JP2000044236A - Article having transparent conductive oxide thin film and its production - Google Patents
Article having transparent conductive oxide thin film and its productionInfo
- Publication number
- JP2000044236A JP2000044236A JP10208948A JP20894898A JP2000044236A JP 2000044236 A JP2000044236 A JP 2000044236A JP 10208948 A JP10208948 A JP 10208948A JP 20894898 A JP20894898 A JP 20894898A JP 2000044236 A JP2000044236 A JP 2000044236A
- Authority
- JP
- Japan
- Prior art keywords
- substrate
- range
- ratio
- article
- film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 25
- 239000010409 thin film Substances 0.000 title description 12
- 239000000758 substrate Substances 0.000 claims abstract description 45
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 18
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 17
- 238000000608 laser ablation Methods 0.000 claims abstract description 12
- 238000004544 sputter deposition Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 17
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 16
- 239000004973 liquid crystal related substance Substances 0.000 claims description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 14
- 150000001768 cations Chemical class 0.000 claims description 11
- 239000011521 glass Substances 0.000 claims description 10
- 239000004065 semiconductor Substances 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims 2
- 206010021143 Hypoxia Diseases 0.000 claims 1
- 229920000307 polymer substrate Polymers 0.000 claims 1
- 229910052738 indium Inorganic materials 0.000 abstract description 3
- 229910052725 zinc Inorganic materials 0.000 abstract description 3
- 229910052788 barium Inorganic materials 0.000 abstract description 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
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract 1
- 239000011707 mineral Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 32
- 239000011701 zinc Substances 0.000 description 20
- 238000010521 absorption reaction Methods 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 9
- 238000002834 transmittance Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 230000003287 optical effect Effects 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 230000007613 environmental effect Effects 0.000 description 5
- 150000003254 radicals Chemical class 0.000 description 5
- -1 D y Inorganic materials 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 239000000969 carrier Substances 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 2
- 230000005355 Hall effect Effects 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- 229910001026 inconel Inorganic materials 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003826 uniaxial pressing Methods 0.000 description 2
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 101100321669 Fagopyrum esculentum FA02 gene Proteins 0.000 description 1
- 229910005555 GaZnO Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 241001676573 Minium Species 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910007541 Zn O Inorganic materials 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- VRAIHTAYLFXSJJ-UHFFFAOYSA-N alumane Chemical compound [AlH3].[AlH3] VRAIHTAYLFXSJJ-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052713 technetium Inorganic materials 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000000411 transmission spectrum Methods 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/68—Types of semiconductor device ; Multistep manufacturing processes therefor controllable by only the electric current supplied, or only the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched
- H01L29/76—Unipolar devices, e.g. field effect transistors
- H01L29/772—Field effect transistors
- H01L29/78—Field effect transistors with field effect produced by an insulated gate
- H01L29/786—Thin film transistors, i.e. transistors with a channel being at least partly a thin film
- H01L29/7869—Thin film transistors, i.e. transistors with a channel being at least partly a thin film having a semiconductor body comprising an oxide semiconductor material, e.g. zinc oxide, copper aluminium oxide, cadmium stannate
- H01L29/78693—Thin film transistors, i.e. transistors with a channel being at least partly a thin film having a semiconductor body comprising an oxide semiconductor material, e.g. zinc oxide, copper aluminium oxide, cadmium stannate the semiconducting oxide being amorphous
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/40—Electrodes ; Multistep manufacturing processes therefor
- H01L29/43—Electrodes ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/45—Ohmic electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/66007—Multistep manufacturing processes
- H01L29/66969—Multistep manufacturing processes of devices having semiconductor bodies not comprising group 14 or group 13/15 materials
Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明は、高い導電性と可
視、特に青色光透過性を有し、かつ作製が容易である非
晶質性酸化物を含む透明導電体膜を有する物品およびそ
の製造方法に関する。さらに本発明は、本発明の物品か
らなる電極に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an article having a transparent conductor film containing an amorphous oxide which has high conductivity and visible light, particularly blue light transmittance, and is easy to produce, and its production. About the method. Further, the present invention relates to an electrode comprising the article of the present invention.
【0002】[0002]
【従来の技術】光透過型液晶パネルディスプレイは薄
型、軽量の表示装置として各種の電気製品に幅広く用い
られている。特にパーソナルコンピュータやワードプロ
セッサ等のOA機器への導入は活発であり、現在対角約10
インチ程度のノート型パソコンや、省スペースのデスク
トップパソコン用のディスプレイとして益々需要が高ま
っており、更に大面積化、多画素化、高精細化の方向で
改良が加えられている。2. Description of the Related Art Light-transmitting liquid crystal panel displays are widely used in various electric appliances as thin and lightweight display devices. In particular, the introduction to OA equipment such as personal computers and word processors is active.
The demand for displays for notebook computers of about inches and space-saving desktop personal computers is increasing, and improvements are being made in the direction of larger areas, more pixels, and higher definition.
【0003】光透過型の液晶では透明電極が不可欠であ
り、透明電極材料としては主にITOが使用されている。I
TOは紫外域のほぼ全域で透明であり、電気抵抗率を1×
10−4Ωcm程度まで低減できるので、液晶ティスプ
レイ等の透明電極材料として好適であった。近年は、高
精細化の要求に応えてITOのアモルファス相、いわゆ
るアモルファスITOが使用されるようになってきてい
る。アモルファスITOは結晶性のITOに比べてパタ
ーニング性が良好なため、細い電極パターンをきれいに
切れるからである。電気抵抗率は結晶性ITOに比べて
増大してしまうが、液晶ティスプレイの主流を占めるT
FT型の画素電極用には十分な抵抗値であるからであ
る。また、ティスプレイを軽量化するためにプラスチッ
ク基板が用いられる傾向にあり、室温成膜の可能なアモ
ルファスITOが好適と考えられる。結晶性ITOの成
膜には200℃以上の温度を要するからである。[0003] A transparent electrode is indispensable for a light transmission type liquid crystal, and ITO is mainly used as a transparent electrode material. I
TO is transparent over almost the entire ultraviolet region and has an electrical resistivity of 1 ×
Since it can be reduced to about 10 −4 Ωcm, it was suitable as a transparent electrode material such as a liquid crystal display. In recent years, an amorphous phase of ITO, so-called amorphous ITO, has been used in response to a demand for higher definition. This is because amorphous ITO has a better patterning property than crystalline ITO, so that a thin electrode pattern can be cut cleanly. Although the electrical resistivity increases as compared with the crystalline ITO, T which occupies the mainstream of the liquid crystal display.
This is because the resistance value is sufficient for an FT type pixel electrode. Further, a plastic substrate tends to be used to reduce the weight of the display, and amorphous ITO which can be formed at room temperature is considered to be suitable. This is because a temperature of 200 ° C. or higher is required for forming the crystalline ITO.
【0004】[0004]
【発明が解決しようとする課題】アモルファスITOは
その成分の90%以上がIn2O3からなる。このため、
近年の液晶ディスプレイの普及に伴ってIn2O3の価格
が2倍程度まで高騰して、原料コトスを大きくする要因
となっている。また、In2O3は希少金属であって、あ
と30年程度採掘を継続すると枯渇すると予測されてい
る。このような理由から、In2O3の含有量が低く、原
料コストが低く、資源環境負荷が低い材料が必要になり
つつある。In the amorphous ITO, 90% or more of its components are composed of In 2 O 3 . For this reason,
With the spread of liquid crystal displays in recent years, the price of In 2 O 3 has soared to about twice, which is a factor of increasing the raw material cost. Further, In 2 O 3 is a rare metal, and is expected to be depleted when mining is continued for about 30 years. For these reasons, materials having a low content of In 2 O 3, a low raw material cost, and a low environmental burden on resources have been required.
