KR101429042B1 - Synthetic method of nano-sized powder and manufacturing method of high density and conductibility target with using sn-zn for decreasing indium - Google Patents

Synthetic method of nano-sized powder and manufacturing method of high density and conductibility target with using sn-zn for decreasing indium Download PDF

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KR101429042B1
KR101429042B1 KR1020110117275A KR20110117275A KR101429042B1 KR 101429042 B1 KR101429042 B1 KR 101429042B1 KR 1020110117275 A KR1020110117275 A KR 1020110117275A KR 20110117275 A KR20110117275 A KR 20110117275A KR 101429042 B1 KR101429042 B1 KR 101429042B1
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indium
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최병현
지미정
안용관
김은경
최진훈
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한국세라믹기술원
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00Metallic composition of the powder or its coating
    • B22F2301/30Low melting point metals, i.e. Zn, Pb, Sn, Cd, In, Ga

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Abstract

본 발명은 부탄올과 인듐아세테이트, 아연아세테이트 그리고 주석아세테이트를 반응시켜 인듐산화물에 아연산화물과 주석산화물이 18~ 28.7중량% 고용된 단일 결정상 빅스바이트로 이루어진 인듐산화물을 생성하는 청정공정으로 나노크기 분말을 합성하는 방법과 상기 뭉쳐져 있는 인듐 산화물 분말을 분산제를 이용 분산시킨 후 산소 가압하여 현재의 소결온도 1550℃ 또는 1500℃보다 낮은 1350℃에서 인듐 산화물 타겟을 제조하는 방법에 관한 것이다.
본 발명에 따른 아연과 주석이 인듐에 고용된 인듐 산화물 타겟의 경우 청정공정으로 폐수의 배출이 없게 되었고, 또한 현재 상용 아이티오의 소성보다 150~200℃ 낮은 온도에서 소성이 가능하므로 에너지가 절감될 뿐만 아니라 상대밀도 99.7%의 고밀도 타겟을 제조할 수 있고, 비저항이 5x10-4Ωㆍ㎝으로 전기적 성능도 현 아이티오와 대등한 값을 얻을 수 있었다.
The present invention relates to a process for producing indium oxide consisting of monocrystalline bixbyite having 18 to 28.7 wt% of zinc oxide and tin oxide dissolved in indium oxide by reacting butanol with indium acetate, zinc acetate and tin acetate, And a method for producing an indium oxide target at 1350 占 폚, which is lower than the present sintering temperature of 1550 占 폚 or 1500 占 폚 by oxygen pressurization after dispersing the agglomerated indium oxide powder using a dispersant.
In the case of the indium oxide target in which zinc and tin are dissolved in indium according to the present invention, waste water is not discharged in the cleaning process, and the energy can be reduced because the calcination can be performed at a temperature 150 to 200 ° C lower than that of the conventional a- In addition, a high density target with a relative density of 99.7% can be manufactured, and the resistivity is 5x10 -4 Ω · cm, and the electrical performance is comparable to that of the current ATIO.

Description

청정공정 이용 아연과 주석이 인듐에 고용된 인듐산화물(인듐-아연-주석 산화물)의 나노 분말 합성 방법{SYNTHETIC METHOD OF NANO-SIZED POWDER AND MANUFACTURING METHOD OF HIGH DENSITY AND CONDUCTIBILITY TARGET WITH USING SN-ZN FOR DECREASING INDIUM} METHOD OF NANO-SIZED POWDER AND MANUFACTURING METHOD OF HIGH DENSITY AND CONDUCTIVITY TARGET WITH USING SN-ZN FOR DECREASING USING THE CLEANING PROCESS INDIUM}

본 발명은 주석과 아연을 고용하여 인듐을 저감하는 산화물 조성을 설계하고, 청정공정으로 나노분말을 합성하는 방법과 합성된 나노 응집분말을 잘 분산시켜 고밀도 타겟을 제조하는 청정공정 이용 주석과 아연을 고용한 인듐저감 조성(인듐-아연-주석 산화물)나노 분말합성 및 고전도 고밀도 타켓 제조방법에 관한 것이다.
The present invention relates to a method of preparing an oxide composition for reducing indium by employing tin and zinc, a method for synthesizing nanopowder by a clean process, and a clean process for producing a high-density target by dispersing the synthesized nano- (Indium-zinc-tin oxide) nano powder and a method for manufacturing a high-density high-density target.

