KR20050007661A - Method for synthesizing quantum dot using the metal powder - Google Patents
Method for synthesizing quantum dot using the metal powder Download PDFInfo
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- KR20050007661A KR20050007661A KR1020030047196A KR20030047196A KR20050007661A KR 20050007661 A KR20050007661 A KR 20050007661A KR 1020030047196 A KR1020030047196 A KR 1020030047196A KR 20030047196 A KR20030047196 A KR 20030047196A KR 20050007661 A KR20050007661 A KR 20050007661A
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- metal powder
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- 238000000034 method Methods 0.000 title claims abstract description 72
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 61
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- 230000002194 synthesizing effect Effects 0.000 title 1
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 9
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 8
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- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 4
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- 239000000126 substance Substances 0.000 description 3
- 229910000673 Indium arsenide Inorganic materials 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
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- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 2
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/324—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S438/00—Semiconductor device manufacturing: process
- Y10S438/962—Quantum dots and lines
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- Luminescent Compositions (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
Abstract
Description
본 발명은 양자점(quantum dot) 형성방법에 관한 것으로서, 더욱 상세하게는 (a)용매로 희석한 절연체전구체와 금속분말을 섞어 혼합한 후 교반하는 단계; (b)상기 금속분말이 용해된 절연체전구체 용액을 기판상에 성형하는 단계; 및 (c)상기 금속분말이 용해된 절연체전구체 용액이 성형된 기판을 열처리 하는 단계로 구성된다.The present invention relates to a method for forming a quantum dot, and more particularly, (a) mixing a mixture of insulator precursors and metal powder diluted with a solvent, followed by stirring; (b) forming an insulator precursor solution in which the metal powder is dissolved on a substrate; And (c) heat-treating the substrate on which the insulator precursor solution in which the metal powder is dissolved is formed.
상기 양자점이란, 물질이 수십 나노미터 크기를 가지게 되면 양자 효과(Quantum effect)라는 새로운 물성을 보이게 되는데 이러한 양자효과를 나타내는 물리학적 소단위체를 의미한다.The quantum dot, when the material has a size of several tens of nanometers shows a new property called a quantum effect (Quantum effect) means a physical subunit exhibiting this quantum effect.
종래 양자점 형성방법에 대하여는 (ⅰ) 생성된 양자점들의 위치에 따라, 기판 위에 양자점을 형성, 성장 [GaAs 기판 위에 InAs, InP 기판 위에 InAs를 성장] 시키는 방법과, (ⅱ) 기판 또는 절연체 박막 내에 형성하는 방법과, (ⅲ) 기판 위에 양자점을 선택된 영역에만 형성시킨 후 그 위에 다층의 박막(Multi-Layer Thin Film)을 입히는 방법과, (ⅳ) 기존의 스퍼터와 진공 증발 증착법, 화학 기상 증착법, 에피택시 방법을 그대로 사용하면서 입자의 크기와 분포상태 그리고 응집이 일어나는 효과를 최소화하려는 노력을 하고 있으며 공정 중에 생기는 문제점들을 해결, 응용하는 방법과, (ⅴ) 전구체를 기상화시켜 열증발을 이용한 불활성기체응축방법과, (ⅵ) Microwave Plasma, Laser Ablation을 이용하는 기상합성 방법과, (ⅶ) 금속 유기물을 연소화염이나 Hot-Wall Reactor를 이용하여 분해 합성하는 화학기상 응축공정을 이용한 방법과, (ⅷ) 에어 졸 분사 방법을 응용하여 상압 혹은 낮은 진공도에서 금속/합금, 세라믹 나노 분말 뿐만 아니라, 코팅 혹은 도핑형태의 나노 복합분말, 또는 기판에 직접 분사시켜 다량의 또한 좁은 밀도 분포를 갖는 나노 입자를 포함하는 재료를 제조하는 방법과, (ⅸ) 형광체 입자사이의 응집을 방지하고 전구체를 제조하여 핵 성장에 의하여 조립, 성장시키는 것으로 용매의 존재 하에서 형광체 원료물질의 수용액과 발광효과를 갖는 금속을 포함하는 화합물의 수용액을 혼합하여 석출시킨 후 이를 기상의 형광체 원료물질과 열처리하여 반응시켜 발광중심을 첨가한 나노 입자 형광체를 제조하여 기판에 부착시키는 화학적인 방법과, (ⅹ) 이온주입(Ion Implantation)공정을 응용하여 가속 전압과 기판의 온도를 조절하여 기판 내에 원하는 금속 입자를 형성, 그 분포까지 정확하게 조절하는 방법 등이 제시되고 있다.The conventional quantum dot forming method includes (i) forming a quantum dot on a substrate according to the position of the quantum dots generated, and growing [InAs growing on a GaAs substrate, InAs