KR20120072237A - Composition of in-ga-si-zn based oxide - Google Patents
Composition of in-ga-si-zn based oxide Download PDFInfo
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- KR20120072237A KR20120072237A KR1020100134074A KR20100134074A KR20120072237A KR 20120072237 A KR20120072237 A KR 20120072237A KR 1020100134074 A KR1020100134074 A KR 1020100134074A KR 20100134074 A KR20100134074 A KR 20100134074A KR 20120072237 A KR20120072237 A KR 20120072237A
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Abstract
Description
본 발명은 투명도전성 박막 제조용 조성물에 관한 것으로, 더 구체적으로는 유리, 세라믹, 또는 플라스틱 등의 소재 표면에 코팅되어 투명성 및 도전성이 우수한 박막으로 사용될 수 있는 투명도전성 산화물에 관한 것이다.The present invention relates to a composition for manufacturing a transparent conductive thin film, and more particularly, to a transparent conductive oxide which can be used as a thin film having excellent transparency and conductivity by being coated on a material surface such as glass, ceramic, or plastic.
투명도전성 박막은 전기전도도가 높고, 가시광선 투과율이 높아 액정디스플레이(LCD), 플라즈마디스플레이(PDP), 유기발광디스플레(OLED), 터치패널 등에 가장 많이 사용되고 있으며, 이외에도 전자파 흡수 및 차폐, 발열체, 태양전지, 정전기방지 등에 광범위하게 사용되고 있다. Transparent conductive thin films are most commonly used in liquid crystal displays (LCDs), plasma displays (PDPs), organic light emitting displays (OLEDs), and touch panels because they have high electrical conductivity and high visible light transmittance. Widely used in battery, antistatic and the like.
투명도전성 박막을 제조하기 위해 가장 많이 쓰이고 있는 재료로는, 산화인듐 (In2O3)에 산화주석(SnO2)이 3 ~ 10 중량%(wt%)로 도핑된 인듐-주석 산화물(ITO)이 있다. ITO 막을 제조하는 공지된 방법들로는, 분사(spray), 진공기화(vacuum evaporation), 스퍼터링(sputtering) 및 이온플레이팅(ion plating) 등이 있으며 상업적으로는 스퍼터링 방법이 가장 많이 쓰이고 있다. In order to prepare a transparent conductive thin film, indium tin oxide (ITO) doped with indium oxide (In 2 O 3 ) and tin oxide (SnO 2 ) 3 to 10 wt% (wt%). There is this. Known methods for producing ITO membranes include spray, vacuum evaporation, sputtering and ion plating, and sputtering methods are most commonly used commercially.
상기 방법들로 제조된 ITO 막은 투명성이나 도전성이 우수할 뿐만 아니라 에칭성이 우수하고 기판과의 밀착성도 좋아 현재 가장 많이 사용되고 있다. 하지만, 인듐은 희소자원일 뿐 아니라 생체에 유해하며, ITO 타겟을 스퍼터링할 때 노듈(nodule) 발생의 원인이 되기도 한다. 이와 같은 자원의 희소성, 인체유해성, 스퍼터링에서의 노듈 발생 등의 문제 때문에 ITO 중의 인듐을 저감시키거나 ITO를 대체할 수 있는 대체 물질에 대한 연구가 필요하다. The ITO film prepared by the above methods is not only excellent in transparency and conductivity, but also has excellent etching property and good adhesion to the substrate. However, indium is not only a scarce resource but also harmful to a living body, and may also cause nodule when sputtering an ITO target. Due to such scarcity of resources, human hazards, and nodule generation in sputtering, research on alternative materials that can reduce indium in ITO or replace ITO is needed.
이러한 필요성에 대응한 새로운 투명전극용 소재에 대한 연구는, 불소 또는 안티모니가 도핑된 산화주석(FTO, ATO), 알루미늄 또는 갈륨 또는 인듐이 도핑된 산화아연(AZO, GZO, IZO) 등에 대하여 진행되고 있다.In order to meet these needs, research on new transparent electrode materials has been carried out on tin oxide (FTO, ATO) doped with fluorine or antimony, zinc oxide (AZO, GZO, IZO) doped with aluminum or gallium or indium. It is becoming.