인듐-주석산화물인 아이티오(ITO, 인듐산화물 90~95중량%, 주석산화물 5~10중량%)는 주로 평판형 디스플레이에 사용되는 투명전도체로서, 최근 평판형 디스플레이 산업발달과 함께 수요가 급격히 증가하고 있다. 이러한 아이티오의 주성분인 인듐은 몇 년 내에 고갈 위기에 놓여있고, 가격은 고가로 급등할 것이 예측되고 있으며, 아이티오를 재활용 하여도 향후에 이러한 수요를 충당할 수 없게 될 것이다.(ITO, indium oxide 90 to 95 wt%, tin oxide 5 to 10 wt%), which is indium-tin oxide, is a transparent conductor mainly used for a flat panel display. Recently, . Indium, which is the main component of ATIO, is in a crisis of depletion in a few years, prices are expected to surge to high prices, and recycling of Haitio will not be able to meet this demand in the future.

또한, 습식 청정 공정 이용 수십 나노크기 분말 합성은 균일한 소재를 합성하고, 소성온도를 낮추며, 전도성능을 향상시킬 수 있기 때문에 입자크기를 수십 나노크기로 합성하나 필연적으로 뭉침 현상이 발생하여 타겟 제조 시 미세기공이 제거되지 못해 원하는 만큼의 고밀도와 전도성능을 얻을 수 없는 단점이 있다.
In addition, the use of a wet cleaning process enables synthesis of a few tens of nano-sized powders to synthesize homogeneous materials, lowering the firing temperature, and improving the conduction performance, so that the particle size is synthesized to several tens of nanometers, The minute pores can not be removed, so that the desired high density and conduction performance can not be obtained.

따라서, 본 발명의 목적은 인듐산화물양을 18.0~28.7중량% 저감하며, 아이티오 고전도 산화물의 고상합성에서 발생되는 타겟 조성의 불균일성을 해결하고, 소결과정에서의 인듐이나 주석의 휘발을 감소시키기 위해 고상반응 온도보다 200℃이상을 낮출 수 있는 저온화 유도, 습식반응으로 공정상 생성되는 강산이나 강염기에 의한 폐수억제, 합성과정에서의 뭉침 현상 및 소결에서의 저밀도 문제점을 해결하는 것이다.Accordingly, an object of the present invention is to reduce the amount of indium oxide by 18.0 to 28.7% by weight, to solve the non-uniformity of the target composition resulting from the solid-phase synthesis of the high-temperature composite oxide, and to reduce the volatilization of indium and tin during the sintering process This is to solve the problem of low temperature in induction of low temperature which can lower than 200 ℃ than solid phase reaction temperature, suppression of wastewater by strong acid or strong bases produced in process due to wet reaction, aggregation in synthesis process and low density in sintering.

즉, 모물질인 인듐, 주석 및 아연을 아세테이트계 원료로 하고 부탄올을 용매로 사용하여 폐수배출이 없이 합성하여 입자크기를 나노크기로 합성하고, 입자크기 분포가 제어될 수 있게끔 합성 공정을 제어하는 것이며, 이 합성공정에서 분산제로 도데실라민(Dodecylamine)에 하이드록실 프로필 셀룰로오즈(HPC)나 폴리에틸렌글리콜(PEG)을 혼합 첨가하거나 도데시실라민 또는 암모늄폴리메타아크릴레이트 (Ammonium Polymethacrylate)를 단독 첨가하여 나노 입자의 뭉침현상을 제어하는 것이다.In other words, it is possible to synthesize nano-sized particles by synthesizing indium, tin and zinc, which are parent materials, as acetate-based raw materials and butanol as a solvent without wastewater discharge, and control the synthesis process so that the particle size distribution can be controlled In this synthesis process, hydroxylpropyl cellulose (HPC) or polyethylene glycol (PEG) is mixed with dodecylamine as a dispersant or dodecylamine or ammonium polymethacrylate alone is added to the nano- To control the aggregation of the particles.