【0005】そこで本発明の目的は、資源環境負荷の高
いIn2O3の含有量を低く抑えることができ、室温付近
の温度で容易に作製することができ、低抵抗かつ光学吸
収端が紫外域にあり、青色透過性に優れた新規な透明導
電体材料及びその製造方法、さらには、そのような透明
導電体材料を用いた電極を提供することにある。Accordingly, an object of the present invention is to reduce the content of In 2 O 3 , which has a high environmental load on resources, to easily produce the material at a temperature near room temperature, to have a low resistance and an optical absorption edge having an ultraviolet absorption edge. Another object of the present invention is to provide a novel transparent conductor material having excellent blue transmittance and a method for producing the same, and an electrode using such a transparent conductor material.
【0006】本発明者らは、亜鉛-インジウム系酸化物
であって、所定量のアルミニウム又はガリウムを含む酸
化物が、室温付近の温度で容易に作製することができ、
低抵抗かつ光学吸収端が紫外域にあり、青色透過性に優
れていることを見いだして本発明を完成した。The present inventors have found that a zinc-indium oxide containing a predetermined amount of aluminum or gallium can be easily produced at a temperature near room temperature.
The inventors have found that the present invention has low resistance, has an optical absorption edge in the ultraviolet region, and has excellent blue transmittance, and has completed the present invention.
【0007】尚、特開平7-235219号公報には、亜鉛-イ
ンジウム系酸化物からなる透明導電膜が設けられた導電
性透明基材が開示されている。この透明導電膜は、主要
カチオン元素としてインジウム(In)および亜鉛(Z
n)を含有する非晶質酸化物からなり、原子比In/
(In+Zn)が0.8〜0.9の範囲内である。さら
に、この酸化物は、第3元素として、アルミニウム、ガ
リウム、アンチモンまたはゲルマニウムを含有するこ
と、及びその含有量は、導電性の低下を抑制するため原
子比(全第3元素)/(In+Zn+全第3元素)が
0.2以下であることが記載されている。[0007] JP-A-7-235219 discloses a conductive transparent substrate provided with a transparent conductive film made of a zinc-indium oxide. This transparent conductive film is made of indium (In) and zinc (Z
n) containing an amorphous oxide having an atomic ratio of In /
(In + Zn) is in the range of 0.8 to 0.9. Further, this oxide contains aluminum, gallium, antimony or germanium as the third element, and its content is determined by the atomic ratio (total third element) / (In + Zn + total) in order to suppress a decrease in conductivity. (Third element) is 0.2 or less.
【0008】この公報には、上記酸化物からなる透明導
電膜の吸収端についての記述は無く、光学特性について
は光線透過率のみしか明らかにされていない。即ち、上
記透明導電膜が、どのような光線透過率スペクトルを有
するかは明らかでなく、低抵抗であり、光学吸収端が紫
外域にあり、さらに青色透過性に優れているかは不明で
ある。In this publication, there is no description about the absorption edge of the transparent conductive film made of the oxide, and only the light transmittance of the optical characteristics is disclosed. That is, it is not clear what kind of light transmittance spectrum the transparent conductive film has, it is not clear whether the transparent conductive film has low resistance, has an optical absorption edge in an ultraviolet region, and further has excellent blue transmittance.
【0009】[0009]
【課題を解決するための手段】本発明の物品の第1の態
様は、基材の少なくとも一方の表面の少なくとも一部
に、一般式ZnxMyInzO(x+3y/2+3z/2)(式中、Mはアルミ
ニウム及びガリウムのうち少なくとも一つの元素であ
り、比率x/yが0.2〜12の範囲であり、比率z/yが0.4〜
1.4の範囲にある)で表される非晶質酸化物を含有する
膜を有することを特徴とする。本発明の物品の第2の態
様は、基材の少なくとも一方の表面の少なくとも一部
に、一般式ZnxMyInzO(x+3y/2+3z/2)(式中、Mはアルミ
ニウム及びガリウムのうち少なくとも一つの元素であ
り、比率x/yが0.2〜12の範囲であり、比率z/yが0.4〜
1.4の範囲にある)で表され、かつ陽イオンを注入した
ものである非晶質酸化物を含有する膜を有することを特
徴とする。A first aspect of the article of the present invention In order to achieve the above object, according to at least a portion of at least one surface of a substrate, the general formula Zn x M y In z O ( x + 3y / 2 + 3z / 2) (where M is at least one element of aluminum and gallium, the ratio x / y is in the range of 0.2 to 12, and the ratio z / y is 0.4 to
(In the range of 1.4). A second aspect of the article of the present invention, at least a portion of at least one surface of a substrate, the general formula Zn x M y In z O ( x + 3y / 2 + 3z / 2) ( in the formula, M At least one element of aluminum and gallium, the ratio x / y is in the range of 0.2 to 12, and the ratio z / y is 0.4 to
(In the range of 1.4), and a film containing an amorphous oxide which has been implanted with cations.
【0010】さらに本発明は、上記本発明の物品からな
る電極に関する。The present invention further relates to an electrode comprising the article of the present invention.
【0011】本発明の第1の製造方法は、上記本発明の
第1の態様の物品の製造方法であって、一般式ZnxMyInz
O(x+3y/2+3z/2)(式中、Mはアルミニウム及びガリウム
のうち少なくとも一つの元素であり、比率x/yが0.2〜1
2の範囲であり、比率z/yが0.4〜1.4の範囲にある)で
表される酸化物をターゲットとし、基板温度を室温から
300℃の範囲とし、かつ圧力を1×10-2[Pa]〜10[Pa]の範
囲として、スパッタリング法またはレーザーアブレーシ
ョン法により、酸化物膜を形成することを特徴とする。[0011] The first production method of the present invention is a method of manufacturing an article of the first aspect of the present invention, the general formula Zn x M y In z
O (x + 3y / 2 + 3z / 2) (where M is at least one element of aluminum and gallium, and the ratio x / y is 0.2 to 1
2 in which the ratio z / y is in the range of 0.4 to 1.4).
An oxide film is formed by a sputtering method or a laser ablation method at a temperature of 300 ° C. and a pressure of 1 × 10 −2 [Pa] to 10 [Pa].
【0012】本発明の第2の製造方法は、上記本発明の
第2の態様の物品の製造方法であって、一般式ZnxMyInz
O(x+3y/2+3z/2)(式中、Mはアルミニウム及びガリウム
のうち少なくとも一つの元素であり、比率x/yが0.2〜1
2の範囲であり、比率z/yが0.4〜1.4の範囲にある)で
表される酸化物をターゲットとし、基板温度を室温から
300℃の範囲とし、かつ圧力を1×10-2[Pa]〜10[Pa]の範
囲として、スパッタリング法またはレーザーアブレーシ
ョン法により、酸化物膜を形成し、次いで前記酸化物膜
に陽イオンを注入することを特徴とする。[0012] The second manufacturing method of the present invention is a method of manufacturing an article of the second aspect of the present invention, the general formula Zn x M y In z
O (x + 3y / 2 + 3z / 2) (where M is at least one element of aluminum and gallium, and the ratio x / y is 0.2 to 1
2 in which the ratio z / y is in the range of 0.4 to 1.4).