growing on an InP substrate], and (ii) forming in a substrate or an insulator thin film. And (i) forming a quantum dot on a selected region only on a substrate and then applying a multi-layer thin film thereon, (i) conventional sputtering and vacuum evaporation deposition, chemical vapor deposition, epi Efforts have been made to minimize particle size, distribution, and agglomeration effects while using the taxi method, and to solve and apply problems in the process, and (i) inert gases using thermal evaporation by vaporizing precursors. Condensation method, (i) vapor phase synthesis method using microwave plasma and laser ablation, and (i) metal organic matter using combustion flame or hot-wall reactor By using chemical vapor condensation process to decompose and synthesize, and (i) air sol spraying method, in addition to metal / alloy, ceramic nanopowder at normal pressure or low vacuum, as well as coating or doping nanocomposite powder or substrate. Method of producing a material comprising a large amount of nanoparticles having a narrow density distribution by direct injection, (i) the presence of a solvent to prevent aggregation between the phosphor particles and to prepare a precursor to assemble and grow by nuclear growth After mixing and depositing an aqueous solution of a phosphor raw material and an aqueous solution of a compound containing a metal having a luminescent effect, and reacting it by heat treatment with the phosphor raw material of the gas phase to prepare a nanoparticle phosphor added with a light emitting center to attach to the substrate Acceleration voltage and substrate on by means of chemical method and (i) ion implantation process A has been proposed a method of accurately controlled to form the desired metal particles, their distribution in the substrate to control.
그러나, 상기 종래의 양자점 형성방법들은 입자의 정확한 분포 상태 제어, 분사된 막의 정확한 두께 조절이 용이하지 않고 여러 단계를 거치는 등 공정이 복잡하여 생산성(Throughput)이 떨어지거나 제조단가가 높다는 문제점이 있었다.However, the conventional method for forming quantum dots has a problem that productivity is low or manufacturing cost is high due to complicated processes such as precise distribution control of particles and precise thickness control of the sprayed film.
또한, 상기 종래의 양자점 형성방법들 중 화학적 접근 방법에 있어서는 수용액이나 스프레이 분사방식을 사용하여 나노 입자를 제조시 나노 입자의 응결, 소결 및 열처리에 따른 벌크화로 인하여 입자의 응집 현상을 극복하기 위하여 다양한 촉매 및 첨가제가 필요하다는 문제점과 공정의 수율(Yield)이 낮다는 문제점도 있었다. 또한 기존의 분말과 고분자의 혼합으로 나노 입자가 포함된 고분자를 제조하는 경우 처음부터 분말을 수십 내지 수 나노미터의 크기로 제조해야 하는 어려움이있다.In addition, in the chemical approach of the conventional quantum dot forming method in order to overcome the agglomeration of the particles due to the bulking due to the condensation, sintering and heat treatment of the nanoparticles when manufacturing the nanoparticles using an aqueous solution or spray injection method There was a problem in that catalysts and additives were needed and a low yield in the process. In addition, when manufacturing a polymer containing nanoparticles by mixing a conventional powder and a polymer, there is a difficulty in manufacturing the powder to a size of several tens to several nanometers from the beginning.
본 발명자들은 상기와 같은 문제점을 해결하기 위하여 연구한 결과 금속 분말과 상기 금속을 용해시킬 수 있는 절연체전구체를 혼합하여 교반한 후, 이를 기판상에 도포하여 특정조건에서 열처리를 행하면 열처리과정 중에 미세하고 균일한 나노크기를 가지는 금속산화물의 양자점을 형성할 수 있음을 발견하였고, 이를 이용하여 간단하고 경제적인 양자점 형성방법을 제공할 수 있음을 알게 되었다.The present inventors have studied to solve the above problems, and after mixing and stirring the metal powder and the insulator precursor capable of dissolving the metal, it is applied to a substrate and subjected to heat treatment under a specific condition and fine during the heat treatment process It has been found that quantum dots of a metal oxide having a uniform nano size can be formed, and that the method can provide a simple and economical method for forming quantum dots.