만약, 입자크기가 수십 나노이지만 뭉침 현상이 발생하면 나노입자의 성능을 발휘하지 못하기 때문이다.If the particle size is tens of nanometers but the aggregation occurs, the performance of the nanoparticles can not be achieved.

또한, 합성분말을 이용 고밀도 타겟을 제조하기 위해 잘 분산된 나노입자를 이용 과립화(granule)한 다음 일축 성형 및 등가압성형 한 후 고온에서 산소 가압 상태에서도 소결하여 고밀도 타겟을 제조 방법에 대해 제공하는 것이다.In order to manufacture a high-density target using a synthetic powder, granules are granulated using well-dispersed nanoparticles, uniaxially or isostatically pressed, and sintered at a high temperature under oxygen pressure to provide a high density target .

즉, 청정공정으로 고전도성을 나타내는 아이티오 대체 (인듐-주석-아연계)전도소재 합성에서도 뭉침 현상이 나타나는 것을 합성 후 적당한 분산제를 첨가하여 뭉침 현상을 제거하고 건조, 하소과정을 거친 분말을 일축 성형 한 후, 등가압 성형하여 산소가압상태에서 소결하면 미세가공이 제거되어 고밀도 타겟으로 제조가 가능하다.
That is, it is known that a clustering phenomenon occurs even in the synthesis of a transition metal (indium-tin-zinc based) conductive material exhibiting high conductivity in the cleaning process. After the synthesis, a suitable dispersant is added to remove the aggregation phenomenon, After molding, isostatic pressing and sintering in an oxygen pressurized state, micro-machining is removed and a high-density target can be manufactured.

본 발명에 따른 청정공정 이용 주석과 아연을 고용한 인듐저감 조성(인듐-아연-주석 산화물)인 인듐산화물의 나노 분말합성 방법은 부탄올과 인듐아세테이트, 아연아세테이트 그리고 주석아세테이트를 반응시킨 청정공정으로, 인듐산화물에 아연산화물과 주석산화물이 18~ 28.7중량% 고용된 단일 결정상 빅스바이트로 이루어진 인듐산화물인 것을 특징으로 한다.INDUSTRIAL APPLICABILITY According to the present invention, a method for synthesizing a nano powder of indium oxide which is an indium-reduced composition (indium-zinc-tin oxide) in which tin and zinc are dissolved by using the cleaning process according to the present invention is a cleaning process in which butanol is reacted with indium acetate, zinc acetate and tin acetate, And an indium oxide consisting of a single crystal bixbyite having 18 to 28.7 wt% of zinc oxide and tin oxide dissolved in indium oxide.

상기 청정공정으로 제조된 20nm 크기(평균값)의 인듐산화물의 뭉침 현상은 도데실라민에 하이드록실 프로필 셀룰로오즈나 폴리에틸렌글리콜을 혼합 첨가하거나 도데시실라민 또는 암모늄폴리메타아크릴레이트를 단독 첨가하여 분산시키는 방법으로 상기 분산제를 사용하는 것을 특징으로 한다.The agglomeration of the indium oxide having a size of 20 nm (average value) produced by the above-mentioned cleaning process is a method of adding dodecylamine with hydroxylpropylcellulose or polyethylene glycol or dodecylamine or ammonium polymethacrylate alone And the dispersant is used.

상기 합성방법으로 제조된 주석과 아연이 고용된 인듐산화물 분말을 결합제, 이형제와 함께 혼합하여 슬러리 한 후, 슬러리 분무 건조하여 과립(granule)화하여, 1차 일축성형, 2차 등가압 성형하여 타겟 성형체를 제조한 후, 성형체를 가압 산소분위기로 1350℃에서 4시간 소성하여 상대밀도의 99.7%까지 소결된 고전도 고밀도 타켓을 제조하는 것을 특징으로 한다.
The indium oxide powder prepared by the above-described synthesis method is mixed with a binder and a release agent to prepare a slurry, and then the slurry is spray dried to form granules, which are subjected to primary uniaxial pressing, After the compact is produced, the compact is fired at 1350 ° C for 4 hours in a pressurized oxygen atmosphere to produce a high-density high-density target sintered up to 99.7% of the relative density.

