KR101279541B1 - Indium-tin-oxide powder and method for synthesizing indium-tin-oxide thereof, and method for manufacturing indium-tin-oxide target by using the indium-tin-oxide powder - Google Patents
Indium-tin-oxide powder and method for synthesizing indium-tin-oxide thereof, and method for manufacturing indium-tin-oxide target by using the indium-tin-oxide powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 53
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 11
- 230000002194 synthesizing effect Effects 0.000 title abstract description 4
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 title 4
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 50
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 50
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 46
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 41
- IGUXCTSQIGAGSV-UHFFFAOYSA-K indium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[In+3] IGUXCTSQIGAGSV-UHFFFAOYSA-K 0.000 claims abstract description 21
- 239000006104 solid solution Substances 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims abstract description 10
- VBXWCGWXDOBUQZ-UHFFFAOYSA-K diacetyloxyindiganyl acetate Chemical compound [In+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VBXWCGWXDOBUQZ-UHFFFAOYSA-K 0.000 claims description 12
- YJGJRYWNNHUESM-UHFFFAOYSA-J triacetyloxystannyl acetate Chemical compound [Sn+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O YJGJRYWNNHUESM-UHFFFAOYSA-J 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 claims description 9
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 6
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims 1
- 238000000465 moulding Methods 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 12
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 10
- 239000008187 granular material Substances 0.000 description 8
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 7
- 239000013077 target material Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 3
- 230000003472 neutralizing effect Effects 0.000 description 3
- 239000011368 organic material Substances 0.000 description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 3
- 229910001887 tin oxide Inorganic materials 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910001449 indium ion Inorganic materials 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- -1 and thus Chemical compound 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
- B01J6/001—Calcining
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
- C01G1/02—Oxides
Abstract
본 발명은 투명전도성 산화물 필름(TCO film ; Transparent conducting Oxid film) 제조에 사용되는 주석이 고용된 인듐 산화물 분말과, 상기 인듐 산화물 분말을 합성하는 방법 및 상기 인듐 산화물 분말을 이용하여 인듐 산화물 타겟을 제조하는 방법에 관한 것이다.
본 발명에 따른 주석이 고용된 인듐 산화물 분말과 이의 제조방법 및 주석이 고용된 인듐 산화물 분말을 이용한 인듐 산화물 타겟의 제조방법은 부탄올과 금속아세테이트가 반응하여, 주석이 고용된 수산화인듐으로 합성되고, 상기 주석이 고용된 수산환인듐을 300℃에서 하소하여 제조한 것을 특징으로 한다. The present invention provides an indium oxide powder using indium oxide powder in which tin is used for manufacturing a transparent conducting oxide film (TCO film), a method of synthesizing the indium oxide powder, and an indium oxide powder. It is about how to.
According to the present invention, indium oxide powder in which tin is dissolved, a method for preparing the same, and a method for producing indium oxide target using indium oxide powder in which tin is dissolved are synthesized from indium hydroxide in which tin is dissolved by reacting butanol and metal acetate. It is characterized in that the tin in the solid solution of the indium hydroxide ring was calcined at 300 ℃.
Description
본 발명은 투명전도성 산화물 필름(TCO film ; Transparent conducting Oxid film) 제조에 사용되는 주석이 고용된 인듐 산화물 분말과, 상기 인듐 산화물 분말을 합성하는 방법 및 상기 인듐 산화물 분말을 이용하여 인듐 산화물 타겟을 제조하는 방법에 관한 것이다.
The present invention provides an indium oxide powder using indium oxide powder in which tin is used for manufacturing a transparent conducting oxide film (TCO film), a method of synthesizing the indium oxide powder, and an indium oxide powder. It is about how to.
대한민국 등록특허 제10-0850010호(2008년07월28일, 등록)에 "초음파 화학적 반응에 의한 산화 인듐 분말의 제조방법 및 ITO타겟재의 제조방법"이 소개되어 있다. Republic of Korea Patent Registration No. 10-0850010 (July 28, 2008, registered) "indium oxide powder production method by ultrasonic chemical reaction and ITO target material manufacturing method" is introduced.