본 발명은 박막제조장비를 이용한 금속층을 제조할 필요가 없는 간단하며 경제적이고, 동시에, 금속 분말의 종류, 금속 분말의 양 또는 열처리조건을 조절함으로써 양자점의 크기, 밀도 및 분포도를 용이하게 조절할 수 있는 양자점 형성방법을 제공하는 것을 목적으로 한다.The present invention is simple and economical without the need to manufacture a metal layer using a thin film manufacturing equipment, and at the same time, it is possible to easily control the size, density and distribution of the quantum dots by adjusting the type of metal powder, the amount of metal powder or heat treatment conditions It is an object to provide a method for forming a quantum dot.
또한, 본 발명은 재료를 액상으로 제조함으로써 스핀코팅, 스프레이, 캐스팅, 제팅, 디스펜싱 등의 도포방법을 사용할 수 있어 원하는 형상의 도포, 대면적의 도포, 굴곡면에의 도포 및 선택된 부분의 도포가 가능한 양자점 형성방법을 제공하는 것을 목적으로 한다.In addition, the present invention can use a coating method such as spin coating, spraying, casting, jetting, dispensing by manufacturing the material in the liquid phase, so that the coating of the desired shape, the large area, the coating on the curved surface and the coating of the selected part It is an object of the present invention to provide a method for forming quantum dots.
도 1a는 금속분말이 용해된 절연체전구체를 기판상에 도포한 것을 나타내는 도식적 단면도이다.1A is a schematic cross-sectional view showing an insulator precursor in which metal powder is dissolved on a substrate.
도 1b는 열처리후 기판상에 양자점이 형성된 결과를 나타내는 도식적 단면도이다.1B is a schematic cross-sectional view showing a result of quantum dots formed on a substrate after heat treatment.
도 2은 본 발명의 양자점 형성방법의 일실시예에 따라 형성된 구리 산화물 양자점의 투과전자현미경 사진이다.2 is a transmission electron micrograph of a copper oxide quantum dot formed according to an embodiment of the method of forming a quantum dot of the present invention.
도 3은 본 발명의 양자점 형성방법의 일실시예에 따라 형성된 철 산화물 양자점의 투과전자현미경 사진이다.3 is a transmission electron micrograph of an iron oxide quantum dot formed in accordance with an embodiment of the method of forming a quantum dot of the present invention.
도 4는 본 발명의 양자점 형성방법의 일실시예에 따라 형성된 망간 산화물 양자점의 투과전자현미경 사진이다.4 is a transmission electron micrograph of a manganese oxide quantum dot formed in accordance with an embodiment of the method of forming a quantum dot of the present invention.
도 5a는 400℃에서 1시간 열처리 하여 형성된 구리산화물 양자점의 투과전자현미경 사진이다.5A is a transmission electron micrograph of a copper oxide quantum dot formed by heat treatment at 400 ° C. for 1 hour.
도 5b는 300℃에서 2시간 열처리 하여 형성된 구리산화물 양자점의 투과전자현미경 사진이다.5B is a transmission electron micrograph of a copper oxide quantum dot formed by heat treatment at 300 ° C. for 2 hours.
본 발명은 양자점 형성방법에 있어서 (a) 용매로 희석한 절연체전구체와 금속분말을 섞어 혼합하고 교반하는 단계; (b) 상기 금속 분말이 용해된 절연체전구체 용액을 기판상에 성형하는 단계; 및 (c) 상기 성형된 기판을 단계적으로 최고온도가 200℃ 내지 500℃가 되도록 열처리하는 단계를 포함하는 것을 특징으로 하는양자점 형성방법을 제공한다.The present invention provides a method for forming a quantum dot comprising the steps of: (a) mixing and stirring an insulator precursor diluted with a solvent and a metal powder; (b) forming an insulator precursor solution in which the metal powder is dissolved on a substrate; And (c) heat-treating the molded substrate in a stepwise manner such that the maximum temperature is 200 ° C. to 500 ° C.