본 발명의 효과는 우선 아연과 주석을 고용시킨 인듐 산화물을 제조할 수 있으므로 인듐 사용량을 18.0~28.7중량%로 저감할 수 있었고, 또한 분말을 청정공정으로 합성함으로서 폐수 발생없이 합성할 수 있었으며, 20nm 크기 합성물의 뭉침 현상을 분산제를 사용하여 잘 분산시킴으로서 현재 아이티오 타겟 이상의 고밀도인 상대밀도의 99.7%이상인 인듐이 저감된 주석-아연-인듐 산화물 타겟을 제조 할 수 있었고, 또한 <도 1>과 같이 아이티오와 대등한 비저항 특성을 갖는 투명전도체를 얻을 수 있는 효과가 있었다.
INDUSTRIAL APPLICABILITY The effect of the present invention can be achieved by first preparing indium oxide with zinc and tin dissolved therein. Therefore, the amount of indium used can be reduced to 18.0 to 28.7 wt%, and the powder can be synthesized in a clean process, Size composite was well dispersed by using a dispersant, it was possible to produce a tin-zinc-indium oxide target in which indium was reduced to 99.7% or more of high density relative density higher than that of the current iota target, and as shown in Fig. 1 It is possible to obtain a transparent conductor having a resistivity characteristic equivalent to that of ATIO.

도 1은 본 발명으로 합성한 아연과 주석이 18~28.7중량% 고용된 인듐산화물을 이용하여 제작한 막의 투명 특성 그림
도 2는 본 발명으로 합성한 아연과 주석이 고용된 인듐산화물 분말의 주사 전자 현미경 사진
도 3은 아연과 주석이 고용된 인듐산화물을 성형하여 1350℃에서 소결한 타겟과 그 타겟의 미세구조
도 4는 아연과 주석이 고용된 인듐산화물 분말을 분무 건조한 과립
표 1은 아연과 주석이 고용된 인듐산화물 분말을 이용하여 제조한 타겟의 소결조건에 따른 특성
1 is a graph showing the transparency of a film prepared using indium oxide with 18 to 28.7 wt% solids of zinc and tin synthesized according to the present invention
2 is a scanning electron micrograph of zinc and tin-dissolved indium oxide powder synthesized according to the present invention
Fig. 3 is a graph showing the relationship between a target sintered at 1350 deg. C by molding zinc oxide and tin-dissolved indium oxide,
Fig. 4 is a graph showing the relationship between the concentration of zinc oxide and tin-dissolved indium oxide powder
Table 1 shows the characteristics of the target prepared by using indium oxide powder in which zinc and tin are dissolved, according to sintering conditions

이하, 본 발명에서의 실시를 위한 구체적인 내용을 설명하면 다음과 같다. Hereinafter, specific details for carrying out the present invention will be described.

청정공정을 이용한 인듐저감 조성의 습식합성은 출발 원료로 인듐아세테이트 , 아연아세테이트 및 주석아세테이트와 용매로 부탄올을 혼합하고 합성하여, 아연과 주석이 인듐에 고용된 수산화 인듐을 합성하고, 이 아연과 주석이 인듐에 고용된 수산화인듐을 하소하여 아연과 주석이 인듐에 고용된 인듐 산화물을 제조한다. 합성 시 각각의 금속아세테이트로부터 해리된 금속 착이온이 부탄올에서 해리된 수소 착이온과의 결합으로 아연과 주석이 고용된 수산화인듐이 합성되고, 부산물로 부틸아세테이트가 생성되어 아세테이트산과 금속수화물 생성을 억제하는 물이 발생하지 않지 않는다. 따라서 침전제로 사용하는 강산이나 강염기를 투입하지 않아도 반응이 진행되므로 산이나 염기 이온을 제거하는 세척공정이 요구되지 않는다.The wet synthesis of the indium-reducing composition using a clean process is a process in which indium acetate, zinc acetate and tin acetate are mixed with butanol as a starting material and synthesized to synthesize indium hydroxide in which zinc and tin are dissolved in indium, This indium hydroxide dissolved in indium is calcined to produce an indium oxide in which zinc and tin are dissolved in indium. During the synthesis, metal complex ions dissociated from each metal acetate are combined with hydrogen complex ions dissociated from butanol to synthesize indium hydroxide in which zinc and tin are dissolved, and butyl acetate is produced as a byproduct to inhibit acetate acid and metal hydrate formation Water does not occur. Therefore, a washing process for removing acidic or basic ions is not required since the reaction proceeds without the addition of a strong acid or a strong base to be used as a precipitant.

