KR101616881B1 - METHOD FOR MANUFACTURING In-Ga-Zn BASED SPUTTERING TARGET - Google Patents
METHOD FOR MANUFACTURING In-Ga-Zn BASED SPUTTERING TARGET Download PDFInfo
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- KR101616881B1 KR101616881B1 KR1020130164034A KR20130164034A KR101616881B1 KR 101616881 B1 KR101616881 B1 KR 101616881B1 KR 1020130164034 A KR1020130164034 A KR 1020130164034A KR 20130164034 A KR20130164034 A KR 20130164034A KR 101616881 B1 KR101616881 B1 KR 101616881B1
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Abstract
인듐-갈륨-아연계 스퍼터링 타겟 제조 방법이 개시된다. 본 발명에 의한 인듐-갈륨-아연계 스퍼터링 타겟 제조 방법은 인듐 질산염 : 갈륨 질산염 : 아연 질산염 분말을 0.8~1.2 : 0.8~1.2 : 10~20 의 몰비로 준비 하여 1차 분쇄 하는 단계; 1차 분쇄된 분말에 아세톤을 첨가하여 2차 분쇄 하는 단계; 상기 아세톤 용액에 불산을 첨가하여 불화물을 생성 하는 단계; 상기 불화물을 건조하고 소결하는 단계를 포함한다.A method of manufacturing an indium-gallium-zinc-based sputtering target is disclosed. The method for preparing an indium-gallium-zinc-based sputtering target according to the present invention comprises: preparing indium nitrate: gallium nitrate: zinc nitrate powder at a molar ratio of 0.8: 1.2: 0.8-1.2: 10-20; Adding the acetone to the first pulverized powder to perform second pulverization; Adding fluoric acid to the acetone solution to produce a fluoride; And drying and sintering the fluoride.
Description
본 발명은 스퍼터링 타겟 제조방법에 관한 것으로, 보다 구체적으로는 투명전극 물질로 이용되는 인듐-갈륨-아연계 산화물의 스퍼터링 타겟 제조방법에 관한 것이다.The present invention relates to a method for manufacturing a sputtering target, and more particularly, to a method for manufacturing a sputtering target of an indium-gallium-zinc-based oxide used as a transparent electrode material.
최근, 액정 디스플레이나 태양전지 등에는 도전성이고 또한 빛에 대하여 투명한 전극(투명전극)이 사용되고 있다. 이와 같은 성질을 갖는 재료로서는, 예를 들면, In2O3-SnO2(ITO), In2O3-ZnO(IZO), ZnO-Al2O3(AZO) 등의 산화물 재료가 알려져 있다. 이와 같은 재료는 스퍼터링(sputtering)법에 의하여 액정 디스플레이나 태양전지 상에 박막으로서 형성된 후에, 전극으로 패터닝되어, 투명전극이 된다. Recently, electrodes (transparent electrodes), which are conductive and transparent to light, are used for liquid crystal displays, solar cells, and the like. As materials having such properties, for example, oxide materials such as In2O3-SnO2 (ITO), In2O3-ZnO (IZO), and ZnO-Al2O3 (AZO) are known. Such a material is formed as a thin film on a liquid crystal display or a solar cell by a sputtering method, and then is patterned as an electrode to become a transparent electrode.
상기 스퍼터링법은 박막을 형성해야 하는 액정 디스플레이 등의 액정과 스퍼터링 타겟(이하, 타겟이라 한다)을 대향시켜서 배치하고, 이들 사이에서 가스 방전을 발생시켜, 이 가스 방전에 의해 발생한 이온이 타겟의 표면에 부딪혀, 그 충격에 의해 방출된 원자(입자)를 대향하는 기판에 부착시켜서 박막이 형성된다. The sputtering method is a method in which a liquid crystal such as a liquid crystal display for forming a thin film and a sputtering target (hereinafter, referred to as a target) are arranged to face each other and a gas discharge is generated therebetween, And the atoms (particles) emitted by the impact are attached to the opposing substrate to form a thin film.
상기 타겟은 박막(투명전극)이 되는 재료로 형성되고, 투명전극의 특성은 이 타겟의 특성을 반영한다. The target is formed of a material that becomes a thin film (transparent electrode), and the characteristics of the transparent electrode reflect the characteristics of the target.
