KR20050004578A - Method of manufacturing ITO nano powder - Google Patents

Method of manufacturing ITO nano powder Download PDF

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KR20050004578A
KR20050004578A KR1020030044818A KR20030044818A KR20050004578A KR 20050004578 A KR20050004578 A KR 20050004578A KR 1020030044818 A KR1020030044818 A KR 1020030044818A KR 20030044818 A KR20030044818 A KR 20030044818A KR 20050004578 A KR20050004578 A KR 20050004578A
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ito
acetate
organic solvent
producing
powder
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KR100608318B1 (en
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홍성제
한정인
이찬재
김영훈
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전자부품연구원
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00Compounds of tin
    • C01G19/02Oxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G15/00Compounds of gallium, indium or thallium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

PURPOSE: A preparation method of nano-sized indium tin oxide(ITO) powder using colloidal dispersion of In and Sn in organic solvent as a start material is provided, which excludes the washing/neutralizing process for decrease in production process and cost, and lowers preparation temperature. CONSTITUTION: The nano-sized indium tin oxide(ITO) powder is prepared by the following steps of: (S10) preparing each colloidal solution containing In and Sn by separately dissolving indium acetate and tin acetate in organic solvent such as acetone, isopropyl alcohol or ethanol at room temperature, wherein the use of starting materials in the form of acetate, not chloride, reduces cost, process and temperature in the production of ITO powder; (S20) mixing In-solution and Sn-solution in a volume ratio of 85:15 - 95:5, and stirring the mixed solution to vaporize organic solvent; (S30) drying solvent-removed materials at 50-150deg.C for 20-40min to get a composite gel; (S40) thermal treating the composite gel at 250-350deg.C; and (S50) grinding thermal-treated composite and sieving.

Description

아이티오 나노 분말의 제조 방법{Method of manufacturing ITO nano powder}Method of manufacturing ITO nano powder

본 발명은 ITO 나노 분말의 제조 방법에 관한 것으로, 보다 상세하게는 유기물 콜로이드를 사용함으로써, 세척/중화 등 공정을 제거하여 공정 단축 및 단가 낮출 수 있고, Cl-기를 배제함으로써, 공정 수행온도를 낮추고, 공정의 안정성을 향상시키며, 환경 오염 요인을 제거할 수 있는 ITO 나노 분말의 제조 방법에 관한 것이다.The present invention relates to a method for producing ITO nanopowder, and more specifically, by using an organic colloid, it is possible to shorten the process and lower the cost by removing the process, such as washing / neutralization, by removing the Cl - group, to lower the process running temperature In addition, the present invention relates to a method for preparing ITO nanopowders which can improve process stability and remove environmental pollution factors.

최근, IMT-2000 등 이동통신 분야가 괄목할만한 성장을 하고 있다.Recently, the mobile communication field such as IMT-2000 is growing remarkably.

IMT-2000은 동영상 서비스 등 고품위의 서비스가 실현될 것으로 기대된다. 동영상 서비스를 위해 필요한 기능은 여러 가지가 있는데, 그 중 고품질의 표시장치(Display)도 중요한 부분을 차지한다.IMT-2000 is expected to realize high quality service such as video service. There are many functions necessary for video service, and high quality display is an important part.

이러한 표시장치에 ITO막은 투명하여 전극으로 사용되고 있으며, 이 ITO막은 ITO 나노 분말을 증착시키면 형성된다.In such a display device, an ITO film is transparent and is used as an electrode. The ITO film is formed by depositing ITO nanopowders.

특히, ITO 나노 분말은 전술된 표시장치뿐만 아니라 각종 전자소자의 투명전극을 제작하는 증착 재료로서 널리 사용된다.In particular, ITO nanopowder is widely used as a deposition material for manufacturing transparent electrodes of various electronic devices as well as the display device described above.

ITO 나노 분말은 분말의 크기가 작으므로, 증착된 ITO막의 밀도를 증가시키고, 이에 따라 특성이 향상된 전극을 제작할 수 있다.Since the ITO nanopowder has a small powder size, it is possible to increase the density of the deposited ITO film, thereby manufacturing an electrode having improved properties.

이런 ITO 나노 분말의 제조방법은 대부분 습식법으로 제조된다.The manufacturing method of such ITO nanopowder is mostly manufactured by a wet method.