따라서 폐수 없이 아연과 주석이 고용한 인듐산화물 분말 합성 및 이의 합성방법을 제공하는 것이다.Therefore, it is an object of the present invention to provide a method for synthesizing indium oxide powder in which zinc and tin are dissolved without wastewater and a method for synthesizing the same.

본 발명에서는 아연과 주석을 고용한 인듐 저감 산화물 합성 방법은 먼저 부탄올에 금속아세테이트를 투입하여 아연과 주석이 고용된 수산화인듐을 합성하는 단계와, 합성된 아연과 주석이 고용된 수산화인듐을 300℃에서 하소함으로써, 빅스바이트(bixybyite) 단일 결정상을 갖는 아연과 주석이 고용된 산화인듐 분말을 합성하는 단계로 구성된다. In the present invention, a method of synthesizing indium-reduced oxides containing zinc and tin is characterized in that a metal acetate is first added to butanol to synthesize indium hydroxide in which zinc and tin are dissolved and a step in which the synthesized zinc and tin- To thereby synthesize zinc and tin-dissolved indium oxide powder having a bixbyite single crystal phase.

수십 나노크기의 분말의 뭉침 현상을 분산시키기 위해 청정공정으로 합성한 주석과 아연이 인듐에 고용된 인듐산화물을 물과 분산제를 넣고 어트리션밀에서 해쇄하였다. 이때 사용한 분산제로는 도데실라민, 도데실라민+하이드록실프로필셀룰로오즈, 도데실라민+폴리에틸렐그리콘 및 암모늄 폴리메타아크릴레이트 4종류로 각각 사용한다. In order to disperse the aggregation phenomenon of tens of nano-sized powders, indium oxide in which indium is dissolved in tin and zinc synthesized by a clean process was impregnated with water and a dispersing agent and pulverized in an induction mill. As the dispersing agent used herein, four types of dodecylamine, dodecylamine + hydroxylpropylcellulose, dodecylamine + polyethyleneglycone and ammonium polymethacrylate are used.

위와 같이 합성한 분말을 주사현미경으로 관찰한 결과 분말의 특성은 <도 2>와 같이 입자크기가 평균 20nm 크기이었으며, 비표면적은 150m2/g이었다. The powder thus synthesized was observed with a scanning electron microscope. The powder had an average particle size of 20 nm and a specific surface area of 150 m 2 / g as shown in FIG. 2.

고밀도 타겟은 앞서 잘 분산된 수십 나노크기를 갖는 아연과 주석을 고용한 인듐산화물 분말을 과립화하여 등가압 성형한 후 0.5bar 산소가압분위기에서 1350℃ 4시간 유지 소결하여 고밀도로 제조하였다.The high density target was prepared by isostatic pressing with a well dispersed indium oxide powder with several tens of nano sized zinc and tin, followed by sintering at 1350 ℃ for 4 hours in oxygen pressurized atmosphere of 0.5 bar.

1350℃에서 4시간 유지하여 소결한 직경 4인치크기의 타겟과 소결된 소결체에 대해 주사전자현미경으로 미세구조를 관찰한 결과 치밀한 조직을 나타낸 사진을 <도 3>에 나타내었다. 이때의 상대밀도는 아이티오 99.5%보다 높은 99.7%를 얻을 수 있었고, 비저항은 5x10-4Ωㆍ㎝으로 아이티오와 거의 유사한 값을 얻을 수 있었다.FIG. 3 is a photograph showing a dense structure as a result of observing the microstructure of the sintered body having a diameter of 4 inches held at 1350 ° C. for 4 hours by a scanning electron microscope. The relative density was 99.7% higher than ATIO 99.5% and the resistivity was 5 × 10 -4 Ω ㆍ ㎝.