그러나, 이들 대체 재료들 또한 고가의 비용이 소모되는 등의 문제가 있으며, 따라서 보다 경제적인 방법으로 고투명도 및 고전도도를 갖는 투명도전성 박막을 안정적으로 얻을 수 있는 방안에 대한 연구가 절실히 요구되고 있다.However, these alternative materials also suffer from problems such as high cost, and thus, there is an urgent need for research on a method of stably obtaining a transparent conductive thin film having high transparency and high conductivity in a more economical manner. .
본 발명은 상술한 바와 같은 종래기술의 문제점을 해결하기 위한 것으로서, 인듐-갈륨-실리콘-아연을 포함하는 산화물에 있어서 인듐, 갈륨, 실리콘 및 아연의 원자비를 적정 범위로 제어함으로써 보다 경제적으로 고투명도 및 고전도도 특성을 갖는 산화물계 조성물을 제공하는 것을 목적으로 한다.The present invention is to solve the problems of the prior art as described above, more economically high transparency by controlling the atomic ratio of indium, gallium, silicon and zinc in an appropriate range in the oxide containing indium-gallium-silicon-zinc An object of the present invention is to provide an oxide-based composition having degree and high conductivity characteristics.
본 발명에 따른 인듐-갈륨-실리콘-아연 산화물계 조성물은, 인듐(In), 갈륨(Ga), 실리콘(Si), 아연(Zn) 및 산소(O)를 포함하고, (In+Ga)/(In+Ga+Si+Zn)의 원자비가 15at.% 이상 및 85at.% 이하의 비율로 함유되어 있는 것을 특징으로 한다.Indium-gallium-silicon-zinc oxide-based composition according to the present invention comprises indium (In), gallium (Ga), silicon (Si), zinc (Zn) and oxygen (O), and (In + Ga) / An atomic ratio of (In + Ga + Si + Zn) is contained at a ratio of 15 at% or more and 85 at.% Or less.
또한, 본 발명은, 인듐(In), 갈륨(Ga), 실리콘(Si), 아연(Zn) 및 산소(O)를포함하고, (In+Ga)/(In+Ga+Si+Zn)의 원자비가 15at.% 이상 및 85at.% 이하의 비율로 함유되어 있는 인듐-갈륨-실리콘-아연 산화물계 조성물로 형성된 투명도전성막을 포함하는 전자기기를 제공한다. 여기서, 투명도전성막의 두께는 0Å 초과 및 5,000Å 이하로 형성될 수 있다. 그리고, 전자기기는 액정디스플레이, 플라즈마디스플레이, 유기발광 디스플레이, 터치패널 등과 같은 디스플레이 장치일 수 있다.In addition, the present invention includes indium (In), gallium (Ga), silicon (Si), zinc (Zn), and oxygen (O), and includes (In + Ga) / (In + Ga + Si + Zn). An electronic device including a transparent conductive film formed of an indium-gallium-silicon-zinc oxide-based composition containing an atomic ratio of 15 at% or more and 85 at% or less is provided. Herein, the thickness of the transparent conductive film may be formed to be greater than 0 mm and less than 5,000 mm. The electronic device may be a display device such as a liquid crystal display, a plasma display, an organic light emitting display, a touch panel, or the like.
앞에서 설명한 바와 같이, 본 발명의 인듐-갈륨-실리콘-아연 산화물계 조성물을 이용하여 제조한 박막은 가시광선 투과율이 80%이상이고 전기전도도가 우수하며 기판과의 접합성이 좋기 때문에, LCD, PDP, OLED 및 터치패널 등에 전극으로 사용될 수 있을 뿐만 아니라 전자파 차폐재, 발열체, 태양전지 등에도 사용될 수 있기 때문에 산업적으로 가치가 매우 높다.
As described above, the thin film prepared by using the indium-gallium-silicon-zinc oxide-based composition of the present invention has a visible light transmittance of 80% or more, has excellent electrical conductivity, and has good adhesion with a substrate. Not only can be used as an electrode for OLED and touch panel, but also can be used for electromagnetic wave shielding material, heating element, solar cell, etc., so the industrial value is very high.
도 1은 본 발명에 따른 인듐-갈륨-실리콘-아연 산화물로 제조된 투명도전상막(실시예 2)에 대하여 주사형전자현미경으로 얻은 이미지이다.
도 2는 본 발명에 따른 인듐-갈륨-실리콘-아연 산화물로 제조된 투명도전상막(실시예 7)에 대하여 주사형전자현미경으로 얻은 이미지이다.
