,而容易 防止大氣中氣體成分的侵入。又,於濺鍍時,不易產生源自於該空隙之異常放電、及濺鍍靶的破裂。 When the relative density is 95% or more, when the oxide sintered body is used as a sputtering target, the voids in the sputtering target can be reduced, and it is easy to Prevent the intrusion of gaseous components in the atmosphere. In addition, during sputtering, abnormal discharge originating from the void and cracking of the sputtering target are less likely to occur.
又,實施形態之透明導電膜,於波長300nm的穿透率較佳為52%以上,更佳為55%以上,又更佳為58%以上,再更佳為60%以上。 Furthermore, the transparent conductive film of the embodiment preferably has a transmittance at a wavelength of 300 nm of 52% or more, more preferably 55% or more, still more preferably 58% or more, and still more preferably 60% or more.
<氧化物濺鍍靶之各製造步驟> <Each production step of oxide sputtering target>
實施形態之氧化物濺鍍靶例如可藉由如下述所示之方法製造。首先,混合原料粉末。原料粉末通常為In2O3粉末、Nb2O5粉末及SnO2粉末。各原料粉末之平均粒徑較佳係皆為5μm以下,又,各原料粉末彼此之平均粒徑差較佳為2μm以下。又,原料粉末之平均粒徑,係藉由雷射繞射散射式粒度分布測定法所測得之在累積體積50容量%之體積累積直徑D50。 The oxide sputtering target of the embodiment can be produced, for example, by the method shown below. First, the raw material powders are mixed. The raw material powders are usually In 2 O 3 powder, Nb 2 O 5 powder and SnO 2 powder. The average particle diameter of each raw material powder is preferably 5 μm or less, and the difference between the average particle diameters of the raw material powders is preferably 2 μm or less. In addition, the average particle diameter of the raw material powder is the volume cumulative diameter D 50 at 50 volume % of the cumulative volume measured by a laser diffraction scattering particle size distribution measurement method.
各原料粉末之混合比率,可以使氧化物燒結體成為所期望之構成元素比的方式適當地決定。 The mixing ratio of each raw material powder can be appropriately determined so that the oxide sintered body has a desired constituent element ratio.
各原料粉末,由於一般粒子呈現凝聚,故較佳為事先粉碎後混合、或一邊混合一邊進行粉碎。 Each of the raw material powders is preferably pulverized in advance and then mixed, or pulverized while being mixed, since generally particles are aggregated.
原料之粉碎方法或混合方法並無特別限制,例如可將原料粉末置入瓶中,以球磨機進行粉碎或混合。 The pulverization method or mixing method of the raw materials is not particularly limited. For example, the raw material powder can be put into a bottle and pulverized or mixed with a ball mill.
所得之混合粉末可直接成形作為成形體,並對其進行燒結,但亦可視需要於混合粉末加入黏結劑進行成形而作為成形體。該黏結劑可使用周知之粉末冶金法中製得成形體時所使用的黏結劑,例如聚乙烯醇、丙烯酸乳膠黏結劑等。又,亦可於混合粉末加入分散介質調製成 漿料,並對該漿料進行噴霧乾燥製作成顆粒,再使該顆粒成形。 The obtained mixed powder can be directly formed as a formed body and then sintered, but it can also be formed as a formed body by adding a binder to the mixed powder as required. The binder can be a well-known binder used in powder metallurgy to prepare a shaped body, such as polyvinyl alcohol, acrylic latex binder, and the like. In addition, it can also be prepared by adding a dispersion medium to the mixed powder. slurry, and spray-drying the slurry to prepare pellets, and then shaping the pellets.
成形方法可使用以往之粉末冶金法所採用的方法,例如冷壓或CIP(Cold Isostatic Pressing:冷均壓成形)等。 As the molding method, a conventional powder metallurgy method, such as cold pressing or CIP (Cold Isostatic Pressing: Cold Isostatic Pressing), can be used.
又,亦可將混合粉末先進行暫時加壓以製作成暫時成形體,再將其粉碎後所得之粉碎粉末進行正式加壓以製作成形體。 Alternatively, the mixed powder may be temporarily pressurized to prepare a temporary compact, and then the pulverized powder obtained by pulverizing it may be subjected to full pressure to prepare a compact.
又,亦可使用滑鑄法(slip casting)等濕式成形法來製作成形體。成形體之相對密度通常為50至75%。 In addition, a formed body can also be produced by a wet molding method such as slip casting. The relative density of the shaped body is usually 50 to 75%.
接著,將所得之成形體進行燒製,以製作成燒結體。製作該燒結體之燒結爐並無特別限制,可使用製造陶瓷燒結體時能使用的燒結爐。 Next, the obtained molded body is fired to produce a sintered body. The sintering furnace for producing the sintered body is not particularly limited, and a sintering furnace that can be used for producing a ceramic sintered body can be used.