상기 초음파 화학적 반응에 의한 산화 인듐 분말의 제조방법은 초음파 화학적 반응에 의한 산화 인듐 분말의 제조방법에 있어서, 인듐 이온을 포함하는 수용액을 제조하는 단계와, 상기 수용액과 중화제를 교반하면서 초음파 반응하는 단계와, 중화제 수용액 상에 초음파를 인가하면서 상기 인듐 이온 수용액을 반응시키는 역중화 초음파 화학적 반응 단계와, 상기 반응에 의해 수산화 인듐 분말을 제조하는 단계와, 상기 제조된 수산화 인듐 분말을 세정 및 건조하는 단계와, 건조된 상기 분말을 열처리를 통해 산화하는 단계를 포함하여 구성되는 것을 특징으로 한다. The manufacturing method of the indium oxide powder by the ultrasonic chemical reaction in the manufacturing method of the indium oxide powder by the ultrasonic chemical reaction, preparing an aqueous solution containing indium ions, and the ultrasonic reaction while stirring the aqueous solution and the neutralizing agent And, the neutralizing ultrasonic chemical reaction step of reacting the aqueous solution of indium ions while applying an ultrasonic wave to the neutralizing aqueous solution, preparing an indium hydroxide powder by the reaction, washing and drying the prepared indium hydroxide powder And oxidizing the dried powder through heat treatment.
또한, 상기 초음파 화학적 반응에 의한 ITO타겟재의 제조방법은 상기 산화 인듐 분말과 산화 주석 분말을 혼합하는 단계와, 상기 혼합된 분말을 조립 후 가압 성형하여 타겟재를 얻는 단계와, 상기 혼합된 분말을 조립 후 가압 성형하여 타겟재를 얻는 단계와, 상기 타겟재를 소결하는 단계와, 상기 소결된 타겟재를 면가공 및 절단하는 단계를 포함하여 구성되는 것을 특징으로 한다. In addition, the manufacturing method of the ITO target material by the ultrasonic chemical reaction comprises the steps of mixing the indium oxide powder and tin oxide powder, the step of obtaining a target material by assembling the mixed powder and pressurized, and the mixed powder It is characterized in that it comprises a step of obtaining a target material by pressing molding after assembly, the step of sintering the target material, the surface processing and cutting the sintered target material.
그러나, 상기 초음파 화학적 반응에 의한 산화 인듐 분말의 제조방법 및 ITO타겟재의 제조방법은 제조된 수산화 인듐 분말을 세정하는 단계에서 염산, 질산, 황산 등을 함유하는 다량의 폐수가 발생되는 문제가 있다. However, the method of preparing the indium oxide powder and the ITO target material by the ultrasonic chemical reaction has a problem that a large amount of wastewater containing hydrochloric acid, nitric acid, sulfuric acid, etc. is generated in the step of washing the prepared indium hydroxide powder.
또한, 합성단계에서 산화인듐 등 단일 원료만을 합성하여 제조한 후, 복합 산화물 TCO 제조에 사용되는 타겟의 인듐 자리에 고용할 원료인 산화주석을 혼합하는 과정을 거쳐 복합 산화물을 제조하므로 타겟의 조성 불균일성이 발생될 수 있으며, 산화인듐, 산화주석을 혼합하여 제조한 타겟의 경우 소결하는 과정에서 주석의 휘발이 쉽게 일어나기 때문에 타겟의 조성 불균일성이 발생할 수 있는 문제점이 있었다.
In addition, since the composite oxide is prepared by synthesizing only a single raw material such as indium oxide in the synthesis step and then mixing tin oxide, which is a raw material to be dissolved in the indium of the target used for manufacturing the composite oxide TCO, the composition is not uniform in composition. This may occur, and in the case of a target prepared by mixing indium oxide and tin oxide, there is a problem in that composition non-uniformity of the target may occur because the volatilization of tin easily occurs during the sintering process.