An oxide film is formed by a sputtering method or a laser ablation method at a temperature of 300 ° C. and a pressure of 1 × 10 −2 [Pa] to 10 [Pa], and then cations are applied to the oxide film. It is characterized by injection.
【0013】[0013]
【発明の実施の態様】本発明の第1の態様の物品 一般式ZnxMyInzO(x+3y/2+3z/2)中、Mはアルミニウム及
びガリウムのいずれか単独であってもよいし、Mはアル
ミニウム及びガリウムが共存してもよい。アルミニウム
及びガリウムが共存する場合、アルミニウムとガリウム
の比率には特に制限はない。但し、アルミニウムの比率
が増えると結晶化温度が高くなる傾向がある。ガリウム
の比率が増えると結晶化温度が低くなる傾向がある。DESCRIPTION OF THE PREFERRED EMBODIMENTSArticle of the first aspect of the invention General formula ZnxMyInzO(x + 3y / 2 + 3z / 2)M is aluminum and
And gallium alone, and M is
Minium and gallium may coexist. aluminum
Aluminum and gallium when gallium and
Is not particularly limited. However, the ratio of aluminum
Increases, the crystallization temperature tends to increase. gallium
Increases, the crystallization temperature tends to decrease.
【0014】比率(x/y)は0.2以上、12以下の範囲で
あり、x/yが0.2未満では原料コストが高くなる。x
/yが12を超えるとZn成分が大きくなりすぎて大気中
で化学的に不安定になる。好ましい比率(x/y)は1
〜10の範囲であり、より好ましくは4〜10の範囲で
ある。比率(z/y)は0.4以上、1.4以下の範囲
であり、z/yが0.4未満ではIn2O3が不足し、電
気伝導性が低下する。z/yが1.4を超えるとGa2
O3成分が不足して青色領域の透明性が低下する。好ま
しい比率(z/y)は0.6以上1.4以下の範囲であ
り、より好ましくは0.8以上1.2以下の範囲であ
る。The ratio (x / y) is in the range of 0.2 or more and 12 or less. When x / y is less than 0.2, the cost of raw materials increases. x
If / y exceeds 12, the Zn component becomes too large and becomes chemically unstable in the atmosphere. The preferred ratio (x / y) is 1
-10, more preferably 4-10. The ratio (z / y) is in the range of 0.4 or more and 1.4 or less. When z / y is less than 0.4, In 2 O 3 becomes insufficient and electric conductivity is reduced. When z / y exceeds 1.4, Ga 2
Insufficient O 3 components reduce the transparency in the blue region. The preferred ratio (z / y) is in the range of 0.6 or more and 1.4 or less, more preferably in the range of 0.8 or more and 1.2 or less.
【0015】さらに本発明の物品において、比率x/(x
+y+z)が0.5以上であることが、原料コストを下げ、環
境負荷を低減するという観点から好ましい。比率x/(x
+y+z)は、好ましくは0.6〜0.9の範囲である。さ
らに本発明の物品が有する膜において、上記酸化物は、
実質的全量が非晶質であることが、透過率及び導電性の
点で好ましいが、透過率及び導電性を損なわない程度
に、結晶質の酸化物を含有することもできる。Further, in the article of the present invention, the ratio x / (x
+ y + z) is preferably 0.5 or more from the viewpoint of reducing raw material costs and reducing environmental load. Ratio x / (x
+ y + z) preferably ranges from 0.6 to 0.9. Further, in the film of the article of the present invention, the oxide,
It is preferable that substantially the entire amount is amorphous in terms of transmittance and conductivity. However, a crystalline oxide may be contained to such an extent that transmittance and conductivity are not impaired.
【0016】本発明の酸化物の導電性は、伝導帯におけ
るキャリア電子の量が所定の範囲にあるときに良好とな
る。そのようなキャリア電子の量は、1×1018/cm
3〜1×1022/cm3の範囲である。また、好ましいキ
ャリア電子の量は、1×1019/cm3〜5×1021/
cm3の範囲である。尚、キャリア電子の量は、例え
ば、ファンデアパウ法電気伝導率測定装置により測定す
ることができる。The conductivity of the oxide of the present invention becomes good when the amount of carrier electrons in the conduction band is within a predetermined range. The amount of such carrier electrons is 1 × 10 18 / cm
It is in the range of 3 to 1 × 10 22 / cm 3 . Further, the preferable amount of carrier electrons is 1 × 10 19 / cm 3 to 5 × 10 21 / cm.
cm 3 . The amount of carrier electrons can be measured by, for example, a van der Pauw electrical conductivity measuring device.
【0017】本発明の第2の態様の物品 本発明の第2の態様の物品において、一般式ZnxMyInzO
(x+3y/2+3z/2)の式中、Zn、M、比率(x/y)及び比
率(z/y)については、前記本発明の第1の態様の物
品と同様である。比率x/(x+y+z)及び非晶質であるこ
とについても、前記本発明の第1の態様の物品の導電性
酸化物と同様である。[0017]Article of the second aspect of the invention In the article according to the second aspect of the present invention, the general formula ZnxMyInzO
(x + 3y / 2 + 3z / 2)In the formula, Zn, M, ratio (x / y) and ratio
About the rate (z / y), the thing of the said 1st aspect of this invention
Same as the product. Ratio x / (x + y + z) and amorphous
And the conductivity of the article of the first aspect of the present invention.
Same as oxide.
【0018】さらに、本発明の第2の態様の物品は、上
記一般式で表される酸化物に、陽イオンを注入したもの
である。本発明の第2の態様の物品では、酸素欠損を導
入すること以外に、陽イオンを注入することによりキャ
リア電子が伝導帯に注入されて、導電性を発現させるこ
とができる。Further, the article according to the second aspect of the present invention is obtained by implanting cations into the oxide represented by the above general formula. In the article according to the second aspect of the present invention, in addition to introducing oxygen vacancies, carrier electrons can be injected into the conduction band by injecting cations, thereby exhibiting conductivity.
【0019】本発明の第2の態様の物品が有する導電性
酸化物に注入される陽イオンは、一般式ZnxMyInzO
(x+3y/2+3z/2)で表される酸化物の結晶構造を破壊する
ことなく、固溶できるものであれば特に制限はない。但
し、イオン半径の小さいイオンの方が結晶格子中に固溶
しやすい傾向があり、イオン半径が大きくなる程、結晶
構造を破壊し易くなる傾向がある。上記のような陽イオ
ンとしては、例えば、H、Li、Be、B、C、Na、
Mg、Al、Si、K、Ca、Sc、Ti、V、Cr、
Mn、Fe、Co、Ni、Cu、Zn、Ga、Ge、
Y、Zr、Nb、Mo、Tc、Ru、Rh、Pd、A
g、Cd、In、Sn、Sb、Cs、Ba、La、C
e、Pr、Nd、Pm、Sm、Eu、Gd、Tb、D
y、Ho、Er、Tm、Yb、Lu、Hf、Ta、W、
Re、Os、Ir、Pt、Au、Hg、Tl、Pb、B
iを挙げることができる。The positive ions implanted into the conductive oxide having the article of the second aspect of the present invention have the general formula Zn x M y In z O
There is no particular limitation as long as it can form a solid solution without destroying the crystal structure of the oxide represented by (x + 3y / 2 + 3z / 2) . However, ions having a small ionic radius tend to form a solid solution in the crystal lattice, and the larger the ionic radius, the more likely the crystal structure is broken. Examples of the above cations include H, Li, Be, B, C, Na,
Mg, Al, Si, K, Ca, Sc, Ti, V, Cr,
Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge,
Y, Zr, Nb, Mo, Tc, Ru, Rh, Pd, A
g, Cd, In, Sn, Sb, Cs, Ba, La, C
e, Pr, Nd, Pm, Sm, Eu, Gd, Tb, D
y, Ho, Er, Tm, Yb, Lu, Hf, Ta, W,
Re, Os, Ir, Pt, Au, Hg, Tl, Pb, B
i.