燒製溫度係以1300℃至1600℃為佳,更佳為1400℃至1600℃。燒結溫度愈高,愈可得到高密度的燒結體,另一方面,由抑制燒結體組織巨大化以防止破裂的觀點,較佳為控制在上述溫度以下。 The firing temperature is preferably 1300°C to 1600°C, more preferably 1400°C to 1600°C. The higher the sintering temperature, the more dense a sintered body can be obtained. On the other hand, it is preferable to control the temperature below the above-mentioned temperature from the viewpoint of suppressing the enlargement of the structure of the sintered body and preventing cracking.
在該燒製溫度之保持時間係以3至30小時為佳,更佳為5至20小時。當保持時間在上述範圍內時,可得到高密度的燒結體。由高密度化及防止破裂的觀點考量,升溫速度較佳為100至500℃/h。燒製環境以氧環境為佳。 The holding time at the firing temperature is preferably 3 to 30 hours, more preferably 5 to 20 hours. When the holding time is within the above range, a high-density sintered body can be obtained. From the viewpoints of densification and crack prevention, the temperature increase rate is preferably 100 to 500°C/h. The firing environment is preferably an oxygen environment.
接著,對所得之燒結體進行切削加工。該切削加工係使用平面研磨機等進行。又,切削加工後之表 面粗度Ra,可藉由選定切削加工所使用之磨石之研磨粒的大小來適當地進行控制。 Next, the obtained sintered body is subjected to cutting processing. This cutting process is performed using a surface grinder or the like. Also, the table after cutting The surface roughness Ra can be appropriately controlled by selecting the size of the abrasive grains of the grindstone used for cutting.
藉由使切削加工後之燒結體與基材接合而製作成濺鍍靶。基材之材質可適當選擇不銹鋼、銅、或鈦等。接合材可使用銦等低熔點焊料。 A sputtering target is produced by joining the sintered body after cutting and the base material. The material of the substrate can be appropriately selected from stainless steel, copper, or titanium. As the bonding material, low melting point solder such as indium can be used.
[實施例1] [Example 1]
將平均粒徑為0.7μm之In2O3粉末、平均粒徑為1.2μm之Nb2O5粉末、及平均粒徑為0.9μm之SnO2粉末,於瓶中藉由氧化鋯球進行球磨機乾式混合,調製成混合粉末。 The In 2 O 3 powder with an average particle size of 0.7 μm, the Nb 2 O 5 powder with an average particle size of 1.2 μm, and the SnO 2 powder with an average particle size of 0.9 μm were placed in a bottle by zirconia balls. Mix to make a mixed powder.
又,原料粉末之平均粒徑係使用日機裝股份有限公司製的粒度分布測定裝置HRA進行測定。於該測定時,溶劑係使用水,以測定物質之折射率2.20進行測定。 In addition, the average particle diameter of a raw material powder was measured using the particle size distribution measuring apparatus HRA by Nikkiso Co., Ltd. product. In this measurement, water was used as the solvent, and the measurement was performed at a refractive index of 2.20 of the measurement substance.
又,於調製混合粉末時,係以使銦以In2O3換算的話成為94.5質量%、鈮以Nb2O5換算的話成為5.0質量%、錫以SnO2換算的話成為0.5質量%的方式調配各原料粉末。 In addition, when preparing the mixed powder, it was prepared so that indium would be 94.5 mass % in terms of In 2 O 3 , niobium would be 5.0 mass % in terms of Nb 2 O 5 , and tin would be 0.5 mass % in terms of SnO 2 . each raw material powder.
接著,對於混合粉末添加6質量%之已稀釋為4質量%的聚乙烯醇,使用研缽將聚乙烯醇充分塗抹於粉末,使其通過5網眼的篩網。接著,將所得之粉末以200kg/cm2的條件暫時加壓,將所得之暫時成形體以研缽粉碎。接著,將所得之粉碎粉填充於加壓用模具,以加壓壓力1t/cm2進行成形60秒鐘,製得成形體。 Next, 6 mass % of polyvinyl alcohol diluted to 4 mass % was added to the mixed powder, and polyvinyl alcohol was sufficiently applied to the powder using a mortar and passed through a 5-mesh sieve. Next, the obtained powder was temporarily pressurized under the condition of 200 kg/cm 2 , and the obtained temporary compact was pulverized with a mortar. Next, the obtained pulverized powder was filled in a press mold, and molded at a press pressure of 1 t/cm 2 for 60 seconds to obtain a molded body.