그러므로, 종래의 ITO 나노 분말의 제조방법을 설명하면, 첫 번째 방법은, InCl3, In(NO3)3및 SnCl4, Sn(NO3)4, NH4OH 등을 원료물질로 한 습식 침전법으로 제조한다.Therefore, when the conventional method for producing ITO nanopowders is described, the first method is wet precipitation using InCl 3 , In (NO 3 ) 3 and SnCl 4 , Sn (NO 3 ) 4 , NH 4 OH as raw materials. Manufactured by law.

이 때, 원료 물질이 다량의 염소(Cl) 및 질산(NO3) 성분을 함유하고 있으므로, 처리 공정이 매우 까다롭고 잔존하는 Cl 및 NO3가 입자 및 소자에 미치는 악영향을 제거하기 위해서, Cl 및 NO3제거를 위한 폐수처리 및 600 ~ 700℃ 이상에서 열처리 공정을 한다.At this time, since the raw material contains a large amount of chlorine (Cl) and nitric acid (NO 3 ) components, the treatment process is very demanding and Cl and NO 3 are removed in order to remove the adverse effects of remaining Cl and NO 3 on the particles and the device. Wastewater treatment for NO 3 removal and heat treatment at 600 ~ 700 ℃.

이와 같은, 고온 열처리 공정에서만 분말 입자가 성장한다.The powder particles grow only in this high temperature heat treatment step.

그 결과, 50 ~ 80㎚의 조대한 입도 분포를 갖게 되어 나노 분말로서의 특성, 재현성 및 안정성이 저하할 수 있다.As a result, it has coarse particle size distribution of 50-80 nm, and the characteristic, reproducibility, and stability as a nano powder may fall.

따라서, 이와 같은 고온 열처리 공정을 개선하기 위해서는 저온에서 공정을 진행하고, 또한 ITO 복합체 분말의 균일성 향상 및 저가격화를 위해선 동시 열처리 및 합성법이 필요하다.Therefore, in order to improve such a high temperature heat treatment process, a simultaneous heat treatment and a synthesis method are required to improve the uniformity and lower the cost of the ITO composite powder.

두 번째 방법은 공침법을 이용하여 인듐 주석 산화물 분말을 제조하였다.In the second method, indium tin oxide powder was prepared using the coprecipitation method.

이 방법에선, ITO 나노 분말을 제조하기 위한 원료물질은 In(NO3)3ㆍ7H2O와 SnCl4ㆍ5H2O를 사용하거나 인듐 주석 합금을 HCl에 녹여 사용한다.In this method, the raw materials for producing ITO nanopowders are In (NO 3 ) 3 · 7H 2 O and SnCl 4 · 5H 2 O, or indium tin alloy is dissolved in HCl.

그 후, 두 가지 물질을 섞어 교반하는 과정에서 NH4OH를 첨가하여 pH를 조절하여 인듐-주석 수산화물을 석출한다.Thereafter, in the process of mixing and stirring the two substances, NH 4 OH is added to adjust the pH to precipitate indium-tin hydroxide.

여기서, 석출물은 Cl-이온의 제거를 위해 반복적으로 수세를 실시하고, 600 ~ 700℃의 고온에서 열처리하여 잔량의 유해 이온들을 제거하고 결정상을 완성한다.Here, the precipitate is repeatedly washed with water to remove Cl ions, and heat treated at a high temperature of 600 to 700 ° C. to remove residual ions and complete a crystal phase.

세 번째 방법은 습식법을 이용하여 ITO 나노 분말을 제작하였다.A third method was to prepare ITO nanopowder by using the wet method.

이 방법은 인듐과 주석이 포함되어 있는 Cl-또는 NO3 -용액을 제조 후, 분산제와 NH4OH를 첨가하여 pH를 조절하여 인듐-주석 수산화물을 석출 후, 700℃에서 1시간동안 가열한다.In this method, after preparing a Cl - or NO 3 - solution containing indium and tin, the pH is adjusted by adding a dispersant and NH 4 OH to precipitate indium tin hydroxide, and then heated at 700 ° C. for 1 hour.

여기서, 인듐 주석 용액은 InCl3ㆍ4H2O와 SnCl4을 공침(Coprecipitation, 共沈)시킨다.Here, the indium tin solution co-precipitates InCl 3 · 4H 2 O and SnCl 4 .