【0020】本発明の電極 本発明の電極は、上記本発明の第1または第2の態様の
物品を含むものである。本発明の電極における導電層の
膜厚は、電極に要求される光学的特性、伝導性及び用途
等を考慮して適宜決定できる。例えば、液晶パネル用電
極の場合には、下限は約30nmであり、上限は約1μ
mである。但し、酸化物に含まれる元素の種類によって
は、可視領域に一部吸収を有するものもあり、その場合
には、比較的薄い膜が好ましい。また、可視領域にほと
んどまたはまったく吸収を有さないものについては、膜
厚を厚くすることで、より高い伝導性を得ることができ
る。[0020]The electrode of the present invention The electrode of the present invention is the electrode of the first or second aspect of the present invention.
Includes goods. Of the conductive layer in the electrode of the present invention
The film thickness depends on the optical characteristics, conductivity and application required for the electrode.
It can be appropriately determined in consideration of such factors. For example, for LCD panel
For poles, the lower limit is about 30 nm and the upper limit is about 1 μm.
m. However, depending on the type of element contained in the oxide
May have some absorption in the visible region, in which case
Is preferably a relatively thin film. Also, almost
For those that have little or no absorption, use membranes
By increasing the thickness, higher conductivity can be obtained
You.
【0021】透明基板としては、ガラスや樹脂などの透
明な基体を挙げることができる。即ち、ガラス質・高分
子性等にかかわらず、あらゆる透明材料を基板として利
用することができる。また基板形態も平面基板、シー
ト、フィルム等あらゆる形態に対応する。ガラス基板
は、液晶ディスプレイなどに多く用いられる。ガラス基
板には、ソーダ系ガラスと低アルカリガラスがあり、一
般的にはソーダ系ガラスが広く用いられている。但し、
カラーディスプレイや高品質ディスプレイなどには低ア
ルカリガラスが優れている。可視領域における透明性が
高く、平面性の優れたガラスを用いることが好ましい。Examples of the transparent substrate include transparent substrates such as glass and resin. That is, any transparent material can be used as the substrate irrespective of vitreous or polymeric properties. In addition, the form of the substrate corresponds to any form such as a flat substrate, a sheet, and a film. Glass substrates are often used for liquid crystal displays and the like. Glass substrates include soda-based glass and low-alkali glass, and soda-based glass is generally widely used. However,
Low alkali glass is excellent for color displays and high quality displays. It is preferable to use glass having high transparency in the visible region and excellent flatness.
【0022】樹脂基板としては、例えば、ポリエステル
基板、PMMA基板等が挙げられる。樹脂基板は、ガラ
ス基板に比べて、軽量であること、薄いこと、可撓性が
あって形の自由度が高いことなどを生かした多くの用途
が検討されている。例えば、電子写真用フィルム、液晶
ディスプレイ、光メモリ、透明タブレントスイッチ、帯
電防止フィルム、熱線反射フィルム、面発熱フィルムな
どである。液晶ディスプレイには、可視領域における透
明性が高いこと、平面性に優れることの他に、加工性、
耐衝撃性、耐久性、組立プロセスへの適合性などを考慮
して用いることが好ましい。Examples of the resin substrate include a polyester substrate and a PMMA substrate. Many uses of resin substrates, which are lighter, thinner, more flexible and more flexible in shape than glass substrates, are being studied. For example, an electrophotographic film, a liquid crystal display, an optical memory, a transparent lent switch, an antistatic film, a heat ray reflective film, a surface heating film, and the like. Liquid crystal displays have high transparency in the visible region, excellent flatness, processability,
It is preferable to use it in consideration of impact resistance, durability, compatibility with an assembly process, and the like.
【0023】また、本発明の電極は、前記透明基板上に
設けた下地層上に設けることもできる。下地層として
は、カラーフィルター、TFT層、EL発光層、金属
層、半導体層及び絶縁体層などを挙げることができる。
また、下地層は2種以上を併設することもできる。Further, the electrode of the present invention can be provided on a base layer provided on the transparent substrate. Examples of the base layer include a color filter, a TFT layer, an EL light emitting layer, a metal layer, a semiconductor layer, and an insulator layer.
Further, two or more types of underlayers can be provided.
【0024】本発明の電極は、種々の用途に利用するこ
とができる。例えば、液晶ディスプレイ、ELディスプ
レイ及び太陽電池等の電極として好適に用いることがで
きる。液晶ディスプレイにはTFT型、STN型やMI
M型など種々の型があるが、いずれの場合にも透明電極
にはさまれた液晶に電場を加え、液晶の配向方向を制御
して表示する原理を用いている。本発明の電極は、上記
透明電極として用いることができる。例えば、TFT型
のカラー液晶ディスプレイの構造は、バックライト、第
一の偏光板、TFT基板、液晶、カラーフィルター基板
及び第二の偏光板の6つの部分からなる。液晶の配向方
向を制御するためにTFT基板上とカラーフィルター基
板上に透明電極を形成する必要があるが、本発明の透明
電極は上述の方法によりTFT基板上にもカラーフィル
ター基板上にも形成することができる。本発明の透明電
極は、透明性が高くかつ導電性も高いのでTFT基板上
またはカラーフィルター基板上に設ける透明電極として
最適である。The electrode of the present invention can be used for various applications. For example, it can be suitably used as an electrode of a liquid crystal display, an EL display, a solar cell, or the like. For liquid crystal displays, TFT type, STN type and MI
There are various types such as the M type, but in each case, an electric field is applied to the liquid crystal sandwiched between the transparent electrodes, and the principle of displaying by controlling the orientation direction of the liquid crystal is used. The electrode of the present invention can be used as the transparent electrode. For example, the structure of a TFT type color liquid crystal display is composed of a backlight, a first polarizing plate, a TFT substrate, a liquid crystal, a color filter substrate, and a second polarizing plate. It is necessary to form a transparent electrode on the TFT substrate and the color filter substrate in order to control the alignment direction of the liquid crystal. The transparent electrode of the present invention is formed on the TFT substrate and the color filter substrate by the above-described method. can do. Since the transparent electrode of the present invention has high transparency and high conductivity, it is most suitable as a transparent electrode provided on a TFT substrate or a color filter substrate.
【0025】また、本発明の透明電極は、ELディスプ
レイ用電極として用いることもできる。ELディスプレ
イには分散型、ルモセン構造型や二重絶縁構造型などが
あるが、いずれの場合にも透明電極と背面電極の間にE
L発光層を挟み込む基本構造を有し、本発明の電極は、
上記の透明電極として最適である。Further, the transparent electrode of the present invention can be used as an electrode for an EL display. EL displays include a dispersion type, a lumocene structure type and a double insulation structure type, and in each case, an E is provided between the transparent electrode and the back electrode.
The electrode of the present invention has a basic structure sandwiching the L light emitting layer,
It is most suitable as the above transparent electrode.