본 발명은 상기 금속분말의 금속이 구리(Cu), 아연(Zn), 주석(Sn), 코발트(Co), 철(Fe), 카드늄(Cd), 납(Pb), 마그네슘(Mg), 바륨(Ba), 몰리브덴(Mo), 인듐(In), 니켈(Ni), 텅스텐(W), 비스무트(Bi), 은(Ag), 망간(Mn) 및 이들의 합금으로 이루어지는 군으로부터 선택되는 것을 특징으로 하는 양자점 형성 방법을 제공한다.In the present invention, the metal of the metal powder is copper (Cu), zinc (Zn), tin (Sn), cobalt (Co), iron (Fe), cadmium (Cd), lead (Pb), magnesium (Mg), barium (Ba), molybdenum (Mo), indium (In), nickel (Ni), tungsten (W), bismuth (Bi), silver (Ag), manganese (Mn), and alloys thereof. A quantum dot forming method is provided.
본 발명은 상기 절연체전구체가 금속이 용해될 수 있는 산성전구체인 것을 특징으로 하는 양자점 형성방법을 제공한다.The present invention provides a method for forming a quantum dot, characterized in that the insulator precursor is an acid precursor in which metal can be dissolved.
본 발명은 상기 산성전구체가 카르복실기(-COOH)를 포함하는 산성전구체인 것을 특징으로 하는 양자점 형성방법을 제공한다.The present invention provides a method for forming a quantum dot, characterized in that the acid precursor is an acid precursor containing a carboxyl group (-COOH).
본 발명은 상기 용매가 N-메틸피롤리돈(NMP), 물(Water), N-디메틸아세트아미드(N-dimethylacetamide), 디글림(diglyme) 중에서 선택되는 1종 이상인 것을 특징으로 하는 양자점 형성방법을 제공한다.The method of the present invention is characterized in that the solvent is at least one selected from N-methylpyrrolidone (NMP), water (Water), N-dimethylacetamide (N-dimethylacetamide), diglyme (diglyme) To provide.
본 발명은 상기 (a)단계 이후에 상기 금속분말 및 절연체전구체가 충분히 반응하도록 하는 추가 교반단계를 더욱 포함하는 것을 특징으로 하는 양자점 형성방법을 제공한다.The present invention provides a method for forming a quantum dot, further comprising an additional stirring step for sufficiently reacting the metal powder and the insulator precursor after the step (a).
본 발명은 상기 (c)단계 이전에 상기 금속분말이 용해된 절연체전구체 용액이 성형된 기판을 80℃ 내지 150℃에서 중간 열처리를 수행하는 단계를 더욱 포함하는 것을 특징으로 하는 양자점 형성방법을 제공한다.The present invention provides a method for forming a quantum dot further comprising the step of performing an intermediate heat treatment at 80 ° C to 150 ° C on the substrate on which the insulator precursor solution in which the metal powder is dissolved is formed before step (c). .
본 발명은 상기 (a)단계 이전에 상기 절연체전구체와 용매를 혼합한 용액을상기 기판상에 증착한 후, 80℃ 내지 150℃로 제2 중간 열처리를 수행하는 단계를 더욱 포함하는 것을 특징으로 하는 양자점 형성방법을 제공한다.The present invention further comprises the step of performing a second intermediate heat treatment at 80 ° C. to 150 ° C. after depositing the solution in which the insulator precursor and the solvent are mixed on the substrate before step (a). Provided is a method of forming a quantum dot.
본 발명은 상기 금속 분말이 용해된 절연체전구체를 상기 기판상에 성형하는 방법이 스핀 코팅(Spin coating), 제팅(Jetting), 분사(Spray), 프린팅(Printing), 브러싱(Brusing), 캐스팅(Casting), 블레이드 코팅(Blade coating), 디스펜싱(Dispensing), 몰딩(Molding)방법 중에서 선택되는 어느 하나의 방법인 것을 특징으로 하는 양자점 형성방법을 제공한다.According to the present invention, the method of forming the insulator precursor in which the metal powder is dissolved on the substrate is performed by spin coating, jetting, spraying, printing, brushing, casting, and the like. ), A blade coating, a dispensing, and a molding method are provided.