그 후, 중화과정 또는 수세 과정을 반복하여 Cl-이온을 제거한 후, 슬러리(Slurry)를 제조, 교반 밀(Agitation mill)을 이용하여 혼합 분쇄한다.Thereafter, the neutralization process or water washing process is repeated to remove Cl ions, and then a slurry is prepared and mixed and ground using an agitation mill.

연이어, 600 ~ 700℃에서 열처리하여 잔량의 유해 이온들을 제거하고 결정을 완성한다.Subsequently, heat treatment is performed at 600 to 700 ° C. to remove residual ions and complete the crystal.

이상과 같이, 종래 기술에 따른 ITO막 제조 방법은 Cl-및 OH-기를 포함한 유독성 폐수 및 유해 가스가 발생하게 되는데, 환경 오염의 방지를 위해 폐수를 모아 처리하고, 발생한 유해 가스를 물에 용해하여 폐수로 만든 후, 이를 기존에 모인 폐수와 함께 처리해야 한다.As described above, the ITO membrane manufacturing method according to the prior art generates toxic wastewater and harmful gases including Cl and OH groups. The waste water is collected and treated to prevent environmental pollution, and the generated harmful gases are dissolved in water. After it is made of waste water, it must be disposed of together with the existing waste water.

이 과정에서 엄청난 양의 폐수가 발생하게 되고, 이러한 폐수를 처리하기 위한 비용이 많이 소요되는 문제점이 발생된다.In this process, a huge amount of wastewater is generated, and a costly problem of treating such wastewater is generated.

또한, 600 ~ 700℃의 고온 열처리 공정을 사용하기 때문에 입도가 10 ~ 80 nm으로 불균일하고 매우 조대한 분말이 함께 섞이는 문제점이 발생된다.In addition, since the high temperature heat treatment process of 600 ~ 700 ℃ is used, there is a problem that the particle size is non-uniform and very coarse powder mixed with 10 ~ 80 nm.

한편, 한국 공개 특허(1991-15498호)에는 아세트산 염을 열분해시켜 ITO 나노분말을 제조하였는데, 이는 염을 그대로 열분해 하는 과정에서 입자간 뭉침 및 이로 인한 입자 조대화가 발생되는 단점이 있다.On the other hand, Korean Laid-Open Patent (1991-15498) prepared an ITO nanopowder by pyrolyzing the acetic acid salt, which has the disadvantage of agglomeration between particles and coarse grains in the process of pyrolyzing the salt as it is.

그리고, 일본 특허 출원 번호 'JP 1992-360973호'에는 전기분해법을 이용하여 ITO 분말을 제조하였는데, 이 경우 제조량에 한계가 있고, 특히 비양론적 화합물 분말이 생성되므로, 고온의 열처리가 필요하고 이로 인해 분말 입자가 성장하여 공정이 불안정한 단점이 있다.In addition, Japanese Patent Application No. JP 1992-360973 prepared ITO powder by using an electrolysis method. In this case, there is a limit in the amount of production, in particular, because aprotic compound powder is produced, and therefore, a high temperature heat treatment is required, There is a disadvantage in that the powder particles grow and the process is unstable.

또한, 미국 특허 'US 7,894,798호'에는 챔버내에서 플라즈마에 의한 반응을 이용하여 ITO 입자를 생성하였는데, 챔버 크기 및 용량 문제로 생산에 한계가 있고, 제조 단가가 매우 높으며, 플라즈마가 매우 고온이므로 조대한 입자가 생성되는 단점이 있다.In addition, U.S. Pat.No. 7,894,798 produced ITO particles using a reaction by plasma in a chamber, which has limitations in production due to chamber size and capacity issues, high manufacturing costs, and high plasma. There is a disadvantage in that particles are produced.