【0026】本発明の電極は、透明性及び導電性が高い
ことから、太陽電池用電極としても優れている。太陽電
池は、pn接合型、ショットキーバリア型、ヘテロ接合
型、ヘテロフェイス接合型やpin型などに分類される
が、いずれの場合にも透明電極と背面電極の間に半導体
や絶縁体を挟み込む基本構造を有する。太陽電池は、半
導体界面の光起電力効果を利用して、光エネルギーを電
気に変換する素子であるので、なるべく広いスペクトル
範囲にわたって光を半導体界面に導くことが必要であ
り、透明電極の透明性は高くなくてはならない。また、
太陽電池の透明電極は半導体界面に生成した光生成キャ
リアを収集して端子に導き出す機能を持つので、光生成
キャリアをなるべく有効に収集するためには透明電極の
導電性が高くなくてはならない。本発明の透明電極は、
450nmより短波長の光を含む、可視領域全域の広い
スペクトル範囲にわたって光を半導体界面に導くことが
できる上に導電性が高いので太陽電池用の電極として優
れている。The electrode of the present invention is excellent as a solar cell electrode because of its high transparency and conductivity. Solar cells are classified into pn junction type, Schottky barrier type, hetero junction type, hetero face junction type, pin type, etc. In any case, a semiconductor or insulator is sandwiched between the transparent electrode and the back electrode. It has a basic structure. Since a solar cell is a device that converts light energy into electricity using the photovoltaic effect of a semiconductor interface, it is necessary to guide light to the semiconductor interface over as wide a spectral range as possible, and the transparency of the transparent electrode Must be high. Also,
A transparent electrode of a solar cell has a function of collecting photogenerated carriers generated at a semiconductor interface and guiding the generated carriers to a terminal. Therefore, in order to collect photogenerated carriers as effectively as possible, the conductivity of the transparent electrode must be high. The transparent electrode of the present invention,
Since light can be guided to the semiconductor interface over a wide spectral range of the entire visible region including light with a wavelength shorter than 450 nm and has high conductivity, it is excellent as an electrode for a solar cell.
【0027】本発明の製造方法 本発明の第1及び第2の製造方法は、それぞれ、上記本
発明の第1及び第2の態様の物品の製造方法である。本
発明の第1の製造方法では、一般式ZnxMyInzO
(x+3y/2+3z/2)(式中、Mはアルミニウム及びガリウムの
うち少なくとも一つの元素であり、比率x/yが0.2〜12
の範囲であり、比率z/yが0.4〜1.4の範囲にある)で表
される酸化物をターゲットとして用いる。本発明の第2
の製造方法では、第1の製造方法と同様に、一般式ZnxM
yInzO(x+ 3y/2+3z/2)(式中、Mはアルミニウム及びガリ
ウムのうち少なくとも一つの元素であり、比率x/yが0.
2〜12の範囲であり、比率z/yが0.4〜1.4の範囲にあ
る)で表される酸化物をターゲットを用いる。[0027]Production method of the present invention The first and second manufacturing methods of the present invention
4 is a method for manufacturing the article according to the first and second aspects of the invention. Book
In the first production method of the invention, the general formula ZnxMyInzO
(x + 3y / 2 + 3z / 2)(Where M is aluminum and gallium
At least one of which has a ratio x / y of 0.2 to 12
And the ratio z / y is in the range of 0.4 to 1.4).
The oxide to be used is used as a target. Second embodiment of the present invention
In the production method of the above, similarly to the first production method, the general formula ZnxM
yInzO(x + 3y / 2 + 3z / 2)(Where M is aluminum and gully
At least one of the elements having a ratio x / y of 0.
2 to 12, and the ratio z / y is in the range of 0.4 to 1.4.
Is used as the target.
【0028】本発明の製造方法では、形成される薄膜の
組成が、ターゲットの密度により変化することは殆どな
い。但し、レーザーパルス照射によるターゲットのダメ
ージを考慮すると、ターゲットとして用いる酸化物は、
相対密度が好ましくは40%以上であり、さらに好ましく
は70%以上である。ターゲットとしては例えば、焼結体
を用いることができる。また、形成される薄膜の組成は
ターゲットとのずれは少なく、多くても5%であることか
ら、ターゲット組成は、所望の薄膜組成と同一とするこ
とができる。但し、必要により、ターゲット組成を変更
することはできる。In the manufacturing method of the present invention, the composition of the formed thin film hardly changes depending on the density of the target. However, considering the damage of the target due to laser pulse irradiation, the oxide used as the target is
The relative density is preferably at least 40%, more preferably at least 70%. For example, a sintered body can be used as the target. In addition, the composition of the thin film to be formed has little deviation from the target and is at most 5%, so that the target composition can be the same as the desired thin film composition. However, the target composition can be changed if necessary.
【0029】ターゲットは、例えば、x/y>1の範囲で
は、ZNの酸化物との混晶焼結体、あるいはZNの酸化物を
整数倍だけ含んだ、ホモロガスの焼結体を用いることが
できる。As the target, for example, in the range of x / y> 1, it is possible to use a mixed crystal sintered body with a ZN oxide or a homologous sintered body containing an integer multiple of the ZN oxide. it can.
【0030】本発明の製造方法では、基板温度を室温か
ら300℃の範囲とし、かつ1×10-2[Pa]〜10[Pa]の圧力範
囲の酸素雰囲気あるいは酸素ラジカル雰囲気中で、スパ
ッタリング法またはレーザーアブレーション法により、
酸化物膜を形成する。スパッタリング法及びレーザーア
ブレーション法においても、基板温度を室温から300℃
の範囲とし、かつ圧力(酸素分圧)を1×10-2[Pa]〜10
[Pa]の範囲とすることで、非晶質の酸化物膜を形成する
ことができる。基板温度は、好ましくは0〜150℃の
範囲であり、かつ圧力は、好ましくは0.01[Pa]〜1
[Pa]の範囲である。In the manufacturing method of the present invention, the sputtering method is performed in an oxygen atmosphere or an oxygen radical atmosphere at a substrate temperature in the range of room temperature to 300 ° C. and a pressure in the range of 1 × 10 -2 [Pa] to 10 [Pa]. Or by laser ablation method,
An oxide film is formed. In the sputtering method and the laser ablation method, the substrate temperature is raised from room temperature to 300 ° C.
And the pressure (oxygen partial pressure) is 1 × 10 -2 [Pa] to 10
When the thickness is in the range of [Pa], an amorphous oxide film can be formed. The substrate temperature is preferably in the range of 0 to 150 ° C., and the pressure is preferably 0.01 [Pa] to 1
It is in the range of [Pa].
【0031】スパッタリング法は、常法により行うこと
ができる。また、レーザーアブレーション法では、薄膜
形成装置内の酸素分圧の制御は、酸素分子を適当なリー
クバルブ等から系内に導入することにより行うことがで
きるが、特に、レーザーアブレーション装置内に設置し
たラジカル銃により行うことが、膜中に含まれる酸素量
を制御しやすいとうい観点から適当である。尚、ラジカ
ル銃とはrfプラズマにより酸素等のガスのラジカル種
を発生させ真空系内に導入する装置である。The sputtering method can be performed by a conventional method. In the laser ablation method, the control of the oxygen partial pressure in the thin film forming apparatus can be performed by introducing oxygen molecules into the system from an appropriate leak valve or the like. The use of a radical gun is appropriate from the viewpoint that the amount of oxygen contained in the film can be easily controlled. The radical gun is a device that generates radical species of gas such as oxygen by rf plasma and introduces the radical species into a vacuum system.