상기 타겟 중 Indium-tin oxide(ITO)는 인듐 산화물(indium oxide)층에 주석을 도핑한 물질로 오늘날 수많은 액정 디스플레이와 태양 전지 등에 사용되는 소자로서 투명성과 함께 높은 전도성을 가진다.Indium tin oxide (ITO) in the target is a material doped with indium oxide (indium oxide) layer and used for many liquid crystal displays and solar cells today, and has transparency and high conductivity.
그러나, In 은 희유 금속으로써, ITO를 생산 하는데 매우 고가의 비용이 들고 있어, ITO를 대체하기 위한 물질의 개발이 활발하다.However, since In is a rare metal, it is very expensive to produce ITO, and materials for replacing ITO are actively developed.
ITO의 대체 물질로 In-Ga-Zn의 산화물을 혼합한 IGZO계가 주목을 받고 있으나, 이와 같은 3 성분계 이상의 원료를 혼합하여 스퍼터링 타겟을 제조할 때에는 원료를 매우 균일하게 혼합 조절 하여야 최종 박막까지 제조 할 수 있다.An IGZO system in which an oxide of In-Ga-Zn is mixed as a substitute for ITO has attracted attention. However, when the sputtering target is prepared by mixing raw materials of three or more components, it is necessary to prepare the final thin film by controlling the raw materials very uniformly .
공개특허 10-2010-0079320 에서는 이러한 문제를 해결하기 위해 서로 다른 분말을 혼합한 뒤 강한 산성 조건에서 용해를 시키고 이를 다시 염기성 조건으로 변화시켜 금속 다성분계의 수산화염을 만드는 방법을 사용했다. In order to solve such a problem, the method of mixing the different powders, dissolving them under strong acidic conditions, and then changing them to basic conditions, was used to make a metal multi-component hydroxide flame.
이러한 방법은 여러 종류의 금속 이온을 균질하게 섞는 효과를 기대할 수 있으나 강산, 강염기 처리시의 위험성과 추가적인 비용 및 환경문제를 야기할 수 있다. This method can be expected to produce homogeneous mixing of various kinds of metal ions, but it can cause risks and additional costs and environmental problems in the treatment of strong acids and strong bases.
상기의 문제점을 해결하기 위하여 본 발명에서는 강산, 강염기 처리 없이 균일한 스퍼터링 타켓을 제조하는 방법을 제공하고자 한다.In order to solve the above problems, the present invention provides a method for producing a uniform sputtering target without a strong acid or strong base treatment.
본 발명의 일 실시예에 의한 인듐-갈륨-아연계 스퍼터링 타겟 제조 방법은, 인듐 질산염 : 갈륨 질산염 : 아연 질산염 분말을 0.8~1.2 : 0.8~1.2 : 10~20 의 몰비로 준비 하여 1차 분쇄 하는 단계; 1차 분쇄된 분말에 아세톤을 첨가하여 2차 분쇄 하는 단계; 상기 아세톤 용액에 불산을 첨가하여 불화물을 생성 하는 단계; 상기 불화물을 건조하고 소결하는 단계를 포함한다.The method for producing an indium-gallium-zinc-based sputtering target according to an embodiment of the present invention comprises preparing indium nitrate: gallium nitrate: zinc nitrate powder at a molar ratio of 0.8-1.2: 0.8-1.2: 10-20, step; Adding the acetone to the first pulverized powder to perform second pulverization; Adding fluoric acid to the acetone solution to produce a fluoride; And drying and sintering the fluoride.
상기 1차 분쇄 단계는 3~6 시간 수행할 수 있다.The first milling step may be performed for 3 to 6 hours.
상기 불산 : 아세톤은 부피비로 1 : 5~20 으로 첨가될 수 있다.The hydrofluoric acid: acetone may be added in a volume ratio of 1: 5 to 20.
불화물을 생성 하는 단계는 30분 ~ 1시간 수행 할 수 있다.The step of producing the fluoride can be carried out for 30 minutes to 1 hour.
상기 1차 분쇄 및 2차 분쇄 단계는 볼밀(ball mill)을 이용할 수 있다.A ball mill may be used for the primary pulverization and the secondary pulverization.
소결이 완료된 스퍼터링 타겟의 밀도는 5.5~6.5 g/cc 일 수 있다.The density of the sintered sputtering target may be 5.5 to 6.5 g / cc.
본 발명에 의한 인듐-갈륨-아연계 스퍼터링 타겟 제조 방법은 강산, 강염기 처리의 위험성이 없으며, 환경문제의 위험성이 없다.The method for producing an indium-gallium-zinc-based sputtering target according to the present invention has no risk of strong acid and strong base treatment, and there is no risk of environmental problems.