接著,將該成形體進行燒製而作成燒結體。該燒製係在爐內以10L/min流通氧的氧氣流環境下進行,並以燒製溫度1550℃、燒製時間9小時、升溫速度350℃/h、降溫速度100℃/h進行。 Next, the formed body is fired to obtain a sintered body. The firing was carried out in a furnace in an oxygen flow environment with oxygen flowing at 10 L/min at a firing temperature of 1550°C, a firing time of 9 hours, a temperature increase rate of 350°C/h, and a temperature drop rate of 100°C/h.
接著,對所得之燒結體進行切削加工,製得表面粗度Ra為1.0μm之寬度210mm×長度710mm×厚度6mm的氧化物燒結體。又,於該切削加工係使用#170的磨石。 Next, the obtained sintered body was machined to obtain an oxide sintered body having a surface roughness Ra of 1.0 μm and a width of 210 mm×length 710 mm×thickness 6 mm. In addition, the grinding stone of #170 was used for this cutting process.
[實施例2至7] [Examples 2 to 7]
使用與實施例1同樣的方法,製得氧化物燒結體。又,實施例2至7中,於調製混合粉末時,係以使銦、鈮及錫之含有率以In2O3、Nb2O5及SnO2換算的話成為表1所記載之含有率的方式調配各原料粉末。 In the same manner as in Example 1, an oxide sintered body was obtained. In addition, in Examples 2 to 7, when the mixed powder was prepared, the contents of indium, niobium and tin were converted into the contents described in Table 1 in terms of In 2 O 3 , Nb 2 O 5 and SnO 2 . way to prepare each raw material powder.
[比較例1至6] [Comparative Examples 1 to 6]
使用與實施例1同樣的方法,製得氧化物燒結體。又,比較例1至6中,於調製混合粉末時,係以使銦、鈮及錫之含有率以In2O3、Nb2O5及SnO2換算的話成為表1所記載之含有率的方式調配各原料粉末。 In the same manner as in Example 1, an oxide sintered body was obtained. In addition, in Comparative Examples 1 to 6, when the mixed powder was prepared, the contents of indium, niobium and tin were converted into the contents described in Table 1 in terms of In 2 O 3 , Nb 2 O 5 and SnO 2 . way to prepare each raw material powder.
又,於實施例1至7及比較例1至6中,於調製各原料粉末時所測量之各元素的含有率,已藉ICP-AES(Inductively Coupled Plasma Atomic Emission Spectroscopy:感應耦合電漿原子發射光譜法)確認與所得之氧化物燒結體中之各元素的含有率相等。 In addition, in Examples 1 to 7 and Comparative Examples 1 to 6, the content ratio of each element measured when preparing each raw material powder was measured by ICP-AES (Inductively Coupled Plasma Atomic Emission Spectroscopy: Inductively Coupled Plasma Atomic Emission Spectrometry) was confirmed to be equal to the content of each element in the obtained oxide sintered body.
接著,對上述所得之實施例1至7及比較 例1至6的氧化物燒結體,進行相對密度的測定。該相對密度係根據阿基米德法進行測定。 Next, the above-obtained Examples 1 to 7 and their comparison The relative density of the oxide sintered bodies of Examples 1 to 6 was measured. The relative density was measured according to the Archimedes method.
具體而言,係將氧化物燒結體之空中質量除以體積(燒結體之水中質量/在測量溫度的水比重),並以相對於理論密度ρ(g/cm3)之百分率的值作為相對密度(單位:%)。 Specifically, the air mass of the oxide sintered body is divided by the volume (the water mass of the sintered body/the water specific gravity at the measurement temperature), and the value of the percentage relative to the theoretical density ρ (g/cm 3 ) is used as the relative Density (unit: %).
又,該理論密度ρ(g/cm3)係由製造氧化物燒結體時所使用之原料粉末的質量%及密度計算出。具體而言,係依下述之式所計算出。 In addition, the theoretical density ρ (g/cm 3 ) is calculated from the mass % and the density of the raw material powder used for producing the oxide sintered body. Specifically, it is calculated according to the following formula.
ρ={(C1/100)/ρ1+(C2/100)/ρ2+(C3/100)/ρ3}-1 ρ={(C 1 /100)/ρ 1 +(C 2 /100)/ρ 2 +(C 3 /100)/ρ 3 } -1
又,上述式中之C1至C3及ρ1至ρ3,分別表示以下之值。 In addition, C 1 to C 3 and ρ 1 to ρ 3 in the above formula represent the following values, respectively.