【0032】本発明の製造方法のレーザーアブレーショ
ン法に用いるレーザーとしては、紫外域から赤外域のい
ずれの波長、すなわち0.19〜11μm 、望ましくは0.19〜
0.3μm が可能であり、連続発振又はパルス発振のいず
れの方式を採用することができる。レーザー照射時のレ
ーザー強度は、0.0001〜1000J/ cm2・パルス、望ましく
は0.1〜100J/cm2・パルスである。The laser used in the laser ablation method of the production method of the present invention may be any wavelength from the ultraviolet region to the infrared region, that is, 0.19 to 11 μm, preferably 0.19 to 11 μm.
0.3 μm is possible, and either continuous oscillation or pulse oscillation can be employed. Laser intensity at the time of laser irradiation, 0.0001~1000J / cm 2 · pulse, and desirably 0.1~100J / cm 2 · pulse.
【0033】第2の態様の製造方法においては、上記方
法により形成した酸化物膜に陽イオンを注入する。陽イ
オンを注入することによりキャリア電子が伝導帯に注入
されて、導電性を発現させることができる。陽イオン注
入れるイオンは前述の通りである。In the manufacturing method of the second embodiment, cations are implanted into the oxide film formed by the above method. By injecting cations, carrier electrons are injected into the conduction band, so that conductivity can be exhibited. The ions that can be implanted with cations are as described above.
【0034】本発明の製造方法においては、例えば、タ
ーゲットとしてIn:Ga:Zn=1:1:1の焼結体を用いた場合、
6.2×10-3[Ωcm]の薄膜を容易に得ることができる。こ
の場合、高導電性の主因は非晶質物質にも関わらず移動
度が10以上と高い値を示すことによる。また、ターゲッ
トとしてZn成分を増加させたホモロガスIGZO InGaO3(Zn
O)m(m:2以上の整数)の焼結体を用いた場合、4. 3×10-3
[Ωcm]の抵抗率を有する薄膜を容易に得ることができ
る。この理由はキャリア濃度が指数関数的増大傾向を示
すのに対し、移動度がほとんど変化しないことに起因す
る。In the manufacturing method of the present invention, for example, when a sintered body of In: Ga: Zn = 1: 1: 1 is used as a target,
A thin film of 6.2 × 10 −3 [Ωcm] can be easily obtained. In this case, the main cause of the high conductivity is that the mobility shows a high value of 10 or more in spite of the amorphous substance. In addition, a homologous IGZO InGaO 3 (Zn
O) When a sintered body of m (m: an integer of 2 or more) is used, 4.3 × 10 -3
A thin film having a resistivity of [Ωcm] can be easily obtained. The reason for this is that the carrier concentration shows an exponential increase trend, while the mobility hardly changes.
【0035】更に低抵抗化を望む場合は、成膜後に低温
(300℃以下が望ましい)でガス還元法あるいはイオン
注入法を用いることでキャリア密度を上げることによ
り、導電性を向上させることができる。更にターゲット
の組成を変える置換ドーピング効果を利用して、キャリ
ア密度を向上してもよい。If it is desired to further reduce the resistance, the conductivity can be improved by increasing the carrier density by using a gas reduction method or an ion implantation method at a low temperature (preferably 300 ° C. or less) after the film formation. . Further, the carrier density may be improved by utilizing the substitution doping effect of changing the composition of the target.
【0036】[0036]
【発明の効果】本発明の物品は、材料中のIn2O3含
有量が少ないので材料コストが低く、環境負荷が小さ
く、かつ可視光透過率が85%以上であり、かつ吸収短波
長が385nmであることから、白黒画面でもカラー画面で
も膜厚を厚くすることで低抵抗化を図ることが可能であ
る。また、膜を構成する材料の結晶化温度が400℃以上
と高いため、通常の使用温度範囲では、安定な非晶質性
を維持し、抵抗率の変動がないという利点がある。安定
な酸化物であることから耐環境性に優れており、野外で
使用する太陽電池用の透明電極として利用できる。The article of the present invention has a low content of In 2 O 3 in the material, so that the material cost is low, the environmental load is small, the visible light transmittance is 85% or more, and the absorption short wavelength is low. Since the thickness is 385 nm, the resistance can be reduced by increasing the film thickness of both a monochrome screen and a color screen. Further, since the crystallization temperature of the material constituting the film is as high as 400 ° C. or more, there is an advantage that the amorphous property is maintained and the resistivity does not fluctuate in a normal use temperature range. Since it is a stable oxide, it has excellent environmental resistance and can be used as a transparent electrode for solar cells used outdoors.
【0037】また、室温程度の温度での成膜で還元・ア
ニール操作なしに導電性を発現するので、生産効率も高
く、装置も簡便で済み生産コストを低減することができ
る。In addition, since the film is formed at a temperature around room temperature and exhibits conductivity without a reduction / annealing operation, the production efficiency is high, the apparatus is simple and the production cost can be reduced.
【0038】特に、本発明の物品は、優れた電気伝導性
と青色領域を含む可視光透過性を兼ね備えており、有用
な透明電極としてのポテンシャルを持つことから、ディ
スプレイや太陽電池用の電極として利用することができ
る。また、成膜温度を室温付近とすることができるの
で、生産効率が高い。さらに、材料の結晶化温度は高
く、耐環境性にも優れる。In particular, the article of the present invention has both excellent electric conductivity and visible light transmittance including a blue region, and has a potential as a useful transparent electrode, and therefore, is useful as an electrode for a display or a solar cell. Can be used. Further, since the film formation temperature can be set at around room temperature, the production efficiency is high. Further, the crystallization temperature of the material is high and the environment resistance is excellent.
【0039】[0039]
【実施例】本実施例の条件は以下のとおりである。 光源:KrFレーザー励起によるPLD(エネルギー密度4J/cm2) ターゲットはIn:Ga:Zn=1:1:1の焼結体 QZ基板使用 ガス導入 O2 5-40CCM (Pt=7.9×10-2〜1.4 [Pa]) 酸素ラジカル 印加電力 0−150W 抵抗率 6.2×10-3 [Ωcm] キャリア濃度 8.5×1019[/cm3] 移動度 15 [cm/Vs] ターゲットはIn:Ga:Zn=1:1:4の焼結体(ホモロガスInGaO3(ZnO)m m:整数 ) QZ、PMMA基板使用 ガス導入 O2 5-40CCM (Pt=7.9×10-2〜1.4 [Pa]) 抵抗率 4.3×10-3 [Ωcm] キャリア濃度 2.5×1020[/cm3] 移動度 5.8 [cm/Vs]EXAMPLE The conditions of this example are as follows. Light source: PLD by KrF laser excitation (energy density 4J / cm 2 ) Target: In: Ga: Zn = 1: 1: 1 sintered body QZ substrate used Gas introduction O 2 5-40CCM (Pt = 7.9 × 10 -2 ~ 1.4 [Pa]) Oxygen radical applied power 0-150W Resistivity 6.2 × 10 -3 [Ωcm] Carrier concentration 8.5 × 10 19 [/ cm 3 ] Mobility 15 [cm / Vs] Target: In: Ga: Zn = 1: 1: 4 sintered body (Homologous gas InGaO 3 (ZnO) mm : integer) QZ, PMMA substrate used Gas introduction O 2 5-40CCM (Pt = 7.9 × 10 -2 to 1.4 [Pa]) Resistivity 4.3 × 10 -3 [Ωcm] Carrier concentration 2.5 × 10 20 [/ cm 3 ] Mobility 5.8 [cm / Vs]
【0040】1.ターゲットの作成 In2O3、Ga2O3、ZnOの各粉末を、含有金属の比率がそれ
ぞれ1になるように秤量した。秤量した粉末を、遊星ボ
ールミル装置で湿式混合。1000℃で5時間仮焼した後、
再び遊星ボールミルで解砕処理した。この粉体を一軸加
圧で直径20mmの円板状に成形の後CIPをかけた。大気
下、1550℃で2時間焼成して焼結体を得た。XRDによりIn
GaZnO4で表される酸化物が生成していることを確認し
た。1. Preparation of Target Each powder of In 2 O 3 , Ga 2 O 3 , and ZnO was weighed such that the ratio of the contained metals became 1. The weighed powder is wet-mixed with a planetary ball mill. After calcining at 1000 ℃ for 5 hours,
It was crushed again by a planetary ball mill. This powder was formed into a disc having a diameter of 20 mm by uniaxial pressing and then subjected to CIP. The sintered body was obtained by firing at 1550 ° C. for 2 hours in the atmosphere. In by XRD
It was confirmed that an oxide represented by GaZnO 4 was generated.