본 발명은 상기 용매가 N-메틸피롤리돈, 물, N-디메틸아세드아미드, 디글림 중에서 선택되는 1종 이상인 것을 특징으로 하는 양자점 형성방법을 제공한다.The present invention provides a method for forming a quantum dot, characterized in that the solvent is at least one selected from N-methylpyrrolidone, water, N-dimethylacedamide, diglyme.
본 발명은 상기 금속 분말과 절연체전구체를 혼합한 후 교반하는 단계 (a)에서 금속분말의 양의 조절 및/또는 상기 열처리하는 단계 (c)에서 열처리 조건의 조절에 의하여 양자점의 크기, 밀도, 분포도를 제어하는 것을 특징으로 하는 양자점 형성방법을 제공한다.The present invention is the size, density, distribution of the quantum dots by controlling the amount of metal powder in the step (a) and / or the heat treatment step (c) in the step (a) of mixing and stirring the metal powder and the insulator precursor It provides a method for forming a quantum dot characterized in that for controlling.
본 발명은 상기한 방법에 의하여 형성된 금속산화물 양자점이 분산된 것을 특징으로 하는 고분자 박막을 제공한다.The present invention provides a polymer thin film, wherein the metal oxide quantum dots formed by the above method are dispersed.
본 발명은 상기 금속산화물 양자점이 분산된 고분자 박막을 갖는 것을 특징으로 하는 전자부품소자를 제공한다.The present invention provides an electronic component device having a polymer thin film in which the metal oxide quantum dots are dispersed.
이하에서, 본 발명의 금속 분말을 이용한 양자점 형성방법을 공정과 함께 상세히 설명한다.Hereinafter, the quantum dot forming method using the metal powder of the present invention will be described in detail with the process.
제 1 공정: 기판의 준비First step: preparation of the substrate
(1) 기판의 준비 공정(1) substrate preparation step
기판을 트리클로로에틸렌(Trichloroethylene, TCE), 아세톤, 메탄올로 각각 5분간 초음파 세척을 실시하여 기판상의 불순물을 제거한 절연막이 도포될 수 있는 기판을 준비한다.Ultrasonic cleaning is performed on the substrate with trichloroethylene (TCE), acetone, and methanol for 5 minutes, thereby preparing a substrate on which an insulating film from which impurities on the substrate are removed can be applied.
(2) 제2 중간 열처리 공정 :(2) Second intermediate heat treatment process:
본 발명의 일실시예에 따른 양자점 형성방법에 의하여 생성되는 금속산화물 양자점(4)의 밀도를 조절하기 위하여, 하기 제 2 공정을 수행하기 전에 절연체전구체와 용매를 혼합한 용액을 기판상에 증착한 후, 80℃ 내지 150℃의 오븐에서 제2 중간 열처리 단계를 수행한다. 상기 제 2 중간 열처리 단계에 의하여 양자점(4)의 균질도 및 밀도를 더욱 일정하게 형성할 수 있게 된다. 제2 중간 열처리 단계는 선택적 단계이다. 상기 용매는 특별히 한정되지 않고, 절연체전구체의 종류에 따라 다른 것을 선택하여 사용 가능하지만, 바람직하게는 N-메틸피롤리돈(NMP), 물(Water), N-디메틸아세트아미드(N-dimethylacetamide), 디글림(diglyme) 중에서 선택되는 1종 이상을 사용한다.In order to control the density of the metal oxide quantum dots (4) produced by the method for forming quantum dots according to an embodiment of the present invention, a solution in which an insulator precursor and a solvent are mixed is deposited on a substrate before performing the second process. Thereafter, a second intermediate heat treatment step is performed in an oven at 80 ° C to 150 ° C. By the second intermediate heat treatment step, the homogeneity and density of the quantum dots 4 can be formed more uniformly. The second intermediate heat treatment step is an optional step. The solvent is not particularly limited and may be selected and used according to the type of insulator precursor. Preferably, the solvent is N-methylpyrrolidone (NMP), water, or N-dimethylacetamide. Use at least one selected from diglyme.