따라서, 본 발명의 목적은 부탄올과 인듐아세테이트, 주석아세테이트를 혼합하여, 주석이 고용된 수산화 인듐을 합성함으로써, 인듐아세테이트, 주석아세테이트에서 해리된 인듐 착이온, 주석 착이온이 부탄올에서 해리된 수소 착이온과의 결합으로 주석이 고용된 수산화인듐이 합성되고, 부산물로 부틸아세테이트가 생성되어 부틸아세테이트와 금속수화물 생성을 억제하는 물이 발생하지 않기 때문에 촉매로 사용하는 강산을 투입하지 않아도 반응이 진행되므로 산 이온을 제거하는 세척공정이 요구되지 않는 주석이 고용된 산화인듐 분말 및 이의 제조방법을 제공하는 것이다.Accordingly, an object of the present invention is to synthesize indium hydroxide in which tin is dissolved by mixing butanol, indium acetate, and tin acetate, and thus, indium acetate, hydrogen complex in which tin complex is dissociated in butanol. The reaction proceeds without the addition of a strong acid used as a catalyst because indium hydroxide, in which tin is dissolved, is synthesized by binding with ions, and butyl acetate is produced as a by-product, and water that suppresses the production of butyl acetate and metal hydrate is not generated. It is to provide an indium oxide powder in a solid solution of tin that does not require a washing step for removing acid ions and a method for producing the same.
또한, 본 발명의 다른 목적은 위에서 언급한 주석이 고용된 산화인듐 분말을 물 및 분산제와 혼합한 후, 어트리션밀에서 해쇄(disintegtation)하고, 여기에 결합제, 이형제 등을 투입하여 슬러리 상태로 만들어서 스프레이드라이어를 이용하여 분말 성형을 위한 과립으로 제조하며, 제조된 과립을 분말성형프레스를 사용하여 타겟의 성형체를 제조하는 인듐산화물 타겟 제조방법을 제공하는 것이다.
In addition, another object of the present invention is to dissolve the above-mentioned indium oxide powder in the solid solution of the above-mentioned tin with water and a dispersant, and then disintegrate in an attrition mill, and to make a slurry by adding a binder, a release agent, etc. It is to provide a method for producing an indium oxide target to prepare a granule for powder molding using a spray dryer, and to prepare a molded body of the target using a powder molding press.
상기와 같은 목적을 달성하기 위한 본 발명에 따른 주석이 고용된 인듐 산화물 분말은 1.9몰~2몰의 인듐아세테이트와 0.4몰 이하의 주석아세테이트로 구성된 금속아세테이트와 부탄올이 반응하여, 주석이 고용된 수산화인듐으로 합성되고, 상기 주석이 고용된 수산화인듐을 300℃에서 하소하여 제조한 것을 특징으로 한다.Indium oxide powder in a solid solution of tin according to the present invention for achieving the above object is reacted with metal acetate and butanol consisting of 1.9 mol ~ 2 mol of indium acetate and 0.4 mol or less of tin acetate, the hydroxide of tin is dissolved It is synthesized from indium, and characterized in that the indium hydroxide prepared by calcining the solid solution of tin.
상기 부탄올은 n-부탄올, tert-부탄올, 2-부탄올 및 Iso-부탄올 중 어느 하나인 것을 특징으로 한다.The butanol is characterized in that any one of n-butanol, tert-butanol, 2-butanol and Iso-butanol.
본 발명에 따른 주석이 고용된 인듐 산화물 분말 제조방법은Indium oxide powder manufacturing method in which tin is dissolved in accordance with the present invention
(1) 부탄올에 금속아세테이트(인듐아세테이트, 주석아세테이트 혼합물)을 투입하여 주석이 고용된 수산화인듐을 합성하는 단계와,(1) adding metal acetate (indium acetate, tin acetate mixture) to butanol to synthesize indium hydroxide in which tin is dissolved;
(2) 합성된 주석이 고용된 수산화인듐을 300℃의 온도에서 하소함으로써, 주석이 고용된 산화인듐 분말을 제조하는 단계로 구성되는 것을 특징으로 한다.(2) It is characterized by comprising the step of preparing the indium oxide powder in which tin is dissolved by calcining indium hydroxide in which the synthesized tin is dissolved in solid solution at a temperature of 300 ° C.