이에 본 발명은 상기한 바와 같은 문제점을 해결하기 위하여 안출된 것으로, 유기물 콜로이드를 사용함으로써, 세척/중화 등 공정을 제거하여 공정 단축 및 단가 낮출 수 있고, Cl-기를 배제함으로써, 공정 수행온도를 낮추고, 공정의 안정성을 향상시키며, 환경 오염 요인을 제거할 수 있는 ITO 나노 분말의 제조 방법을 제공하는 데 그 목적이 있다.Accordingly, the present invention has been made to solve the above problems, by using an organic colloid, it is possible to shorten the process and lower the cost by removing the process, such as washing / neutralization, by removing the Cl - group, lowering the process running temperature It is an object of the present invention to provide a method for preparing ITO nanopowders that can improve the stability of a process and remove environmental pollution factors.

상기한 본 발명의 목적들을 달성하기 위한 바람직한 양태(樣態)는, In과 Sn이 각각 포함된 유기 용액들을 만드는 제 1 단계와;A preferred aspect for achieving the above object of the present invention is a first step of making organic solutions each containing In and Sn;

상기 In과 Sn이 각각 포함된 유기 용액들을 섞은 후, 유기 용매가 증발되도록 교반하는 제 2 단계와;A second step of mixing the organic solutions each containing In and Sn, and then stirring the organic solvent to evaporate;

상기 제 2 단계 후에, 유기 용매가 증발된 물질을 건조시켜 겔화된 복합화합물을 형성하는 제 3 단계와;After the second step, a third step of drying the material from which the organic solvent is evaporated to form a gelled complex compound;

상기 건조되어 겔화된 복합화합물을 열처리하는 제 4 단계와;A fourth step of heat treating the dried and gelled composite compound;

상기 열처리된 복합화합물을 분쇄하여 IT0 나노 분말을 생성하는 제 5 단계로 구성된 ITO 나노 분말의 제조 방법이 제공된다.There is provided a method for producing ITO nanopowders comprising a fifth step of pulverizing the heat-treated composite compound to produce IT0 nanopowders.

도 1은 본 발명에 따른 ITO 나노 분말 제조 방법을 도시한 플로우챠트1 is a flow chart showing a method for producing ITO nanopowders according to the present invention

도 2는 본 발명에 따라 열처리 온도에 따라 ITO 나노 분말 입자의 비표면적을 도시한 그래프Figure 2 is a graph showing the specific surface area of ITO nanopowder particles according to the heat treatment temperature according to the present invention

도 3은 본 발명에 따른 제조 공정으로 생성된 ITO 나노 분말을 촬영한 사진도Figure 3 is a photograph of the ITO nano powder produced by the manufacturing process according to the present invention

도 4는 본 발명에 따른 제조 공정으로 생성된 ITO 나노 분말의 결정성을 측정한 그래프Figure 4 is a graph measuring the crystallinity of the ITO nano powder produced by the manufacturing process according to the present invention

<도면의 주요부분에 대한 부호의 설명><Description of the symbols for the main parts of the drawings>

10 : IT0 나노 분말10: IT0 Nano Powder

이하, 첨부된 도면을 참조하여 본 발명의 바람직한 실시예를 설명하면 다음과 같다.Hereinafter, exemplary embodiments of the present invention will be described with reference to the accompanying drawings.

도 1은 본 발명에 따른 ITO 나조 분말 제조 방법을 도시한 플로우챠트로서, 먼저, In과 Sn이 각각 포함된 유기 용액들을 만든다.(S10단계)1 is a flowchart illustrating a method for preparing ITO nazo powder according to the present invention. First, organic solutions containing In and Sn, respectively, are prepared.

이 때, 상기 S10단계는, In과 Sn이 각각 포함된 콜로이드 형태의 모물질 약품을 각각 유기 용매에 상온에서 용해하여 유기용액을 만드는 것이 바람직하다.At this time, in step S10, it is preferable to dissolve the colloidal parent material drug containing In and Sn, respectively, at room temperature in an organic solvent to make an organic solution.

그 후, In과 Sn이 각각 포함된 유기 용액들을 섞은 후, 유기 용매가 증발되도록 교반하고(S20단계), 상기 S20단계 후에, 유기 용매가 증발된 물질을 건조시켜 겔화된 복합화합물을 형성한다.(S30단계)Thereafter, after mixing the organic solutions each containing In and Sn, and stirred to evaporate the organic solvent (step S20), after the step S20, the organic solvent evaporated material is dried to form a gelled complex compound. (Step S30)

이 때, 상기 건조는 50 ~ 150℃의 범위내에서 20 ~ 40분동안 건조시키는 것이 바람직하다.At this time, the drying is preferably dried for 20 to 40 minutes in the range of 50 ~ 150 ℃.