제 2 공정 : 금속 분말과 절연체전구체와의 혼합Second Step: Mixing of Metal Powder and Insulator Precursor
절연체전구체와 반응할 수 있는 금속분말을 용매에 희석된 절연체전구체와 혼합하고, 교반한 후, 금속분말과 절연체전구체가 충분히 반응할 수 있도록 추가 교반한다. 상기 추가 교반의 온도 및 시간은 특정범위로 한정되는 것은 아니며, 금속분말과 절연체전구체의 종류에 따라 적절하게 선택될 수 있으나, 상온에서 5분 내지 24시간 동안 교반하며 유지시키는 것이 바람직하다.The metal powder capable of reacting with the insulator precursor is mixed with the insulator precursor diluted in the solvent, and then stirred, followed by further stirring to sufficiently react the metal powder and the insulator precursor. The temperature and time of the additional stirring is not limited to a specific range, and may be appropriately selected according to the type of metal powder and the insulator precursor, but it is preferable to maintain the mixture for 5 minutes to 24 hours at room temperature.
사용가능한 금속분말은 순수 금속분말 또는 순수 금속의 합금 금속분말이다. 본 발명에서 사용 가능한 금속 분말의 금속으로는 구리, 아연, 주석, 코발트, 철, 카드늄, 납, 마그네슘, 바륨, 몰리브덴, 인듐, 니켈, 텅스텐, 비스무트, 은, 망간 및 이들의 합금으로 구성되는 군으로부터 선택된 것을 사용할 수 있다. 또한, 분말의 입자의 크기는 제약이 없고 전구체와의 반응성에 따라 달라질 수 있으나, 1 ㎛ 이하가 바람직하다.Usable metal powders are pure metal powders or alloy metal powders of pure metals. Metals of the metal powder usable in the present invention include copper, zinc, tin, cobalt, iron, cadmium, lead, magnesium, barium, molybdenum, indium, nickel, tungsten, bismuth, silver, manganese, and alloys thereof. The one selected from can be used. In addition, the size of the particles of the powder is not limited and may vary depending on the reactivity with the precursor, preferably 1 μm or less.
혼합되는 금속 분말의 양은 특정 범위로 한정되는 것은 아니다. 금속과 절연체전구체의 반응에 의해 금속 산화물이 형성되므로 금속 분말의 양을 조절하여 금속 산화물 양자점의 밀도를 조절할 수 있다. 예를 들어 금속 분말의 양을 증가시키면, 금속 산화물 양자점의 밀도가 증가된다.The amount of the metal powder to be mixed is not limited to a specific range. Since the metal oxide is formed by the reaction of the metal and the insulator precursor, the density of the metal oxide quantum dots may be controlled by controlling the amount of the metal powder. For example, increasing the amount of metal powder increases the density of the metal oxide quantum dots.
본 발명의 절연체전구체는 구리, 아연, 주석, 코발트, 철, 카드늄, 납, 마그네슘, 바륨, 몰리브덴, 인듐, 니켈, 텅스텐, 비스무트, 은, 망간의 분말 또는 이들 금속의 합금 분말과 반응하여 금속산화물을 석출할 수 있는 절연체전구체이다. 본 발명에서 사용가능한 절연체전구체는 산성 절연체전구체이고, 바람직하게는 카르복실기(R-COOH)를 포함하는 산성 절연체전구체이다. 상기 용매는 특정 용매로 한정되는 것은 아니며, 절연체전구체의 종류에 따라 다른 것을 사용할 수 있으나, N-메틸피롤리돈, 물, N-디메틸아세트아미드, 디글림 중에서 선택되는 1종 이상이 바람직하다.The insulator precursor of the present invention reacts with a powder of copper, zinc, tin, cobalt, iron, cadmium, lead, magnesium, barium, molybdenum, indium, nickel, tungsten, bismuth, silver, manganese or an alloy powder of these metals. It is an insulator precursor that can deposit. The insulator precursor usable in the present invention is an acid insulator precursor, preferably an acid insulator precursor containing a carboxyl group (R-COOH). The solvent is not limited to a specific solvent, and may be different depending on the type of insulator precursor, but at least one selected from N-methylpyrrolidone, water, N-dimethylacetamide, and diglyme is preferable.