또한, 종래 기술에 의한 인듐-갈륨-아연계 스퍼터링 타겟보다 균일한 혼합에 의한 스퍼터링 타겟의 제조가 가능하다. In addition, it is possible to manufacture a sputtering target by uniformly mixing the indium-gallium-zinc-based sputtering target according to the prior art.
도1은 본 발명의 일 실시예 의한 인듐-갈륨-아연계 스퍼터링 타겟의 SEM사진을 나타낸 도면이다.1 is a SEM photograph of an indium-gallium-zinc-based sputtering target according to an embodiment of the present invention.
본 발명의 이점 및 특징, 그리고 그것들을 달성하는 방법은 상세하게 후술되어 있는 실시예들을 참조하면 명확해질 것이다. 그러나, 본 발명은 이하에서 개시되는 실시예들에 한정되는 것이 아니라 서로 다른 다양한 형태로 구현될 수 있으며, 단지 본 실시예들은 본 발명의 개시가 완전하도록 하고, 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자에게 발명의 범주를 완전하게 알려주기 위해 제공되는 것이며, 본 발명은 청구항의 범주에 의해 정의될 뿐이다.Advantages and features of the present invention and methods of achieving them will become apparent with reference to the embodiments described in detail below. However, it is to be understood that the present invention is not limited to the disclosed embodiments, but may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. It is intended that the disclosure of the present invention be limited only by the terms of the appended claims.
본 발명에 의한 인듐-갈륨-아연계 스퍼터링 타겟의 제조방법은, A method of manufacturing an indium-gallium-zinc-based sputtering target according to the present invention includes:
먼저, 인듐 질산염, 갈륨 질산염, 아연 질산염 분말을 준비하여 1차 분쇄한다. 인듐 질산염 : 갈륨 질산염 : 아연 질산염 분말은 0.8~1.2 : 0.8~1.2 : 10~20 의 몰비 인 것이 바람직 하다.First, indium nitrate, gallium nitrate, and zinc nitrate powder are prepared and firstly ground. It is preferable that the molar ratio of indium nitrate: gallium nitrate: zinc nitrate is 0.8-1.2: 0.8-1.2: 10-20.
아연 질산염의 비율이 20 초과일 경우 최종제품의 전도성이 높지 않으며, 균일한 혼합이 어렵다.When the ratio of zinc nitrate is more than 20, the conductivity of the final product is not high, and uniform mixing is difficult.
상기 1차 분쇄는 볼밀(ball mill)을 사용하여 분쇄 하는 것이 바람직하다.The primary pulverization is preferably performed using a ball mill.
또한 상기 1차 분쇄는 3~6시간 수행 하는 것이 바람직하다.The primary pulverization is preferably carried out for 3 to 6 hours.
상기 1차 분쇄가 완료된 분쇄된 분말에 아세톤을 첨가하여 습식 분쇄법을 이용하여 2차 분쇄 한다. Acetone is added to the pulverized powder that has been subjected to the first pulverization, followed by second pulverization using a wet pulverization method.
이 때 아세톤은 질산염이 충분히 용해 될 수 있도록 과량 첨가 될 수 있다.At this time, acetone can be added in an excess amount so that nitrate can be sufficiently dissolved.
또한 상기 2차 볼밀(ball mill)을 사용하여 분쇄 하는 것이 바람직하다.Further, it is preferable to perform pulverization using the above-mentioned secondary ball mill.
상기 아세톤 용액에 불산을 첨가하고, 첨가된 불산은 아세톤 용액과 반응하여 미세한 불화물 분말을 생성 한다.Hydrofluoric acid is added to the acetone solution, and the added hydrofluoric acid reacts with the acetone solution to produce fine fluoride powder.
이 때 상기 불산 : 아세톤은 부피비로 1 : 5~20 으로 첨가되는 것이 바람직하다.In this case, the amount of the hydrofluoric acid: acetone is preferably 1: 5 to 20 by volume.
상기 아세톤의 비율이 5 미만인 경우 분말의 입도가 커지는 문제점이 생길 수 있으며, 20 초과 인 경우 이 후 공정에서 아세톤을 증발 시키기 힘들다.If the ratio of acetone is less than 5, the particle size of the powder may be increased. If the ratio is more than 20, it is difficult to evaporate acetone in the subsequent step.