.C1:氧化物燒結體製造時所使用之In2O3粉末的質量% . C 1 : Mass % of the In 2 O 3 powder used in the production of the oxide sintered body
.ρ1:In2O3之密度(7.18g/cm3) . ρ 1 : Density of In 2 O 3 (7.18 g/cm 3 )
.C2:氧化物燒結體製造時所使用之Nb2O5粉末的質量% . C 2 : Mass % of Nb 2 O 5 powder used in the production of oxide sintered body
.ρ2:Nb2O5之密度(4.47g/cm3) . ρ 2 : Density of Nb 2 O 5 (4.47g/cm 3 )
.C3:氧化物燒結體製造時所使用之SnO2粉末的質量% . C 3 : Mass % of SnO 2 powder used in the production of oxide sintered body
.ρ3:SnO2之密度(6.95g/cm3) . ρ 3 : Density of SnO 2 (6.95g/cm 3 )
接著,對上述所得之實施例1至7及比較例1至6之濺鍍靶用氧化物燒結體,分別進行比電阻(體電阻)的測定。 Next, the specific resistance (bulk resistance) was measured for the oxide sintered bodies for sputtering targets of Examples 1 to 7 and Comparative Examples 1 to 6 obtained above, respectively.
具體而言,係使用三菱化學股份有限公司製Loresta(註冊商標)HP MCP-T410(串列四探針TYPE ESP),使探針接觸加工後之氧化物燒結體的表面,以AUTO RANGE模式進行測定。測定部位為氧化物燒結體之中央附近及四角落共計五處,以各測定值之平均值作為該燒結體之體積電阻值。 Specifically, Loresta (registered trademark) HP MCP-T410 (tandem four-probe TYPE ESP) manufactured by Mitsubishi Chemical Co., Ltd. was used, the probe was brought into contact with the surface of the processed oxide sintered body, and the AUTO RANGE mode was used to measure. The measurement locations were five locations in total near the center and the four corners of the oxide sintered body, and the average value of each measured value was taken as the volume resistance value of the sintered body.
此處,關於實施例1至7及比較例1至6,將混合粉末時所含之各元素的含有率、與相對密度及比電阻(體電阻)的測定結果顯示於表1。 Here, about Examples 1 to 7 and Comparative Examples 1 to 6, Table 1 shows the content ratio of each element contained in the powder mixture, and the measurement results of relative density and specific resistance (volume resistance).
可知實施例1至7之氧化物燒結體的比電阻皆為7.0×10-4Ω.cm以下。因此,藉由實施形態,當使用氧化物燒結體作為濺鍍靶時,可進行使用廉價DC電源的濺鍍,而能提升成膜速度。 It can be seen that the specific resistances of the oxide sintered bodies of Examples 1 to 7 are all 7.0×10 -4 Ω. cm below. Therefore, according to the embodiment, when the oxide sintered body is used as the sputtering target, sputtering using an inexpensive DC power supply can be performed, and the film formation speed can be improved.
接著,由上述實施例1至7及比較例1至6 之氧化物燒結體,製作實施例1至7及比較例1至6的濺鍍靶。該濺鍍靶係使用屬於低熔點焊料之銦作為接合材,並將上述所得之氧化物燒結體接合於銅製的基材而製作。 Next, from the above-mentioned Examples 1 to 7 and Comparative Examples 1 to 6 The oxide sintered bodies were produced as sputtering targets of Examples 1 to 7 and Comparative Examples 1 to 6. This sputtering target is produced by using indium, which is a low melting point solder, as a bonding material, and bonding the oxide sintered body obtained above to a copper base material.
接著,使用所製作之實施例1至7及比較例1至6的濺鍍靶,以下述之條件進行濺鍍成膜,成膜為厚度100nm的薄膜。 Next, using the sputtering targets of Examples 1 to 7 and Comparative Examples 1 to 6 produced, sputtering was performed under the following conditions to form a thin film having a thickness of 100 nm.
.成膜裝置:真空機器工業股份有限公司製EX-3013M(DC濺鍍裝置) . Film-forming device: EX-3013M (DC sputtering device) manufactured by Vacuum Machinery Industry Co., Ltd.
.到達真空度:未達1×10-4Pa . Arrived vacuum degree: less than 1×10 -4 Pa
.濺鍍氣體:Ar/O2混合氣體 . Sputtering gas: Ar/O 2 mixed gas
.濺鍍氣壓:0.4Pa . Sputtering pressure: 0.4Pa
.O2氣體流量:0至2.0sccm . O gas flow: 0 to 2.0sccm
.基板:玻璃基板(Corning公司製EAGLE XG(註冊商標)) . Substrate: Glass substrate (EAGLE XG (registered trademark) manufactured by Corning Corporation)
.基板溫度:室溫 . Substrate temperature: room temperature
.濺鍍電力:3W/cm2 . Sputtering power: 3W/cm 2
又,於實施例1至7及比較例1至6,藉由ICP-AES,確認到濺鍍靶所使用之氧化物燒結體中之各元素的含有率,與所成膜之透明導電膜中之各元素的含有率相等。 In addition, in Examples 1 to 7 and Comparative Examples 1 to 6, it was confirmed by ICP-AES that the content of each element in the oxide sintered body used for the sputtering target was the same as that in the formed transparent conductive film. The content of each element is equal.