그리고, 상기 In과 Sn이 각각 포함된 유기 용액들의 혼합 부피 비율은, In 아세테이트 : Sn 아세테이트 = 85:15 ~ 95:5인 것이 바람직하다.In addition, the mixing volume ratio of the In and Sn-containing organic solutions, respectively, is preferably In acetate: Sn acetate = 85:15 ~ 95: 5.

연이어, 상기 건조되어 겔화된 복합화합물을 250 ~ 350℃ 범위내에서 열처리한다.(S40단계)Subsequently, the dried and gelled composite compound is heat-treated within the range of 250 ~ 350 ℃ (S40 step).

상기 열처리를 250 ~ 350℃ 범위내에서 수행하는 것은 종래 기술에 따른 열처리보다는 상대적으로 저온에서 열처리하는 것이다.Performing the heat treatment within the range of 250 ~ 350 ℃ is a heat treatment at a relatively low temperature than the heat treatment according to the prior art.

계속하여, 상기 열처리된 복합화합물을 분쇄하여 IT0 나노 분말을 생성한다.(S50단계)Subsequently, the heat-treated composite compound is pulverized to produce an IT0 nanopowder.

여기서, ITO 나노 분말을 생성하는 것은, 상기 열처리된 복합화합물을 사발에 넣고 분쇄하여, 미세한 체(Sieve)로 걸러서 ITO 나노 분말을 생성하는 것이 바람직하다.Here, to produce the ITO nanopowder, it is preferable to put the heat-treated composite compound in a bowl and pulverize, to filter the fine sieve to produce the ITO nanopowder.

상기 S30단계와 S40단계 사이에, 상기 S30단계에서 건조된 복합화합물을 분쇄하는 공정이 더 구비되는 것이 바람직하다.Between the step S30 and S40, it is preferable that the step of grinding the complex compound dried in step S30 is further provided.

또한, 상기 In과 Sn이 각각 포함된 콜로이드 형태의 모물질 약품은 In 아세테이트(Acetate)와 Sn 아세테이트이며, 상기 유기용매는 아세톤, 이소프로필 알콜(IPA, Iso propyl alcohol), 에탄올과 메탄올 중 선택된 어느 하나 인 것이 바람직하다.In addition, the parent drug of the colloidal form containing the In and Sn, respectively is In acetate (Acetate) and Sn acetate, the organic solvent is any one selected from acetone, isopropyl alcohol (IPA, Iso propyl alcohol), ethanol and methanol It is preferable to be one.

도 2는 본 발명에 따라 열처리 온도에 따라 ITO 나노 분말 입자의 비표면적을 도시한 그래프로서, 본 발명에 따른 ITO 나노 분말 제조 공정 중, 열처리 공정에서 열처리 온도를 달리하여 ITO 나노 분말 입자의 비표면적을 측정한 것이다.Figure 2 is a graph showing the specific surface area of the ITO nano powder particles according to the heat treatment temperature according to the present invention, the specific surface area of the ITO nano powder particles by varying the heat treatment temperature in the heat treatment step of the ITO nano powder manufacturing process according to the present invention Is measured.

참고로, 상기 ITO 나노 분말의 입자의 비표면적은 클수록 입자의 크기가 작은 것이고, 입자의 비표면적이 작을수록 입자의 크기가 큰 것이다.For reference, the larger the specific surface area of the particles of the ITO nanopowder, the smaller the particle size, and the smaller the specific surface area of the particle, the larger the particle size.

그러므로, 도 2의 그래프를 참조하면, 본 발명의 제조공정을 수행하면서, 약 300℃에서 열처리를 수행하였을 경우, 입자의 비표면적은 크고, 열처리 온도를 증가할수록 입자의 비표면적은 작아진다.Therefore, referring to the graph of FIG. 2, when the heat treatment is performed at about 300 ° C. while performing the manufacturing process of the present invention, the specific surface area of the particles is large, and the specific surface area of the particles decreases as the heat treatment temperature is increased.

결국, 입자의 비표면적이 큰, 즉, 입자의 크기가 작은 열처리 온도는 약 300℃임을 알 수 있다.As a result, it can be seen that the heat treatment temperature having a large specific surface area of the particles, that is, having a small particle size is about 300 ° C.