본 발명에 따른 주석이 고용된 인듐 산화물 분말을 이용한 인듐 산화물 타겟의 제조방법은 위에서 설명한 제조방법으로 제조된 주석이 고용된 인듐 산화물 분말을 물 및 분산제와 혼합한 후, 어트리션밀에서 해쇄(disintegtation)하고, 여기에 결합제, 이형제를 투입하여 슬러리 상태로 만들고, 슬러리를 스프레이드라이어를 이용하여 분말 성형을 위한 과립으로 제조하며, 제조된 과립을 분말성형프레스를 사용하여 제조된 과립은 분말성형프레스를 사용하여 1차 성형한 후 2,000kg/cm2의 압력으로 상온 등압 성형하여 타겟 성형체를 제조하고, 과립 제조를 위해 투입된 유기물을 완전히 제거하기 위해 800℃에서 하소하고, 하소된 성형체를 300℃/hr의 승온속도로 승온하여 1500℃에서 소성하여 타겟을 제조하는 것을 특징으로 한다.
Method for producing an indium oxide target using indium oxide powder in the solid solution of tin according to the present invention, after mixing the indium oxide powder in the solid solution of tin prepared by the above-described manufacturing method with water and a dispersing agent, disintegration in an attrition mill And a binder and a release agent are added to make a slurry state, and the slurry is prepared into granules for powder molding using a spray dryer, and the granules prepared using a powder molding press produce a powder molding press. After the primary molding using to form a target molded body at room temperature isostatic pressure at a pressure of 2,000kg / cm 2 , calcined at 800 ℃ to completely remove the organic material injected for granulation, the calcined molded body 300 ℃ / hr The temperature is raised to a heating rate of the firing at 1500 ℃ characterized in that to produce a target.
이것에 의해, 본 발명에 따른 주석이 고용된 인듐 산화물 분말과 이의 제조방법 및 주석이 고용된 인듐 산화물 분말을 이용한 인듐 산화물 타겟의 제조방법은 인듐아세테이트, 주석아세테이트를 부탄올을 이용하여 합성함으로 폐수 발생이 없이 균일한 나노입자로 이루어진 주석이 고용된 산화인듐을 제조할 수 있으며, 이를 이용하여 고밀도의 인듐산화물 타겟을 제조할 수 있는 효과가 있다.
As a result, indium oxide powder containing tin in accordance with the present invention, a method for preparing the same, and a method for producing the indium oxide target using the indium oxide powder containing tin in combination with indium acetate and tin acetate using butanol generate wastewater. Without this, it is possible to manufacture indium oxide in which tin composed of uniform nanoparticles is dissolved, and there is an effect of manufacturing a high density indium oxide target using the same.
도 1은 본 발명에 따른 주석이 고용된 인듐 산화물 분말을 제조하기 위한 반응장치 개요도
도 2는 주석이 고용된 산화인듐 분말의 엑스선회절분석 패턴
도 3은 주석이 고용된 산화인듐 분말의 주사전자현미경 사진1 is a schematic view of a reactor for producing indium oxide powder in solid solution in accordance with the present invention
2 is an X-ray diffraction pattern of indium oxide powder in solid solution
3 is a scanning electron microscope photograph of indium oxide powder in solid solution of tin
이하, 본 발명에 따른 바람직한 실시예를 도면을 참조하여 상세하게 설명하기로 한다. Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the drawings.
본 발명의 실시예에 따른 주석이 고용된 산화 인듐 분말의 제조방법은 부탄올과 금속아세테이트가 반응하여, 주석이 고용된 수산화인듐으로 합성되고, 상기 주석이 고용된 수산환인듐을 300℃에서 하소하여 제조된다. According to an embodiment of the present invention, a method of preparing a solid solution of indium oxide in which tin is dissolved is synthesized from butanol and metal acetate, in which tin is dissolved in indium hydroxide, and the indium hydroxide in which tin is dissolved is calcined at 300 ° C. Are manufactured.
상기 부탄올은 n-부탄올, tert-부탄올, 2-부탄올 및 Iso-부탄올 중 어느 하나이고, 부탄올과 금속아세테이트가 1 : 2~10의 몰비로 혼합된다.The butanol is any one of n-butanol, tert-butanol, 2-butanol, and Iso-butanol, and butanol and metal acetate are mixed in a molar ratio of 1: 2 to 10.
상기 금속아세테이트는 인듐아세테이트 및 주석아세테이트 혼합물이고, 인듐아세테이트 1.9몰~2몰, 주석아세테이트 0.4몰 이하의 비율로 구성된다.The metal acetate is an indium acetate and tin acetate mixture, and is composed of 1.9 to 2 mol of indium acetate and 0.4 mol or less of tin acetate.