도 3은 본 발명에 따른 인듐-갈륨-실리콘-아연 산화물로 제조된 투명도전상막(실시예 2)의 단면에 대한 주사형전자현미경 이미지이다.1 is an image obtained with a scanning electron microscope for a transparent conductive film (Example 2) made of indium-gallium-silicon-zinc oxide according to the present invention.
2 is an image obtained by a scanning electron microscope for a transparent conductive film (Example 7) made of indium-gallium-silicon-zinc oxide according to the present invention.
3 is a scanning electron microscope image of a cross section of a transparent conductive film (Example 2) made of indium-gallium-silicon-zinc oxide according to the present invention.
본 발명에 따른 인듐-갈륨-실리콘-아연 산화물계 조성물은, 인듐(In), 갈륨(Ga), 실리콘(Si), 아연(Zn) 및 산소(O)를포함하고, (In+Ga)/(In+Ga+Si+Zn)의 원자비가 15at.% 이상 및 85at.% 이하의 비율로 함유되어 있는 것을 특징으로 한다.Indium-gallium-silicon-zinc oxide-based composition according to the present invention comprises indium (In), gallium (Ga), silicon (Si), zinc (Zn) and oxygen (O), and (In + Ga) / An atomic ratio of (In + Ga + Si + Zn) is contained at a ratio of 15 at% or more and 85 at.% Or less.
이러한, 본 발명에 따른 인듐-갈륨-실리콘-아연 산화물계 조성물을 이용하여 투명도전성막을 제조할 수 있는데, 예컨대 In2O3, Ga2O3, SiO2, 그리고 ZnO를 주성분으로 하는 산화물 복합체 제조한 후 이를 스퍼터링하여 투명도전성막을 제조할 수 있다. 여기서, 본 발명에 따른 산화물 복합체는, 예컨대 (1) In2O3, Ga2O3, SiO2, 그리 고ZnO 산화물 분말들을 각각 적당량 천칭한 다음 잘 혼합하여 혼합물을 만드는 단계, (2) 이 혼합물을 금형에 넣고 프레스(press)하여 성형한 후 열처리하여 소결하는 단계 및 (3) 소결된 타겟을 스퍼터링하여 기판에 성막하는 단계를 거쳐 제조할 수 있다. 이하에서는, 본 발명에 따른 실시예를 자세히 설명한다.
Such a transparent conductive film can be prepared using the indium-gallium-silicon-zinc oxide-based composition according to the present invention. For example, an oxide composite based on In 2 O 3 , Ga 2 O 3 , SiO 2 , and ZnO is manufactured. After that, sputtering may be used to prepare a transparent conductive film. Here, in the oxide composite according to the present invention, for example, (1) In 2 O 3 , Ga 2 O 3 , SiO 2 , and an appropriate amount of each of the ZnO oxide powders balance, and then mixed well to form a mixture, (2) The mixture may be prepared by pressing into a mold, forming a mixture, followed by heat treatment and sintering, and (3) sputtering the sintered target to form a film on a substrate. Hereinafter, the embodiment according to the present invention will be described in detail.
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실시예Example
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InIn
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GaGa
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ZnZn
산화물계 조성물 및 투명도전성 물질의 제조 Preparation of Oxide-Based Compositions and Transparent Conductive Materials
[분말혼합조건] 원료분말로서, 산화인듐(In2O3) 분말, 산화갈륨(Ga2O3) 분말, 산화실리콘(SiO2), 그리고 산화아연(ZnO) 분말을 아래 표 1과 같은 원소조성비가 되도록 각각 적당량을 천칭하여 폴레에틸렌제의 포트에 넣고 에탄올을 충분히 채운다. 그 다음, 지르코니아 (ZrO2) 볼(ball)을 이용한 24시간 동안 볼밀링(ball milling) 방법으로 혼합한 후, 이 혼합물을 120℃의 온도로 플레이트 위에서 충분히 저으면서 건조하였다.
[Powder Mixing Conditions] As raw material powders, indium oxide (In 2 O 3 ) powder, gallium oxide (Ga 2 O 3 ) powder, silicon oxide (SiO 2 ), and zinc oxide (ZnO) powder are shown in Table 1 below. Each of the appropriate amounts is added to the composition pot, and the ethanol is sufficiently filled in a pot made of polyethylene. Then, the mixture was mixed by a ball milling method for 24 hours using a zirconia (ZrO 2 ) ball, and then the mixture was dried with sufficient stirring on a plate at a temperature of 120 ° C.