따라서, 전술된 바와 같이, 본 발명에서는 250 ~ 350℃ 내에서 열처리를 수행한다.Therefore, as described above, the present invention performs the heat treatment within 250 ~ 350 ℃.

도 3은 본 발명에 따른 제조 공정으로 생성된 ITO 나노 분말을 촬영한 사진도로서, 도면의 '10'는 ITO 나노 분말이고, 그 직격은 대략 5㎚정도임을 알 수 있다.3 is a photographic view of the ITO nano-powder produced by the manufacturing process according to the present invention, '10' of the figure is ITO nano-powder, it can be seen that the direct line is about 5nm.

그러므로, 본 발명에 따른 ITO 나노 분말 제조 방법으로 생성된 ITO 나노 분말은 나노 단위의 분말을 생성할 수 있는 것이다.Therefore, ITO nanopowders produced by the method for producing ITO nanopowders according to the present invention are those capable of producing powders in nano units.

도 4는 본 발명에 따른 제조 공정으로 생성된 ITO 나노 분말의 결정성을 측정한 그래프로서, 그래프의 X축은 회절 각도( 2θ)이고, Y축은 강도(Intensity)이다.Figure 4 is a graph measuring the crystallinity of the ITO nano-powder produced by the manufacturing process according to the present invention, the X-axis of the graph is the diffraction angle (2θ), Y-axis is the intensity (Intensity).

도 4에 도시된 바와 같이, 제조 공정으로 생성된 ITO 나노 분말은 30.5( 2θ )에서 (222) 결정방향의 큰 피크치가 측정되었고, 36.7( 2θ )에서 (400) 결정방향의 피크치가 측정되었으며, 50.9( 2θ )에서 (440) 결정방향의 피크치가 측정되었으므로, 생성된 ITO 나노 분말의 결정성은 우수한 것임을 알 수 있다.As shown in FIG. 4, the ITO nanopowder produced by the manufacturing process had a large peak value in the (222) crystal direction at 30.5 (2θ) and a peak value in the (400) crystal direction at 36.7 (2θ). Since the peak value of the (440) crystal direction was measured at 50.9 (2θ), it can be seen that the crystallinity of the produced ITO nanopowder is excellent.

<본 발명의 실시예><Example of this invention>

1. 200㎖의 IPA에 9.48g In 아세테이트(Acetate)와 1.18g Sn 아세테이트를 각각 첨가하여 용해 후 두 용액을 합친다.1. After dissolving 9.48g In Acetate and 1.18g Sn Acetate in 200ml IPA, combine the two solutions.

2. 합쳐진 용액을 상온에서 교반하면서 유기용매를 증발시킨다.2. Evaporate the organic solvent while stirring the combined solution at room temperature.

3. 100℃에서 30분간 건조하고, 건조된 물질을 회수하여 1차 분산시킨다.3. Dry at 100 ° C. for 30 minutes, recover the dried material and disperse first.

4. 상기 1차 분산된 분말을 전기로에서 300℃의 온도로 저온 열처리하여 유기물을 제거한다.4. The first dispersed powder is subjected to low temperature heat treatment at a temperature of 300 ° C. in an electric furnace to remove organic matter.

5. 저온 열처리된 분말을 막자 사발에 넣고 균일하게 분쇄하여, 미세한 sieve로 균일하게 2차 분산시킨다.5. Pour low-temperature heat-treated powder into a mortar and pestle and grind it uniformly to disperse uniformly into fine sieve.

<종래 기술의 비교예><Comparative example of the prior art>

1. 200㎖의 D.I. water에 7.17g In 염화물(Chloride) 및 0.75g Sn 염화물을 각각 첨가하여, 용해 후 두 용액을 합친다.1. 200 ml of D.I. 7.17 g In Chloride and 0.75 g Sn chloride are added to the water, respectively, and the two solutions are combined after dissolution.

2. 합쳐진 용액을 교반하면서 소량의 NH4OH를 첨가하여 In(OH)3및 Sn(OH)4침전 분말을 만든다.2. Add a small amount of NH 4 OH while stirring the combined solutions to form In (OH) 3 and Sn (OH) 4 precipitate powders.