(실시 예 1)(Example 1)

반응용기에 부탄올을 넣고 교반하는 상태에서 인듐아세테이트, 아연아세테이트, 주석아세테이트를 금속 아세테이크를 서서히 투입하여 110℃에서 24시간 합성한 후, 혼합물은 진공 회전증발기(Vacuum Rotary Evaporator)를 이용하여 60℃로 24시간 가동하여 부탄올과 부틸아세테이트를 증발시켜 포집함으로서 완전히 건조된 상태로 얻었다.After adding butanol to the reaction vessel and stirring the mixture, indium acetate, zinc acetate and tin acetate were gradually added to the metal acetal and gradually synthesized at 110 ° C for 24 hours. The mixture was then calcined at 60 ° C using a vacuum rotary evaporator For 24 hours, and the butanol and butyl acetate were evaporated and collected to obtain a completely dried state.

합성된 혼합물은 진공 회전증발기(Vacuum Rotary Evaporator)를 이용하여 60℃로 24시간 가동하여 부탄올과 부틸아세테이트를 증발시켜 포집함으로서 완전히 건조된 상태로 얻었다.The synthesized mixture was dried in a vacuum rotary evaporator at 60 ° C for 24 hours to collect butanol and butyl acetate by evaporation to obtain a completely dried state.

건조된 합성물의 결정상은 엑스선회절분석 결과 수산화인듐 결정상이었으며, 상기 수산화인듐 합성물을 300℃에서 10시간 하소하면, 아연과 주석을 인듐에 고용시킨 산화인듐의 결정상인 빅스바이트 결정을 얻을 수 있었다.The crystalline phase of the dried composite was an indium hydroxide crystal phase as a result of X-ray diffraction analysis. When the indium hydroxide composite was calcined at 300 ° C for 10 hours, a big-bite crystal, which is a crystalline phase of indium oxide, in which zinc and tin were dissolved in indium, was obtained.

엑스선회절 피크 값이 약간 이동되어 있는 것은 아연과 주석이 고용된 인듐산화물임을 확인해 주는 것이다.The slightly shifted X-ray diffraction peak value confirms that zinc and tin are solid-dissolved indium oxide.

이렇게 제조된 분말은 물과 분산제인 도데실라민과 하이드록실프로필셀룰로오즈를 넣고 어트리션밀(Attriton mill)에서 6시간 해쇄하고 여기에 결합제, 이형제 등을 투입하여 슬러리(slurry) 상태로 만들었다.Dodecylamine and hydroxylpropylcellulose, which are water and dispersants, were added to the thus-prepared powder, and the resulting powder was pulverized in an Attriton mill for 6 hours, and a binder and a release agent were added thereto to form a slurry state.

위에서 제조한 슬러리는 분무건조기를 이용하여 인입온도 190℃, 배출온도 110℃ 및 분무속도 9500rpm으로 작업하여 과립을 제조하였다.The slurry prepared above was granulated using a spray dryer at a draw temperature of 190 ° C, a discharge temperature of 110 ° C and a spray rate of 9500 rpm.

제조된 과립은 일축 가압프레스를 사용 200kg/㎠의 압력으로 1차 성형한 후, 2차로 2,000kg/㎠의 압력으로 등가압성형(Isostactec pressing)하여 타겟 성형체(green body)를 제조한 후, 산소가압전기로에 넣고 산소압력을 0.5bar로 하여 시간당 300℃로 승온하여 600℃에서 3시간 유지하여 유기물을 완전히 제거한 후 1350℃에서 4시간 소성하여 타겟을 제조하였다.The prepared granules were first molded at a pressure of 200 kg / cm 2 using a uniaxial pressing press and then subjected to isostatic pressing at a pressure of 2,000 kg / cm 2 to form a target green body, The mixture was placed in a pressurized electric furnace, and the temperature was raised to 300 ° C per hour at an oxygen pressure of 0.5 bar. The temperature was maintained at 600 ° C for 3 hours to completely remove the organic materials and then fired at 1350 ° C for 4 hours.

도 4는 분무 건조한 과립이다. 4 is spray-dried granules.