接著,分別由各玻璃基板裁切出既定的大小,對該切出的玻璃基板,測定所濺鍍成膜之實施例1至7及比較例1至6之透明導電膜中之穿透率的波長相依性。 Next, each glass substrate was cut out to a predetermined size, and the cut-out glass substrate was measured for the transmittance of the transparent conductive films of Examples 1 to 7 and Comparative Examples 1 to 6 formed by sputtering. wavelength dependence.
再者,將所切出之玻璃基板於大氣中以200℃熱處理1小時,亦測定熱處理後之透明導電膜中之穿透 率的波長相依性。上述之熱處理前後之穿透率的波長相依性之測定條件,係如以下所述。 Furthermore, the cut glass substrate was heat-treated at 200°C for 1 hour in the atmosphere, and the penetration in the transparent conductive film after heat-treatment was also measured. The wavelength dependence of the rate. The measurement conditions of the wavelength dependence of the transmittance before and after the above-mentioned heat treatment are as follows.
.測定裝置:日立先端科技公司製 紫外可見近紅外分光光度計UH4150 . Measuring device: UV-Vis-NIR spectrophotometer UH4150 manufactured by Hitachi Advanced Technology Co., Ltd.
.掃描速度:600nm/min . Scanning speed: 600nm/min
.波長範圍:200至2600nm . Wavelength range: 200 to 2600nm
又,於透明導電膜的穿透率測定中,先將未進行成膜之素玻璃基板裝設於裝置以測定基線,然後測定各成膜樣品的穿透率。 In addition, in the transmittance measurement of the transparent conductive film, a plain glass substrate without film formation was first installed in the apparatus to measure the baseline, and then the transmittance of each film-forming sample was measured.
第1圖係顯示實施例2及比較例1、4之透明導電膜之熱處理前之穿透率的波長相依性之圖表,第2圖係顯示相同透明導電膜之熱處理後之穿透率的波長相依性之圖表。如第1圖及第2圖所示,藉由對經濺鍍成膜之透明導電膜施以既定的熱處理,可整體提升透明導電膜的穿透率。 Figure 1 is a graph showing the wavelength dependence of transmittance before heat treatment of the transparent conductive films of Example 2 and Comparative Examples 1 and 4, and Figure 2 is a graph showing the wavelength dependence of transmittance after heat treatment of the same transparent conductive films Dependency chart. As shown in FIG. 1 and FIG. 2 , by applying a predetermined heat treatment to the transparent conductive film formed by sputtering, the transmittance of the transparent conductive film can be improved as a whole.
接著,進行成膜後之經熱處理之各透明導電膜之比電阻的測定。該透明導電膜之比電阻測定係使用共和理研公司製的四探針計測器K-705RS進行測定。 Next, the specific resistance of each heat-treated transparent conductive film after film formation was measured. The specific resistance of the transparent conductive film was measured using a four-point probe K-705RS manufactured by Kyowa Riken Co., Ltd.
此處,對於上述實施例1至7及比較例1至6之透明導電膜,將熱處理前後之波長300nm、400nm及550nm下之穿透率的測定結果、與熱處理後之比電阻測定的結果顯示於表2。又,表2所示之比電阻測定的評價基準,係如以下所述。 Here, for the transparent conductive films of Examples 1 to 7 and Comparative Examples 1 to 6, the measurement results of transmittance at wavelengths of 300 nm, 400 nm, and 550 nm before and after heat treatment, and the results of specific resistance measurement after heat treatment are shown. in Table 2. In addition, the evaluation criteria of the specific resistance measurement shown in Table 2 are as follows.
A:比電阻為4.5×10-4Ω.cm以下。 A: The specific resistance is 4.5×10 -4 Ω. cm below.
B:比電阻超過4.5×10-4Ω.cm且為6.0×10-4Ω.cm以下。 B: The specific resistance exceeds 4.5×10 -4 Ω. cm and is 6.0×10 -4 Ω. cm below.
C:比電阻超過6.0×10-4Ω.cm。 C: The specific resistance exceeds 6.0×10 -4 Ω. cm.