3. 침전 분말을 용액과 분리하여 회수 후 물로 씻어내는 수세공정을 수 ~ 수십 차례 반복하여 잔류 염화기를 제거한다.3. Separate the precipitated powder from the solution and remove the residual chloride by repeating the washing process several to several tens of times.

4. 분말을 회수하여 100℃로 가열하여 수분을 증발시킨다.4. Recover the powder and heat it to 100 ° C to evaporate the moisture.

5. 증발이 완료된 물질을 후 다시 튜브 전기로에서 700℃의 온도로 고온 열처리하여 Cl-기를 완전히 제거한다.5. The evaporated material is then heat-treated again at a temperature of 700 ° C. in a tube furnace to completely remove Cl groups.

여기서, 전기로 내부는 질소 또는 산소 분위기를 유지해야 하고, 증발되는 Cl-기는 물에 녹여 폐수 처리할 수 있도록, 튜브 전기로 끝과 물이 담긴 삼각 플라스크를 호스로 연결되어 있어야 한다.Here, the inside of the electric furnace must maintain a nitrogen or oxygen atmosphere, and the evaporated Cl group must be connected to the end of the tube electric furnace and a conical flask containing water by a hose so that the waste water can be treated.

6. 열처리된 분말을 막자 사발에 넣고 균일하게 분쇄하여, 미세한 체(Sieve)로 균일하게 분산시킨다.6. Put the heat treated powder in a mortar and pestle, and grind it uniformly, and disperse it evenly into a fine sieve.

이상 상술한 바와 같이, 본 발명은 유기물 콜로이드를 사용함으로써, 세척/중화 등 공정을 제거하여 공정 단축 및 단가 낮출 수 있고, Cl-기를 배제함으로써, 공정 수행온도를 낮추고, 공정의 안정성을 향상시키며, 환경 오염 요인을 제거할 수 있는 효과가 있다.As described above, the present invention, by using the organic colloid, it is possible to shorten the process and lower the cost by removing the process, such as washing / neutralization, by removing the Cl - group, to lower the process performance temperature, improve the stability of the process, It is effective to remove environmental pollution factors.

또한, 본 발명은 공정 수행 온도를 낮춤으로써, IT0 나노 분말 입자를 초미세화할 수 있는 효과가 있다.In addition, the present invention has the effect of ultra-fine ITO nanoparticles by lowering the process temperature.

본 발명은 구체적인 예에 대해서만 상세히 설명되었지만 본 발명의 기술사상 범위 내에서 다양한 변형 및 수정이 가능함은 당업자에게 있어서 명백한 것이며, 이러한 변형 및 수정이 첨부된 특허청구범위에 속함은 당연한 것이다.Although the invention has been described in detail only with respect to specific examples, it will be apparent to those skilled in the art that various modifications and variations are possible within the spirit of the invention, and such modifications and variations belong to the appended claims.

Claims (9)