또한, 상기 불화물을 생성하는 단계는 30분~1시간 수행 하는 것이 바람직하다.It is preferable that the step of producing the fluoride is performed for 30 minutes to 1 hour.
이후, 아세톤 용액을 증발시킨후 건조하여 불화물 분말을 얻는다. 상기 불화물 분말을 건조하고 소결하여 인듐-갈륨-아연계 스퍼터링 타겟을 제조 한다.Thereafter, the acetone solution is evaporated and dried to obtain a fluoride powder. The fluoride powder is dried and sintered to produce an indium-gallium-zinc-based sputtering target.
완성된 스퍼터링 타겟의 밀도는 5.5~6.5 g/cc 인 것이 바람직하다.
The density of the completed sputtering target is preferably 5.5 to 6.5 g / cc.
[실시예][Example]
인듐 질산염 (Indium nitrate) : 갈륨 질산염 (Gallium nitrate) : 아연 질산염 (Zinc nitrate)의 비율을 몰(mol)비로 1 : 1 : 12로 준비하였다.Indium nitrate: The ratio of gallium nitrate to zinc nitrate was prepared in a molar ratio of 1: 1: 12.
상기 분말을 볼밀 (ball mill)을 이용하여 3시간 동안 1차 분쇄 시킨후,The powder was first pulverized for 3 hours using a ball mill,
아세톤을 과량 첨가하고 2차 분쇄 하였다.Acetone was added in an excess amount, followed by secondary pulverization.
이후, 불산 : 아세톤이 1:10 의 비율로 첨가하여 1시간 동안 불화물을 생성 하였다.Then, fluoric acid: acetone was added at a ratio of 1:10 to produce fluoride for 1 hour.
이렇게 얻어진 불화물 분말을 성형 몰드에 충진한 후 5 ton/cm2 이하의 압력으로 일축성형을 한 뒤 2차로 냉간 정수압 성형을 실시 하였다.The fluoride powder thus obtained was filled in a molding mold, uniaxially molded at a pressure of 5 ton / cm 2 or less, and then subjected to a cold isostatic pressing process.
완성된 성형체를 소결하여 6 g/cc 의 스퍼터링 타겟을 제조 하였다.The finished molded product was sintered to prepare a sputtering target of 6 g / cc.
도 1 은 본 발명의 실시예에 의해 제조된 스퍼터링 타겟의 SEM 사진이다.1 is an SEM photograph of a sputtering target manufactured according to an embodiment of the present invention.
도 1 에서 알 수 있듯, 본 발명에 의하여 제조된 스퍼터링 타겟은 조성의 입도가 1 μm 이내이며, 조성이 균일하게 형성 되었음을 알 수 있다.As can be seen from FIG. 1, it can be seen that the sputtering target prepared according to the present invention has a grain size of 1 μm or less and a uniform composition.
Claims (4)
1차 분쇄된 분말에 아세톤을 첨가하여 2차 분쇄 하는 단계;
상기 아세톤 용액에 불산을 첨가하여 불화물을 생성 하는 단계;
상기 불화물을 건조하고 소결하는 단계를 포함하는;
인듐-갈륨-아연계 스퍼터링 타겟 제조 방법.Preparing indium nitrate: gallium nitrate: zinc nitrate powder at a molar ratio of 0.8-1.2: 0.8-1.2: 10-20;
Adding the acetone to the first pulverized powder to perform second pulverization;
Adding fluoric acid to the acetone solution to produce a fluoride;
Drying and sintering the fluoride;
A method for producing an indium-gallium-zinc-based sputtering target.
상기 1차 분쇄 단계는 3~6 시간 수행하는 인듐-갈륨-아연계 스퍼터링 타겟 제조 방법.The method according to claim 1,
Wherein the primary pulverization step is performed for 3 to 6 hours.
상기 불산 : 아세톤은 부피비로 1 : 5~20 으로 첨가되는 인듐-갈륨-아연계 스퍼터링 타겟 제조 방법.3. The method of claim 2,
Wherein the hydrofluoric acid: acetone is added in a volume ratio of 1: 5 to 20.
소결이 완료된 스퍼터링 타겟의 밀도는 5.5~6.5 g/cc 인 인듐-갈륨-아연계 스퍼터링 타겟 제조 방법.The method of claim 3,
A method for producing an indium-gallium-zinc-based sputtering target, wherein the sintered sputtering target has a density of 5.5 to 6.5 g / cc.
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