於熱處理後的透明導電膜中,將以In2O3換
算的話含有90.0質量%以上之銦、以Nb2O5換算的話含有3.5至6.5質量%之鈮、以SnO2換算的話含有0.5至2質量%之錫的實施例1至7,與未以該含有率含有鈮及錫的比較例1至6進行比較,可知藉由以In2O3換算的話含有90.0質量%以上之銦、以Nb2O5換算的話含有3.5至6.5質量%之鈮、以SnO2換算的話含有0.5至2質量%之錫,使在紫外光區域(波長300nm)的穿透率提升至52%以上。
The transparent conductive film after the heat treatment contains 90.0 mass % or more of indium in terms of In 2 O 3 , 3.5 to 6.5 mass % of niobium in terms of Nb 2 O 5 , and 0.5 to 2 mass % in terms of SnO 2 . By comparing Examples 1 to 7 with tin in mass % and Comparative Examples 1 to 6 in which niobium and tin are not contained at the content ratio, it can be seen that in terms of In 2 O 3 , 90.0 mass % or more of indium is contained, and Nb It contains 3.5 to 6.5 mass % of niobium in terms of 2 O 5 and 0.5 to 2 mass % of tin in terms of SnO 2 , so that the transmittance in the ultraviolet region (
又,於熱處理後之透明導電膜,於實施例1至7中,如表2及第2圖所示,不僅紫外光區域,連可見光區域(例如波長400nm至800nm)亦具有與比較例1至6同等以上的穿透率。亦即,於實施形態,當將該透明導電膜應用於太陽電池的透明電極時,可將射入於該太陽電池之廣範圍波長區域的光運用於發電。 In addition, in Examples 1 to 7, the transparent conductive films after heat treatment, as shown in Table 2 and Figure 2, not only in the ultraviolet light region, but also in the visible light region (for example, wavelengths of 400 nm to 800 nm) have the same characteristics as those in Comparative Examples 1 to 10. 6 The penetration rate of the same or more. That is, in the embodiment, when the transparent conductive film is applied to a transparent electrode of a solar cell, light incident in a wide wavelength region of the solar cell can be used for power generation.
因此,藉由實施形態,可更提升應用該透明導電膜之太陽電池的發電效率。 Therefore, according to the embodiment, the power generation efficiency of the solar cell to which the transparent conductive film is applied can be further improved.
又,將以In2O3換算的話含有90.0質量%以上之銦、以Nb2O5換算的話含有4.0至6.0質量%之鈮、以SnO2換算的話含有0.5至2質量%之錫的實施例1至3、5、6,與未以該含有率含有鈮的實施例4、7連行比較,可知藉由以In2O3換算的話含有90.0質量%以上之銦、以Nb2O5換算的話含有4.0至6.0質量%之鈮、以SnO2換算的話含有0.5至2質量%之錫,可良好地維持透明導電膜的導電性。 In addition, examples in which 90.0 mass % or more of indium is contained in terms of In 2 O 3 , 4.0 to 6.0 mass % of niobium in terms of Nb 2 O 5 , and 0.5 to 2 mass % of tin in terms of SnO 2 are included. 1 to 3, 5, and 6 are compared with those of Examples 4 and 7 that do not contain niobium at this content rate. It can be seen that 90.0 mass % or more of indium is contained in terms of In 2 O 3 , and indium is contained in terms of Nb 2 O 5 . By containing 4.0 to 6.0 mass % of niobium and 0.5 to 2 mass % of tin in terms of SnO 2 , the conductivity of the transparent conductive film can be maintained favorably.
再者,將以In2O3換算的話含有90.0質量% 以上之銦、以Nb2O5換算的話含有4.5至5.5質量%之鈮、以SnO2換算的話含有0.5至2質量%之錫的實施例1至3,與未以該含有率含有鈮的實施例4至7進行比較,可知藉由以In2O3換算的話含有90.0質量%以上之銦、以Nb2O5換算的話含有4.5至5.5質量%之鈮、以SnO2換算的話含有0.5至2質量%之錫,可使在紫色區域(波長400nm)之穿透率提升至93.2%以上。 In addition, the implementation of 90.0 mass % or more of indium in terms of In 2 O 3 , 4.5 to 5.5 mass % of niobium in terms of Nb 2 O 5 , and 0.5 to 2 mass % of tin in SnO 2 conversion Comparing Examples 1 to 3 with Examples 4 to 7 that do not contain niobium at the content ratio, it is found that 90.0 mass % or more of indium is contained in terms of In 2 O 3 , and 4.5 to 4.5 mass % of indium is contained in terms of Nb 2 O 5 . 5.5 mass % of niobium and 0.5 to 2 mass % of tin in SnO 2 conversion can improve the transmittance in the purple region (wavelength 400nm) to 93.2% or more.