아래 표 1을 참고하면, 산소가압 분위기에 따라 밀도의 치밀화 및 전기전도도가 다르게 나타남으로써, 본 발명에서 청정공정으로 합성한 나노크기 분말의 경우 0.5bar 산소가압 분위기로 고상반응보다 온도가 150~200℃ 낮음 1350℃로 치밀하게 소결되었다.As shown in Table 1 below, the densification of densification and the electric conductivity are different depending on the oxygen pressurized atmosphere. In the present invention, nano-size powders synthesized in the present invention have a temperature of 150 to 200 Lt; RTI ID = 0.0 &gt; 1350 C. &lt; / RTI &gt;

O2 압력(bar)O 2 pressure (bar) 결정그레인(Grain, ㎛)Crystal grain (Grain, 占 퐉) 소결밀도(%)Sintered density (%) 비저항(Ω㎝)Resistivity (Ω cm) 0.50.5 3~43 to 4 99.799.7 5x10-4 5x10 -4 0.10.1 1~51-5 99.399.3 7x10-4 7 x 10 -4 0.010.01 1~51-5 99.099.0 8x10-4 8x10 -4

Claims (3)

부탄올과 인듐아세테이트, 아연아세테이트 그리고 주석아세테이트를 반응시킨 청정공정으로, 인듐산화물에 아연산화물과 주석산화물이 18~ 28.7중량% 고용된 단일 결정상 빅스바이트로 이루어진 인듐산화물을 생성하는 청정공정 이용 아연과 주석이 인듐에 고용된 인듐산화물(인듐-아연-주석 산화물)의 나노 분말 합성 방법.
Using a clean process to produce indium oxide consisting of monocrystalline bixbyite with 18-28.7 wt% solids of zinc oxide and tin oxide in indium oxide in a clean process with butanol reacting with indium acetate, zinc acetate and tin acetate. Zinc and tin A method for synthesizing nano powder of indium oxide (indium-zinc-tin oxide) dissolved in indium.
제 1 항에 있어서,
청정공정 이용 아연과 주석이 인듐에 고용된 인듐산화물 나노 분말의 뭉침 현상을 분산제인 도데실라민, 도데실라민+하이드록실프로필셀룰로오즈, 도데실라민+폴리에틸렐그리콘, 암모늄 폴리메타아크릴레이트 중 어느 하나를 사용하여 분산시키는 청정공정 이용 아연과 주석이 인듐에 고용된 인듐산화물(인듐-아연-주석 산화물)의 나노 분말 합성 방법.
The method according to claim 1,
In the clean process, the aggregation phenomenon of indium oxide nanoparticles in which zinc and tin are dissolved in indium is called dodecylamine, dodecylamine + hydroxylpropylcellulose, dodecylamine + polyethyleneglycone, and ammonium polymethacrylate A method for synthesizing nanoparticles of indium oxide (indium-zinc-tin oxide) in which zinc and tin are dissolved in indium by use of a clean process to disperse using either one.
제 2 항에 있어서,
청정공정 이용 아연과 주석이 인듐에 고용된 인듐산화물 나노분말에 분산제를 넣어 분산된 슬러리에 결합제, 이형제를 혼합하여 슬러리를 만들고,
슬러리를 분무 건조하여 과립으로 제조하며,
과립을 1차 일축성형한 후, 2차 등가압 성형하여 타겟 성형체를 제조하고,
성형체를 가압 산소분위기로에서 1350℃에서 4시간 소성하여 제조하는 것을 특징으로 하는 청정공정 이용 아연과 주석이 인듐에 고용된 인듐산화물(인듐-아연-주석 산화물)의 나노 분말 합성 방법.
3. The method of claim 2,
Use of clean process A slurry is prepared by mixing a binder and a releasing agent in a dispersed slurry of indium oxide nano powder in which zinc and tin are dissolved in indium,
The slurry is spray dried to produce granules,
The granules are first uniaxially compacted and then subjected to secondary isostatic pressing to produce a target compact,
(Indium-zinc-tin oxide) in which zinc and tin are dissolved in indium for use in a clean process, characterized in that the compact is produced by firing at 1350 占 폚 for 4 hours in a pressurized oxygen atmosphere.
KR1020110117275A 2011-11-11 2011-11-11 Synthetic method of nano-sized powder and manufacturing method of high density and conductibility target with using sn-zn for decreasing indium KR101429042B1 (en)

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