【0041】ホモロガスInGaO3(ZnO)mの場合は、In
2O3、Ga2O3、ZnOの各粉末を、含有金属の比率が1:1:m(m
は2以上の整数) となるように秤量した。秤量した粉末
を、遊星ボールミル装置で湿式混合。1000℃で5時間仮
焼した後、再び遊星ボールミルで解砕処理した。この粉
体を一軸加圧で直径20mmの円板状に成形の後CIPをかけ
た。大気下、1550℃で2時間焼成して焼結体を得た。XRD
によりそれぞれのm値に対応したInGaO3(ZnO)mで表され
る酸化物が生成していることを確認した。In the case of homologous InGaO 3 (ZnO) m ,
2 O 3 , Ga 2 O 3 , each powder of ZnO, the ratio of the contained metal is 1: 1: m (m
Is an integer of 2 or more). The weighed powder is wet-mixed with a planetary ball mill. After calcining at 1000 ° C. for 5 hours, the mixture was again crushed by a planetary ball mill. This powder was formed into a disc having a diameter of 20 mm by uniaxial pressing and then subjected to CIP. The sintered body was obtained by firing at 1550 ° C. for 2 hours in the atmosphere. XRD
As a result, it was confirmed that an oxide represented by InGaO 3 (ZnO) m corresponding to each m value was generated.
【0042】2.成膜 以下に実施例としてレーザーアブレーション法を用いる
成膜法を示す。 実施例1 上で作成した焼結体のうち、In:Ga:Zn=1:1:1の焼結体の
表面を研磨し、金属Inでインコネル製のホルダーに固定
した。これを日本真空(株)製レーザーアブレーション
装置に固定し、自転させている表面上にラムダフィジッ
ク社製KrFエキシマレーザー光を4J/cm2のエネルギー密
度、パルス間隔5Hzで照射し、プルームをたてた。チャ
ンバー中の雰囲気はO2ガスを15 - 25CCM流し、全圧を0.
8− 1.0[Pa]とした。ターゲットから30mm直上に10mm角
で厚さ0.5mmの石英ガラス基板を設置し、膜厚が均等と
なるように自転させながら30分プルーム中に曝すことに
より、約300nmの薄膜を得た。組成比は蛍光X線法により
得た。膜が均一な非晶質であることはXRDより確認した
(図1)。吸収端は試料の透過及び反射スペクトルから
光学定数を計算することから求めた。電気特性はファン
デアパウ法によるHall効果測定より求めた。2. Film Formation A film formation method using a laser ablation method will be described below as an example. Example 1 Among the sintered bodies prepared above, the surface of the sintered body of In: Ga: Zn = 1: 1: 1 was polished and fixed to a holder made of Inconel with metal In. This was fixed to a laser ablation device manufactured by Japan Vacuum Co., Ltd., and a KrF excimer laser beam manufactured by Lambda Physics Co., Ltd. was irradiated onto the rotating surface at an energy density of 4 J / cm 2 and a pulse interval of 5 Hz to form a plume. Was. The atmosphere in the chamber is O 2 gas flowing at 15-25 CCM, the total pressure is 0.
8-1.0 [Pa] was set. A 10 mm square, 0.5 mm thick quartz glass substrate was placed 30 mm directly above the target, and was exposed to the plume for 30 minutes while rotating so that the film thickness became uniform, thereby obtaining a thin film of about 300 nm. The composition ratio was obtained by a fluorescent X-ray method. XRD confirmed that the film was uniform and amorphous (FIG. 1). The absorption edge was determined by calculating the optical constant from the transmission and reflection spectra of the sample. The electrical characteristics were obtained by measuring the Hall effect by the van der Pauw method.
【0043】[0043]
【表1】 [Table 1]
【0044】実施例2 実施例1と同条件で成膜基板に10mm角で厚さ1.0mmのア
クリル基板を用いることにより、IGZOの非晶質薄膜を得
た。Example 2 An amorphous IGZO thin film was obtained by using a 10 mm square, 1.0 mm thick acrylic substrate as a film-forming substrate under the same conditions as in Example 1.
【0045】[0045]
【表2】 [Table 2]
【0046】実施例3 実施例1と同様にチャンバー雰囲気をO2ガス5-20[CCM]
流し、ラジカルガンを用いてRF電力50Wかけることによ
り酸素ラジカルを発生させ、全圧を0.2− 0.4[Pa]とし
た。Example 3 As in Example 1, the chamber atmosphere was changed to O 2 gas 5-20 [CCM].
Oxygen radicals were generated by flowing and applying RF power of 50 W using a radical gun, and the total pressure was adjusted to 0.2 to 0.4 [Pa].
【0047】[0047]
【表3】 [Table 3]
【0048】実施例4 上で作成した焼結体のうち、In:Ga:Zn=1:1:4の焼結体の
表面を研磨し、金属Inでインコネル製のホルダーに固定
した。これを日本真空(株)製レーザーアブレーション
装置に固定し、自転させている表面上にラムダフィジッ
ク社製KrFエキシマレーザー光を4J/cm2のエネルギー密
度、パルス間隔5Hzで照射し、プルームをたてた。チャ
ンバー中の雰囲気はO2ガスを15 - 25CCM流し、全圧を0.
8− 1.0[Pa]とした。ターゲットから 30mm直上に10mm角
で厚さ0.5mmの石英ガラス基板を設置し、膜厚が均等と
なるように自転させながら30分プルーム中に曝すことに
より、約300nmの薄膜を得た。組成比は蛍光X線法により
得た。膜が均一な非晶質であることはXRDより確認し
た。吸収端は試料の透過及び反射スペクトルから光学定
数を計算することから求めた。電気特性はファンデアパ
ウ法によるHall効果測定より求めた。Example 4 Among the sintered bodies prepared above, the surface of the sintered body of In: Ga: Zn = 1: 1: 4 was polished and fixed to a holder made of Inconel with metal In. This was fixed to a laser ablation device manufactured by Japan Vacuum Co., Ltd., and a KrF excimer laser beam manufactured by Lambda Physics Co., Ltd. was irradiated onto the rotating surface at an energy density of 4 J / cm 2 and a pulse interval of 5 Hz to form a plume. Was. The atmosphere in the chamber is O 2 gas flowing at 15-25 CCM, the total pressure is 0.