상기와 같이 제조된 본 발명에 따른 주석이 고용된 산화 인듐 분말은 10nm~30nm의 나노입자를 가지며, 빅스바이트(bixbyte) 결정상을 갖는다.The indium oxide powder in which tin is dissolved in accordance with the present invention prepared as described above has nanoparticles of 10 nm to 30 nm, and has a bixbyte crystal phase.
상기와 같은 본 발명에 따른 주석이 고용된 산화 인듐 분말을 제조하는 방법은 다음과 같다.The method for producing indium oxide powder in which tin is dissolved in accordance with the present invention as described above is as follows.
(1) 부탄올에 금속아세테이트(인듐아세테이트, 주석아세테이트 혼합물)을 투입하여 주석이 고용된 수산화인듐을 합성한다.(1) Metal acetate (indium acetate, tin acetate mixture) is added to butanol to synthesize indium hydroxide in which tin is dissolved.
이때, 인듐아세테이트, 주석아세테이트에서 해리된 인듐 착이온, 주석 착이온이 부탄올에서 해리된 수소 착이온과의 결합으로 주석이 고용된 수산화인듐이 합성된다. 그리고, 부산물로 부틸아세테이트가 생성되어 아세테이트산과 금속수화물 생성을 억제하는 물이 발생하지 않기 때문에 부틸아세테이트와 금속산화물 생성을 억제하는 인자가 없어 촉매로 사용하는 강산을 투입하지 않아도 반응이 진행되므로 산 이온을 제거하는 세척공정이 요구되지 않는 장점이 있다.At this time, indium hydroxide in which tin is dissolved is synthesized by indium acetate, indium complex ions dissociated in tin acetate, and tin complex ions in combination with hydrogen complex ions dissociated in butanol. In addition, since butyl acetate is generated as a by-product and no water inhibits the formation of acetate acid and metal hydrate, there is no factor that inhibits the production of butyl acetate and metal oxide. There is an advantage that does not require a washing process to remove.
(화학 반응식)(Chemical reaction)
(3-X)CH3(CH2)2CH2OH + (1-X)In(CH3COO)3 + XSn(CH3Coo)2 (3-X) CH 3 (CH 2 ) 2 CH 2 OH + (1-X) In (CH 3 COO) 3 + XSn (CH 3 Coo) 2
⇒ In1 - XSnXSnY(OH)3 + (3-X)CH3(CH2)2CH2CH3COO⇒ In 1 - X Sn X Sn Y (OH) 3 + (3-X) CH 3 (CH 2 ) 2 CH 2 CH 3 COO
(2) 주석이 고용된 수산화인듐을 300℃의 온도에서 하소함으로써, 빅스바이트(bixbyte) 결정상을 갖는 주석이 고용된 산화인듐 분말을 제조하게 된다.(2) Indium hydroxide, in which tin is dissolved, is calcined at a temperature of 300 ° C., thereby producing indium oxide powder in which tin is dissolved in a bixbyte crystal phase.
또한, 본 발명에 따른 인듐 산화물 타겟 제조방법은 위에서 설명한 주석이 고용된 산화인듐 분말을 물 및 분산제와 혼합한 후, 어트리션밀에서 6시간 해쇄(disintegtation)하고, 여기에 결합제, 이형제를 투입하여 슬러리 상태로 만들고, 슬러리를 스프레이드라이어를 이용하여 분말 성형을 위한 과립으로 제조하며, 제조된 과립을 분말성형프레스를 사용하여 제조된 과립은 분말성형프레스를 사용하여 200kg/cm2의 압력으로 1차 성형한 후 2,000kg/cm2의 압력으로 상온 등압 성형하여 타겟 성형체를 제조한다. 또한, 과립 제조를 위해 투입된 유기물을 완전히 제거하기 위해 800℃에서 10시간 하소한다. 그리고, 하소된 성형체를 300℃/hr의 승온속도로 승온하여 1500℃에서 2시간 소성하여 타겟을 제조한다. In addition, in the method for producing an indium oxide target according to the present invention, after mixing indium oxide powder in which tin is dissolved in water and a dispersant, disintegration is performed in an attrition mill for 6 hours, and a binder and a release agent are added thereto. It is made into a slurry state, the slurry is prepared into granules for powder molding by using a spray dryer, and the granules prepared by using a powder molding press are prepared at a pressure of 200 kg / cm 2 using a powder molding press. After the molding, the target molded body is manufactured by isothermal molding at room temperature under a pressure of 2,000 kg / cm 2 . It is also calcined at 800 ° C. for 10 hours in order to completely remove the organic material added for granule preparation. Then, the calcined molded body is heated at a temperature increase rate of 300 ° C./hr and calcined at 1500 ° C. for 2 hours to prepare a target.