再者,將以In2O3換算的話含有90.0質量%以上之銦、以Nb2O5換算的話含有4.8至5.2質量%之鈮、並且以SnO2換算的話含有0.8至1.2質量%之錫的實施例2,與未以該含有率含有鈮及錫的實施例1、3至7進行比較,可知藉由以Nb2O5換算的話含有4.8至5.2質量%之鈮、以SnO2換算的話含有0.8至1.2質量%之錫,使於紫外光區域(波長300nm)的穿透率提升至61.4%以上,並且使於紫色區域(波長400nm)之穿透率提升至94.6%以上。 In addition, it contains 90.0 mass % or more of indium in terms of In 2 O 3 , 4.8 to 5.2 mass % of niobium in terms of Nb 2 O 5 , and 0.8 to 1.2 mass % of tin in terms of SnO 2 . Example 2 was compared with Examples 1, 3 to 7 which did not contain niobium and tin at the content ratios, and it was found that 4.8 to 5.2 mass % of niobium was contained in terms of Nb 2 O 5 and 4.8 to 5.2 mass % in terms of SnO 2 . 0.8 to 1.2 mass % of tin increases the transmittance in the ultraviolet region (wavelength 300nm) to over 61.4% and in the purple region (wavelength 400nm) to over 94.6%.
以上,針對本發明之實施形態進行說明,但本發明並不限定於上述之實施形態,只要在不脫離其主旨之範圍內便可進行各種變更。例如,於實施形態,雖然揭示將透明導電膜應用於太陽電池之例,但可應用實施形態之透明導電膜的裝置,並不限於太陽電池。 As mentioned above, although embodiment of this invention was described, this invention is not limited to the said embodiment, Various changes are possible in the range which does not deviate from the summary. For example, in the embodiment, the example in which the transparent conductive film is applied to the solar cell is disclosed, but the device to which the transparent conductive film of the embodiment can be applied is not limited to the solar cell.
例如,當將實施形態之透明導電膜應用於液晶或有機EL(electro-luminescence)等影像顯示裝置之透明電極時,由於紫外光區域或紫色區域等之短波長區域的穿透率高,故能改善短波長區域的發光效率。 For example, when the transparent conductive film of the embodiment is applied to a transparent electrode of an image display device such as liquid crystal or organic EL (electro-luminescence), since the transmittance of the short wavelength region such as the ultraviolet region and the violet region is high, it can be Improves luminous efficiency in the short wavelength region.
又,藉由將實施形態之透明導電膜應用於紫外線燈等紫外線光源之光學系的抗靜電膜,可提升紫外光區域的發光效率,並且可在不產生靜電的情況下安定地發出紫外光。 Furthermore, by applying the transparent conductive film of the embodiment to an antistatic film of an optical system of an ultraviolet light source such as an ultraviolet lamp, the luminous efficiency in the ultraviolet region can be improved, and ultraviolet light can be stably emitted without generating static electricity.
又,於實施形態,雖然揭示使用板狀之氧化物燒結體製作濺鍍靶之例,但氧化物燒結體的形狀並不限於板狀,亦可為圓筒狀等各種形狀。 In addition, in the embodiment, although the example in which the sputtering target was produced using the oxide sintered body in a plate shape was disclosed, the shape of the oxide sintered body is not limited to the plate shape, and may be various shapes such as a cylindrical shape.
更多的效果及變形例,可容易地由業者導出。因此,本發明之更廣泛的樣態,並不限定於以上所表示且記述之特定的詳細狀況及代表的實施形態。因此,只要不脫離錄附之申請專利範圍及其均等物所定義之整體發明概念的精神或範圍,可進行各種變更。 More effects and modifications can be easily derived by manufacturers. Therefore, the broader aspect of the present invention is not limited to the specific details and representative embodiments shown and described above. Therefore, various modifications can be made without departing from the spirit or scope of the overall inventive concept defined by the appended claims and their equivalents.