[성형 및 소결조건] 이렇게 건조된 혼합분말을 금형에 넣고, 300Kg/㎠의 압력으로 프레스하여 성형한 다음 대기 중에서 소결하였다. 소결을 위한 승온 속도는 5 ℃/min이었고, 소결은 1400℃에서 6시간 동안 하였다. 이 성형체의 조성분석은 EPMA(전자탐침미세분석기)를 이용하여 수행하였다(각 성분의 원소조성비는 표 1 참조).
[Molding and Sintering Conditions] The dried powder powder thus dried was put into a mold, press-molded at a pressure of 300 Kg / cm 2, and sintered in air. The rate of temperature increase for sintering was 5 ° C./min and sintering was carried out at 1400 ° C. for 6 hours. Composition analysis of the molded body was carried out using an EPMA (electron probe microanalyzer) (see Table 1 for the element composition ratio of each component).
[진공증착조건] 다음으로 진공증착법에 의해 위 소결체를 기판 상에 증착하였다. 여기서, 기판으로는 유리 기판을 사용하였으며, 50W의 RF전력으로 3×10-3 Torr의 가스압 상태에서 수행하였고, 이때 아르콘(Ar)의 가스 유량은 40 sccm이었다. 기판의 온도는 상온에서 수행하였으며, 막 두께는 2,000Å ~ 5,000Å이 되도록 형성하였다.
[Vacuum Deposition Conditions] Next, the above sintered body was deposited on a substrate by a vacuum deposition method. Here, a glass substrate was used as the substrate, and was performed at a gas pressure of 3 × 10 −3 Torr with an RF power of 50 W, wherein a gas flow rate of arcon (Ar) was 40 sccm. The temperature of the substrate was performed at room temperature, and the film thickness was formed to be 2,000 kPa to 5,000 kPa.
[평가조건] 이와 같이 형성된 투명도전성막의 조성을 EPMA를 이용하여 측정하였고, 그 결과를 표 3에 나타내었다. 그리고, 투명도전성막의 전기전도도는 3,000Å 두께의 막에 대해 4포인트 프로브 표면저항 측정기를 이용하여 측정하였다. 또한, 투명도 측정은 3000Å 두께의 막에 대해 550nm에서의 투과율을 측정하였다. 투명도전성막의 물성은 아래 표 4에 나타내었다.
[Evaluation Conditions] The composition of the transparent conductive film thus formed was measured using EPMA, and the results are shown in Table 3. The electrical conductivity of the transparent conductive film was measured using a four-point probe surface resistance meter on a film having a thickness of 3,000 kPa. In addition, the transparency measurement measured the transmittance | permeability at 550 nm with respect to the film of 3000 micrometers thickness. Physical properties of the transparent conductive film are shown in Table 4 below.
구분
division
(In+Ga+Si+Zn)(In + Ga) /
(In + Ga + Si + Zn)
구분
division
(In+Ga+Si+Zn)(In + Ga) /
(In + Ga + Si + Zn)
(550 nm)Transmittance (%)
(550 nm)
(오옴/□)resistance
(Ohm / □)
본 발명에 의해 제조된 유전체 유리에 대해 X-선 회절 분석기와 전자현미경을 이용하여 분석한 결과, 실시예 1~4는 비정질이었고 실시예 5~7은 결정질이었다. 표 4에서 보듯이, 본 발명의 범위에 속하는 인듐-갈륨-실리콘-아연 산화물계 조성물을 이용하여 제조한 투명도전성 박막은 가시광선 투과율이 평균 80% 이상으로 나타났고, 전기전도도 또한 우수함을 확인할 수 있었으며, 아울러 기판과의 접합성도 양호한 것으로 나타났다. 예시적으로, 실시예 2와 실시예 7에 대한 주사형전자현미경 이미지를 각각 도 1과 도 2에 나타내었으며, 특히 실시예 2의 경우 단면 구조를 주사형전자현미경으로 확인한 결과 접합성이 양호함을 볼 수 있었다.
The dielectric glass prepared according to the present invention was analyzed using an X-ray diffraction analyzer and an electron microscope. As a result, Examples 1 to 4 were amorphous and Examples 5 to 7 were crystalline. As shown in Table 4, the transparent conductive thin film prepared by using the indium-gallium-silicon-zinc oxide-based composition belonging to the scope of the present invention exhibited an average visible light transmittance of 80% or more and an excellent electrical conductivity. Moreover, the adhesiveness with the board | substrate also showed favorable. For example, scanning electron microscope images of Examples 2 and 7 are shown in FIGS. 1 and 2, respectively, and in Example 2, the cross-sectional structure of the scanning electron microscope was confirmed by the scanning electron microscope. Could see.