이와 같은 본 발명에 따른 인듐 산화물 타겟 제조방법으로 제조된 타겟은 겉보기밀도가 6.64로 이론밀도의 95%를 나타낸다.
The target prepared by the method for producing an indium oxide target according to the present invention has an apparent density of 6.64, representing 95% of the theoretical density.
(실시예)(Example)
도 1에 도시된 반응장치 개요도와 같이 교반과 가열이 가능한 맨틀(10)에 장착되어 있는 4구 유리질 반응용기(2ℓ)에 부탄올 470.51g을 투입하고 마그네틱 스틸러(magnetic stirrer)로 300rpm으로 교반하는 상태에서 인듐아세테이트 198.94g, 주석아세테이트 8.49g을 각각 칭량하여 천천히 투입한 후 110℃로 가열하였다. 1, 470.51 g of butanol was added to a four-necked glassy reaction vessel (2 L) mounted on a
이때 반응용기 상단 뚜껑의 3구는 모두 막고 나머지 1구에 냉각기(20)를 설치하여 증발되는 부탄올 및 부틸아세테이트가 응축되도록 함으로써, 부탄올과 부틸아세테이트의 증발을 억제하였다. At this time, all three holes of the upper lid of the reaction vessel were blocked and the
혼합물은 교반을 지속하며 110℃까지 온도가 상승된 시점부터 온도를 유지하며 24시간 합성을 지속한 후 온도가 상온이 될 때까지 교반을 계속 실시하였다. The mixture was kept stirring and the temperature was maintained from the point where the temperature was raised to 110 ° C., and the synthesis was continued for 24 hours, and then the stirring was continued until the temperature became room temperature.
완전히 식은 상태의 합성이 완료된 혼합물은 진공 회전증발기(Vacuum Rotary Evaporator)에서 60℃에서 24시간 가동하여 혼합물 내의 부탄올과 부틸아세테이트를 증발시켜 응축용기에 포집하여 완전히 건조된 합성물을 얻었다.The completely cooled mixture was operated at 60 ° C. for 24 hours in a vacuum rotary evaporator to evaporate butanol and butyl acetate in the mixture to collect in a condensation vessel to obtain a completely dried composite.
건조된 합성물의 결정상은 도 2의 엑스선회절분석 결과 (A)에 나타난 대로 수산화인듐 결정상이며, 상기 수산화인듐 합성물을 300℃에서 10시간 하소하면, 주석이 고용된 산화인듐을 얻을 수 있었다. The crystal phase of the dried composite was an indium hydroxide crystal phase as shown in X-ray diffraction analysis (A) of FIG. 2. When the indium hydroxide composite was calcined at 300 ° C. for 10 hours, indium oxide in which tin was dissolved could be obtained.
이때 얻어진 주석이 고용된 산화인듐의 입자크기는 도 3의 주사전자현미경 사진에 나타난 대로 10~30nm 이었으며, 비표면적은 140m2/g이었으며, 결정상은 도 2의 엑스선회절분석 결과인 (B)에 나타난 대로 인듐산화물과 동일한 빅스바이트(bixbyte)를 나타내었으며, 엑스선회절 피크 값이 약간 이동되어 있는 것으로 주석이 고용된 인듐산화물임을 확인할 수 있었다.The particle size of indium oxide in which tin was obtained was 10-30 nm, as shown in the scanning electron micrograph of FIG. 3, the specific surface area was 140 m 2 / g, and the crystal phase was obtained in (B), which is the result of X-ray diffraction analysis of FIG. 2. As shown, it showed the same bixbyte as indium oxide, and the X-ray diffraction peak value was slightly shifted to confirm that tin was a solid solution of indium oxide.