In과 Sn이 각각 포함된 유기 용액들을 만드는 제 1 단계와;A first step of making organic solutions each containing In and Sn; 상기 In과 Sn이 각각 포함된 유기 용액들을 섞은 후, 유기 용매가 증발되도록 교반하는 제 2 단계와;A second step of mixing the organic solutions each containing In and Sn, and then stirring the organic solvent to evaporate; 상기 제 2 단계 후에, 유기 용매가 증발된 물질을 건조시켜 겔화된 복합화합물을 형성하는 제 3 단계와;After the second step, a third step of drying the material from which the organic solvent is evaporated to form a gelled complex compound; 상기 건조되어 겔화된 복합화합물을 열처리하는 제 4 단계와;A fourth step of heat treating the dried and gelled composite compound; 상기 열처리된 복합화합물을 분쇄하여 IT0 나노 분말을 생성하는 제 5 단계로 구성된 ITO 나노 분말의 제조 방법.A method for producing ITO nanopowders comprising a fifth step of grinding the heat-treated composite compound to produce an IT0 nanopowder. 제 1 항에 있어서,The method of claim 1, 상기 제 1 단계는,The first step is, In과 Sn이 각각 포함된 콜로이드 형태의 모물질 약품을 각각 유기 용매에 상온에서 용해하여 유기용액을 만드는 것을 특징으로 하는 ITO 나노 분말의 제조 방법.A method of producing ITO nanopowders, characterized in that an organic solution is prepared by dissolving a colloidal parent material of In and Sn, respectively, in an organic solvent at room temperature. 제 2 항에 있어서,The method of claim 2, 상기 In과 Sn이 각각 포함된 콜로이드 형태의 모물질 약품은,The parent material drug of the colloidal form containing each of In and Sn, In 아세테이트(Acetate)와 Sn 아세테이트인 것을 특징으로 하는 ITO 나노 분말의 제조 방법.Method for producing ITO nanopowders, characterized in that In acetate (Acetate) and Sn acetate. 제 3 항에 있어서,The method of claim 3, wherein 상기 In과 Sn이 각각 포함된 유기 용액들의 혼합 부피 비율은,The mixing volume ratio of the organic solutions containing In and Sn, respectively, In 아세테이트 : Sn 아세테이트 = 85:15 ~ 95:5인 것을 특징으로 하는 ITO 나노 분말의 제조 방법.In acetate: Sn acetate = 85:15 ~ 95: 5 A method for producing ITO nano powder, characterized in that. 제 3 항에 있어서,The method of claim 3, wherein 상기 유기용매는,The organic solvent, 아세톤, 이소프로필 알콜(IPA, Iso propyl alcohol), 에탄올과 메탄올 중 선택된 어느 하나 인 것을 특징으로 하는 ITO 나노 분말의 제조 방법.Acetone, isopropyl alcohol (IPA, Iso propyl alcohol), a method for producing ITO nano powder, characterized in that any one selected from ethanol and methanol. 제 1 항에 있어서,The method of claim 1, 상기 제 5 단계에서 ITO 나노 분말을 생성하는 것은,In the fifth step of producing the ITO nano powder, 상기 열처리된 복합화합물을 사발에 넣고 분쇄하여, 미세한 체(Sieve)로 걸러서 ITO 나노 분말을 생성하는 것을 특징으로 하는 ITO 나노 분말의 제조 방법.Method of producing ITO nanopowder, characterized in that to put the heat-treated complex compound in a bowl and pulverized, to filter the fine sieve (Sieve) to produce ITO nanopowder. 제 1 항에 있어서,The method of claim 1, 상기 제 3 단계와 제 4 단계 사이에,Between the third and fourth steps, 상기 제 3 단계에서 건조된 복합화합물을 분쇄하는 공정이 더 구비되는 것을특징으로 하는 ITO 나노 분말의 제조 방법.Method for producing ITO nanopowders characterized in that the step of further grinding the complex compound dried in the third step. 제 1 항에 있어서The method of claim 1 상기 제 3 단계의 건조는,The drying of the third step is, 50 ~ 150℃의 범위내에서 20 ~ 40분 동안 건조시키는 것을 특징으로 하는 ITO 나노 분말의 제조 방법.Method for producing ITO nanopowder, characterized in that for 20 to 40 minutes to dry in the range of 50 ~ 150 ℃. 제 1 항 내지 제 8 항 중 어느 한 항에 있어서,The method according to any one of claims 1 to 8, 상기 열처리는,The heat treatment is, 250 ~ 350℃ 범위내에서 수행하는 것을 특징으로 하는 ITO 나노 분말의 제조 방법.Method for producing ITO nanopowder, characterized in that performed in the range of 250 ~ 350 ℃.
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US9273073B2 (en) 2011-06-28 2016-03-01 3M Innovative Properties Company Tin dioxide nanopartcles and method for making the same
CN113649589A (en) * 2021-08-18 2021-11-16 昆明理工大学 Preparation method of spherical indium tin alloy nano powder based on organic system

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KR100663714B1 (en) * 2005-12-29 2007-01-03 성균관대학교산학협력단 Method of forming a composition for synthesizing ito and method of patterning ito synthesized from said composition
CN100427192C (en) * 2006-04-04 2008-10-22 张文知 An addictive-free, long-term stable, high-solid, transparent and conductive nano crystalline water dispersion and method for preparing same
US9273073B2 (en) 2011-06-28 2016-03-01 3M Innovative Properties Company Tin dioxide nanopartcles and method for making the same
CN113649589A (en) * 2021-08-18 2021-11-16 昆明理工大学 Preparation method of spherical indium tin alloy nano powder based on organic system

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