8-1.0 [Pa] was set. A 10 mm square quartz glass substrate having a thickness of 0.5 mm was placed 30 mm directly above the target, and exposed to the plume for 30 minutes while rotating so that the film thickness became uniform, thereby obtaining a thin film of about 300 nm. The composition ratio was obtained by a fluorescent X-ray method. It was confirmed by XRD that the film was uniform and amorphous. The absorption edge was determined by calculating the optical constant from the transmission and reflection spectra of the sample. The electrical characteristics were obtained by measuring the Hall effect by the van der Pauw method.
【0049】[0049]
【表4】 [Table 4]
【図1】 InGaZnO4で表される酸化物が生成しているこ
とを確認するXRDの結果。FIG. 1 is a result of XRD confirming that an oxide represented by InGaZnO 4 is generated.
【手続補正書】[Procedure amendment]
【提出日】平成10年10月2日(1998.10.
2)[Submission date] October 2, 1998 (1998.10.
2)
【手続補正1】[Procedure amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】発明の名称[Correction target item name] Name of invention
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【発明の名称】 透明導電性酸化物薄膜を有する物品
及びその製造方法An article having a transparent conductive oxide thin film and a method for producing the same
───────────────────────────────────────────────────── フロントページの続き (72)発明者 細野 秀雄 神奈川県横浜市長津田町4259 東京工業大 学応用セラミックス研究所内 (72)発明者 川副 博司 神奈川県横浜市長津田町4259 東京工業大 学応用セラミックス研究所内 Fターム(参考) 2H092 HA04 MA05 MA23 MA30 NA25 PA01 5G307 FA01 FA02 FB01 FC09 FC10 5G323 BA02 BB05 BB06 BC02 BC03 ──────────────────────────────────────────────────の Continuing on the front page (72) Inventor Hideo Hosono 4259 Nagatsutacho, Yokohama City, Kanagawa Prefecture Inside the Tokyo Institute of Technology Applied Ceramics Research Laboratory (72) Inventor Hiroshi Kawasoe 4259 Nagatsutacho, Yokohama City, Kanagawa Prefecture Tokyo Institute of Technology Applied Ceramics Research In-house F-term (reference) 2H092 HA04 MA05 MA23 MA30 NA25 PA01 5G307 FA01 FA02 FB01 FC09 FC10 5G323 BA02 BB05 BB06 BC02 BC03
Claims (14)
も一部に、一般式ZnxMyIn zO(x+3y/2+3z/2)(式中、Mは
アルミニウム及びガリウムのうち少なくとも一つの元素
であり、比率x/yが0.2〜12の範囲であり、比率z/yが
0.4〜1.4の範囲にある)で表される非晶質酸化物を含有
する膜を有することを特徴とする物品。Claims: 1. At least one surface of a substrate
Some of the general formula ZnxMyIn zO(x + 3y / 2 + 3z / 2)(Where M is
At least one element of aluminum and gallium
And the ratio x / y is in the range of 0.2 to 12, and the ratio z / y is
(Between 0.4 and 1.4)
An article characterized in that it has a film to be formed.
も一部に、一般式ZnxMyIn zO(x+3y/2+3z/2)(式中、Mは
アルミニウム及びガリウムのうち少なくとも一つの元素
であり、比率x/yが0.2〜12の範囲であり、比率z/yが
0.4〜1.4の範囲にある)で表され、かつ陽イオンを注入
したものである非晶質酸化物を含有する膜を有すること
を特徴とする物品。2. At least one surface of the substrate
Some of the general formula ZnxMyIn zO(x + 3y / 2 + 3z / 2)(Where M is
At least one element of aluminum and gallium
And the ratio x / y is in the range of 0.2 to 12, and the ratio z / y is
0.4 to 1.4) and implanted with cations
Having a film containing an amorphous oxide
Articles characterized by the following.
m3の範囲になるように、酸素欠損量d及び陽イオンの注
入量を選んだ請求項2記載の物品。3. The amount of carrier electrons is 1 × 10 18 to 1 × 10 22 / c.
As the range of m 3, article of claim 2, wherein the selected amount of injected oxygen deficiency d and cations.
項1〜3のいずれか1項に記載の物品。4. The article according to claim 1, wherein the ratio x / (x + y + z) is 0.5 or more.
板またはガラス基板である、請求項1〜4のいずれか一
項に記載の物品。5. The article according to claim 1, wherein the substrate is a polymer substrate, a polymer flexible substrate, or a glass substrate.
高分子からなる、請求項5に記載の物品。6. The article according to claim 5, wherein the substrate comprises a transparent polymer on a film or a sheet.
品からなる電極。7. An electrode comprising the article according to any one of claims 1 to 6.
請求項7に記載の電極。8. The electrode according to claim 7, wherein the conductive layer comprises a homogeneous amorphous oxide film.
求項7または8に記載の電極。9. The electrode according to claim 7, further comprising a base layer between the substrate and the conductive layer.
半導体層及び絶縁層から成る群から選ばれる1または2以
上の層である請求項9記載の電極。10. The electrode according to claim 9, wherein the underlayer is one or more layers selected from the group consisting of a filter layer, a TFT layer, an EL layer semiconductor layer, and an insulating layer.
たは太陽電池に用いられる請求項8〜10のいずれか1
項に記載の電極。11. A liquid crystal display, an EL display or a solar cell for use in any one of claims 8 to 10.
An electrode according to the item.
って、一般式ZnxMyInzO(x+3y/2+3z/2)(式中、Mはアル
ミニウム及びガリウムのうち少なくとも一つの元素であ
り、比率x/yが0.2〜12の範囲であり、比率z/yが0.4〜
1.4の範囲にある)で表される酸化物をターゲットと
し、基板温度を室温から300℃の範囲とし、かつ圧力を1
×10-2[Pa]〜10[Pa]の範囲として、スパッタリング法ま
たはレーザーアブレーション法により、酸化物膜を形成
することを特徴とする方法。12. A method of manufacturing an article of claim 1, formula Zn x M y In z O ( x + 3y / 2 + 3z / 2) ( wherein, M is one of aluminum and gallium At least one element, the ratio x / y is in the range of 0.2 to 12, and the ratio z / y is 0.4 to
1.4), the substrate temperature should be in the range of room temperature to 300 ° C, and the pressure should be 1
A method characterized by forming an oxide film by a sputtering method or a laser ablation method in a range of × 10 -2 [Pa] to 10 [Pa].
って、一般式ZnxMyInzO(x+3y/2+3z/2)(式中、Mはアル
ミニウム及びガリウムのうち少なくとも一つの元素であ
り、比率x/yが0.2〜12の範囲であり、比率z/yが0.4〜
1.4の範囲にある)で表される酸化物をターゲットと
し、基板温度を室温から300℃の範囲とし、かつ圧力を1
×10-2[Pa]〜10[Pa]の範囲として、スパッタリング法ま
たはレーザーアブレーション法により、酸化物膜を形成
し、次いで前記酸化物膜に陽イオンを注入することを特
徴とする方法。13. A method of manufacturing an article of claim 2, general formula Zn x M y In z O ( x + 3y / 2 + 3z / 2) ( wherein, M is one of aluminum and gallium At least one element, the ratio x / y is in the range of 0.2 to 12, and the ratio z / y is 0.4 to
1.4), the substrate temperature should be in the range of room temperature to 300 ° C, and the pressure should be 1
A method characterized by forming an oxide film by a sputtering method or a laser ablation method in a range of × 10 -2 [Pa] to 10 [Pa], and then implanting cations into the oxide film.
処理及び/または還元処理を行う、請求項12または1
3に記載の製造方法。14. A heat treatment and / or reduction treatment at a temperature in the range of 10 to 300 ° C. after film formation.
3. The production method according to 3.
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