이렇게 제조된 분말은 물과 분산제를 함께 넣고 어트리션밀에서 6시간 해쇄하고 여기에 결합제, 이형제 등을 투입하여 슬러리 상태로 만들어서 스프레이드라이어를 이용하여 분말 성형을 위한 과립으로 제조하였다. The powder thus prepared was put together with water and a dispersant, pulverized in an attrition mill for 6 hours, and added with a binder, a mold release agent, and the like to make a slurry, thereby preparing granules for powder molding using a spray dryer.
제조된 과립은 분말성형프레스를 사용하여 200kg/cm2의 압력으로 1차 성형한 후 2,000kg/cm2의 압력으로 상온 등압 성형하여 타겟의 성형체를 제조하였다.The prepared granules were first molded using a powder molding press at a pressure of 200 kg / cm 2 , and then subjected to isothermal pressure molding at a pressure of 2,000 kg / cm 2 to prepare a molded body of the target.
상기의 과정을 거쳐 제조된 타겟의 성형체는 과립 제조를 위해 투입된 유기물을 완전히 제거하기 위해서 800℃에서 10시간 하소하였다. 하소된 성형체는 300℃/hr의 승온속도로 승온하여 1500℃에서 2시간 소성하여 타겟을 제조하였다. 이렇게 제조된 타겟은 겉보기밀도가 6.81로 이론밀도의95%를 나타내었다.
The molded product of the target prepared through the above process was calcined at 800 ° C. for 10 hours in order to completely remove the organic material introduced for granulation. The calcined molded body was heated to a temperature increase rate of 300 ° C / hr and calcined at 1500 ° C for 2 hours to prepare a target. The target thus prepared had an apparent density of 6.81, representing 95% of the theoretical density.
Claims (4)
A metal acetate composed of 1.9 mol to 2 mol of indium acetate, 0.4 mol or less of tin acetate and butanol react with each other to synthesize tin in solid solution of indium hydroxide, and indium hydroxide in which tin is dissolved is calcined at 300 ° C. A method for producing indium oxide powder in which tin is dissolved.
상기 부탄올은 n-부탄올, tert-부탄올, 2-부탄올 및 Iso-부탄올 중 어느 하나인 것을 특징으로 하는 주석이 고용된 인듐 산화물 분말 제조방법.
The method of claim 1,
The butanol is a tin-solid indium oxide powder manufacturing method characterized in that any one of n-butanol, tert-butanol, 2-butanol and Iso-butanol.
(2) 합성된 주석이 고용된 수산화인듐을 300℃의 온도에서 하소함으로써, 주석이 고용된 산화인듐 분말을 제조하는 단계로 구성되는 것을 특징으로 하는 주석이 고용된 인듐 산화물 분말 제조방법.
(1) adding metal acetate (indium acetate, tin acetate mixture) to butanol to synthesize indium hydroxide in which tin is dissolved;
(2) A method for producing indium oxide powder in which tin is dissolved, comprising calcining indium hydroxide dissolved in synthesized tin at a temperature of 300 ° C. to produce indium oxide powder in which tin is dissolved.
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| JPH06329415A (en) * | 1993-05-26 | 1994-11-29 | Japan Energy Corp | Production of indium oxide-tin oxide powder |
| KR100670621B1 (en) | 2001-08-13 | 2007-01-17 | 도와 고교 가부시키가이샤 | Tin-containing indium oxides, a process for producing them, a coating solution using them and electrically conductive coatings formed of them |
| KR20090087702A (en) * | 2008-02-13 | 2009-08-18 | 삼성코닝정밀유리 주식회사 | Indium tin oxide sintered body and indium tin oxide target |
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2010
- 2010-11-18 KR KR1020100114727A patent/KR101279541B1/en active IP Right Grant
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06329415A (en) * | 1993-05-26 | 1994-11-29 | Japan Energy Corp | Production of indium oxide-tin oxide powder |
| KR100670621B1 (en) | 2001-08-13 | 2007-01-17 | 도와 고교 가부시키가이샤 | Tin-containing indium oxides, a process for producing them, a coating solution using them and electrically conductive coatings formed of them |
| KR20090087702A (en) * | 2008-02-13 | 2009-08-18 | 삼성코닝정밀유리 주식회사 | Indium tin oxide sintered body and indium tin oxide target |
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