이와 같이, 본 발명에 따른 인듐-갈륨-실리콘-아연 산화물계 조성물로 형성한 투명도전성막은 투명도, 전도도 및 기판과의 접합성이 매우 우수한 것으로 나타났으며 따라서 본 발명에 따른 조성물을 이용하면 보다 경제적으로 고투명도 및 고 전도도 특성을 갖는 투명도전성막을 형성할 수 있다. 본 발명에 따른 조성물은 전자기기, 예컨대, 액정디스플레이, 플라즈마디스플레이, 유기발광 디스플레이, 터치패널 등과 같은 디스플레이 장치에서 투명도전성막으로 이용할 수 있으며, 이외에도 전자파 차폐재, 발열체, 태양전지, 정전기방지장치 등에도 유리하게 사용될 수 있다.
As described above, the transparent conductive film formed of the indium-gallium-silicon-zinc oxide-based composition according to the present invention was found to have excellent transparency, conductivity, and adhesion to the substrate. A transparent conductive film having high transparency and high conductivity characteristics can be formed. The composition according to the present invention can be used as a transparent conductive film in display devices such as electronic devices, for example, liquid crystal displays, plasma displays, organic light emitting displays, touch panels, and the like, in addition to electromagnetic wave shielding materials, heating elements, solar cells, and antistatic devices. It can be used advantageously.
지금까지 본 발명의 바람직한 실시예에 대해 설명하였으나, 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자는 본 발명의 본질적인 특성을 벗어나지 않는 범위 내에서 변형된 형태로 구현할 수 있을 것이다. 그러므로 여기서 설명한 본 발명의 실시예는 한정적인 관점이 아니라 설명적인 관점에서 고려되어야 하고, 본 발명의 범위는 상술한 설명이 아니라 특허청구범위에 나타나 있으며, 그와 동등한 범위 내에 있는 모든 차이점은 본 발명에 포함되는 것으로 해석되어야 한다.While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the invention. Therefore, the embodiments of the present invention described herein are to be considered in descriptive sense only and not for purposes of limitation, and the scope of the present invention is shown in the appended claims rather than the foregoing description, and all differences within the equivalent scope of the present invention Should be interpreted as being included in.
Claims (4)
It contains indium (In), gallium (Ga), silicon (Si), zinc (Zn) and oxygen (O), and the atomic ratio of (In + Ga) / (In + Ga + Si + Zn) is 15 at% or more. And an indium-gallium-silicon-zinc oxide-based composition, which is contained at a ratio of 85 at% or less.
It contains indium (In), gallium (Ga), silicon (Si), zinc (Zn) and oxygen (O), and the atomic ratio of (In + Ga) / (In + Ga + Si + Zn) is 15 at% or more. And a transparent conductive film formed of an indium-gallium-silicon-zinc oxide-based composition, which is contained at a rate of 85 at% or less.
상기 전자기기는 디스플레이 장치인 것을 특징으로 하는 인듐-갈륨-실리콘-아연 산화물계 조성물로 형성된 투명도전성막을 포함하는 전자기기.
The method of claim 2,
The electronic device includes a transparent conductive film formed of an indium-gallium-silicon-zinc oxide-based composition, characterized in that the display device.
상기 투명도전성막의 두께가 0Å 초과 및 5,000Å 이하인 것을 특징으로 하는 전자기기.
The method of claim 2,
And the thickness of the transparent conductive film is greater than 0 mm and less than 5,000 mm.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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US9541784B2 (en) | 2013-08-09 | 2017-01-10 | Samsung Display Co., Ltd. | Liquid crystal display and method for fabricating the same |
KR20190119556A (en) * | 2019-10-08 | 2019-10-22 | 엘지디스플레이 주식회사 | array substrate for liquid crystal display device and fabricating method of the same |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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US9541784B2 (en) | 2013-08-09 | 2017-01-10 | Samsung Display Co., Ltd. | Liquid crystal display and method for fabricating the same |
KR20190119556A (en) * | 2019-10-08 | 2019-10-22 | 엘지디스플레이 주식회사 | array substrate for liquid crystal display device and fabricating method of the same |
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