Claims (7)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2018069268 | 2018-03-30 | ||
| JP2018-069268 | 2018-03-30 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| TW201942088A TW201942088A (en) | 2019-11-01 |
| TWI768149B true TWI768149B (en) | 2022-06-21 |
Family
ID=68061105
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| TW107139172A TWI768149B (en) | 2018-03-30 | 2018-11-05 | Oxide sintered body, sputtering target and transparent conductive film |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP7203088B2 (en) |
| TW (1) | TWI768149B (en) |
| WO (1) | WO2019187269A1 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116730710A (en) * | 2023-02-07 | 2023-09-12 | 中山智隆新材料科技有限公司 | A kind of high-valent element doped indium tin oxide material and its preparation method and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW201118058A (en) * | 2009-10-26 | 2011-06-01 | Jx Nippon Mining & Metals Corp | Indium oxide sintered body and indium oxide transparent conductive film |
| TW201216477A (en) * | 2004-03-09 | 2012-04-16 | Idemitsu Kosan Co | Thin film transistor and substrate with thin film transistor and production method of them and liquid crystal display apparatus and related apparatus and related method, sputtering target and transparent conductive film produced by using the same and tra |
| TW201413014A (en) * | 2012-08-10 | 2014-04-01 | Mitsubishi Materials Corp | Sputter target for forming transparent oxide film and method of producing the same |
| TW201506183A (en) * | 2013-07-12 | 2015-02-16 | Samsung Display Co Ltd | Method of manufacturing a sputtering target |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02309511A (en) * | 1989-05-24 | 1990-12-25 | Showa Denko Kk | Transparent conductive film |
| JP3128124B2 (en) * | 1989-06-13 | 2001-01-29 | 東ソー株式会社 | Conductive metal oxide sintered body and use thereof |
| JP2005258115A (en) * | 2004-03-12 | 2005-09-22 | Idemitsu Kosan Co Ltd | Thin film transistor type substrate, thin film transistor type liquid crystal display device, and method of manufacturing thin film transistor type substrate |
| JP5436343B2 (en) * | 2010-06-04 | 2014-03-05 | 出光興産株式会社 | Sputtering target, transparent conductive film and transparent conductive glass substrate |
| WO2011152682A2 (en) * | 2010-06-04 | 2011-12-08 | 주식회사 나노신소재 | Transparent conductive layer, target for transparent conductive layer and a process for producing the target for transparent conductive layer |
-
2018
- 2018-10-16 JP JP2020509586A patent/JP7203088B2/en active Active
- 2018-10-16 WO PCT/JP2018/038464 patent/WO2019187269A1/en not_active Ceased
- 2018-11-05 TW TW107139172A patent/TWI768149B/en active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW201216477A (en) * | 2004-03-09 | 2012-04-16 | Idemitsu Kosan Co | Thin film transistor and substrate with thin film transistor and production method of them and liquid crystal display apparatus and related apparatus and related method, sputtering target and transparent conductive film produced by using the same and tra |
| TW201118058A (en) * | 2009-10-26 | 2011-06-01 | Jx Nippon Mining & Metals Corp | Indium oxide sintered body and indium oxide transparent conductive film |
| TW201413014A (en) * | 2012-08-10 | 2014-04-01 | Mitsubishi Materials Corp | Sputter target for forming transparent oxide film and method of producing the same |
| TW201506183A (en) * | 2013-07-12 | 2015-02-16 | Samsung Display Co Ltd | Method of manufacturing a sputtering target |
Also Published As
| Publication number | Publication date |
|---|---|
| JP7203088B2 (en) | 2023-01-12 |
| JPWO2019187269A1 (en) | 2021-04-08 |
| WO2019187269A1 (en) | 2019-10-03 |
| TW201942088A (en) | 2019-11-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI488826B (en) | An indium oxide sintered body, an indium oxide transparent conductive film, and a method for producing the transparent conductive film | |
| KR102030892B1 (en) | Ito sputtering target and method for manufacturing same, ito transparent electroconductive film, and method for manufacturing ito transparent electroconductive film | |
| TWI661069B (en) | Manufacturing method of sputtering target | |
| JP5224073B2 (en) | Oxide deposition material and method for producing the same | |
| KR102493208B1 (en) | Cylindrical sputtering target, cylindrical compact, manufacturing method of cylindrical sputtering target, manufacturing method of cylindrical sintered compact and manufacturing method of cylindrical compact | |
| TWI778100B (en) | Oxide sintered body and sputtering target | |
| TWI768149B (en) | Oxide sintered body, sputtering target and transparent conductive film | |
| JP2011074479A (en) | Target for ion plating for producing zinc oxide-based transparent conductive thin film, and zinc oxide-based transparent conductive thin film | |
| CN101208453B (en) | Gallium oxide-zinc oxide-based sputtering target, method for forming transparent conductive film, and transparent conductive film | |
| WO2014021374A1 (en) | Oxide sintered body and tablet obtained by processing same | |
| JP5381724B2 (en) | Method for producing ZnO vapor deposition material | |
| JP5381725B2 (en) | Method for producing ZnO vapor deposition material | |
| CN102549191A (en) | Target for zno-based transparent conductive film and method for producing same | |
| TWI696597B (en) | Sintered body, sputtering target material and method for manufacturing sintered body | |
| JP5018553B2 (en) | ZnO vapor deposition material, method for producing the same, and ZnO film formed thereby | |
| CN101208452A (en) | Gallium oxide-zinc oxide-based sputtering target, method for forming transparent conductive film, and transparent conductive film | |
| KR20180116281A (en) | Oxide-sintered body and oxide-transparent conductive film | |
| TWI683018B (en) | IZO target material and its manufacturing method | |
| JP6155919B2 (en) | Composite oxide sintered body and oxide transparent conductive film | |
| JP5018552B2 (en) | ZnO vapor deposition material, method for producing the same, and ZnO film formed thereby | |
| WO2013042747A1 (en) | Oxide sintered body, method for producing same, and oxide transparent conductive film | |
| WO2025115478A1 (en) | Oxide sputtering target and method for manufacturing same | |
| CN110318026A (en) | Sputter target |