제 3 공정 : 금속분말이 용해된 절연체전구체의 기판상으로의 성형Third step: forming the insulator precursor in which the metal powder is dissolved onto the substrate
금속분말이 용해된 절연체전구체 용액을 기판상에 성형한다. 본 발명은 액상의 재료를 도포하므로 성형방법으로서 스핀 코팅(Spin coating), 제팅(Jetting), 분사(Spray), 프린팅(Printing), 브러싱(Brusing), 캐스팅(Casting), 블레이드 코팅(Blade coating), 디스펜싱(Dispensing), 몰딩(Molding)방법 중 어느 하나의 방법이 사용 가능하다. 또한, 평평한 기판이외에 굴곡이 있는 면에 도포가 가능하고, 상기 제팅 방법, 디스펜싱 방법을 사용하면, 선택된 부분에만 양자점의 형성이 가능하다.An insulator precursor solution in which metal powder is dissolved is formed on a substrate. Since the present invention applies a liquid material, as a forming method, spin coating, jetting, spraying, printing, brushing, casting, blade coating, etc. Any one of a dispensing and molding method may be used. In addition, it is possible to apply to the curved surface other than the flat substrate, and by using the jetting method and the dispensing method, it is possible to form quantum dots only in selected portions.
도 1a는 금속분말이 용해된 절연체전구체를 기판상에 도포한 것을 나타내는 도식적 단면도이다.1A is a schematic cross-sectional view showing an insulator precursor in which metal powder is dissolved on a substrate.
제 4 공정: 중간 열처리4th process: intermediate heat treatment
상기 제 3 공정에 의하여 금속분말이 용해된 절연체전구체 용액이 성형된 상기 기판을 80℃ 내지 150℃로 중간 열처리를 수행한다. 상기 중간 열처리에 의해 용매는 증발되어 고분자의 점성이 증가하여 이온의 이동이 제한된다.By performing the third process, the substrate on which the insulator precursor solution in which the metal powder is dissolved is formed is subjected to an intermediate heat treatment at 80 ° C to 150 ° C. By the intermediate heat treatment, the solvent is evaporated to increase the viscosity of the polymer to limit the movement of ions.
제 5 공정: 열처리5th process: heat treatment
상기 제 4 공정인 중간 열처리 단계를 거친 상기 기판(1)을 질소 분위기의 관상로에서 단계적으로 최고온도가 200℃ 내지 500℃, 바람직하게는 250℃ 내지 400℃가 되도록 열처리한다. 상기 열처리의 최고온도 및 처리시간은 사용하는 금속분말 및 절연체전구체의 종류에 따라 상기 범위내에서 적절하게 선택한다.The substrate 1, which has undergone the intermediate heat treatment step as the fourth process, is heat-treated in a tubular furnace of nitrogen atmosphere step by step so that the maximum temperature is 200 ° C to 500 ° C, preferably 250 ° C to 400 ° C. The maximum temperature and treatment time of the heat treatment are appropriately selected within the above ranges depending on the type of metal powder and insulator precursor used.
열처리 온도가 높으면 반응이 활발하여 금속 산화물 형성속도가 증가하나 온도가 높을수록 이온의 이동과 형성된 산화물의 확산이 빨라진다. 따라서, 열처리 단계에서 열처리 최고 온도, 열처리 유지 시간, 최고 온도까지의 도달시간 및 중간 열처리 단계의 유무 등을 변화시켜 반응속도, 이온의 이동 및 금속산화물의 확산을 조절하면 양자점의 크기와 분포도를 용이하게 조절할 수 있다.The higher the heat treatment temperature, the more active the metal oxide formation rate is, but the higher the temperature, the faster the movement of ions and the diffusion of the formed oxide. Therefore, the size and distribution of quantum dots can be easily controlled by controlling the reaction rate, ion movement and diffusion of metal oxides by changing the maximum heat treatment temperature, heat treatment holding time, reaching time to maximum temperature, presence of intermediate heat treatment stages, etc. Can be adjusted.
도 1b는 열처리후 기판상에 양자점이 형성된 결과를 나타내는 도식적 단면도이다.1B is a schematic cross-sectional view showing a result of quantum dots formed on a substrate after heat treatment.
실시예Example
실시예 1 : 구리분말을 이용한 양자점의 형성Example 1 Formation of Quantum Dots Using Copper Powder
평균입도가 4 ㎛인 구리분말과 절연체전구체로서 NMP용매에 희석한 BPDA-PDA(Biphenyltetracarboxylic dianhydride-p-phenylenediamine)폴리아믹산을 혼합한 후 교반하였다. 상기 혼합물을 상온에서 24시간 두어 충분히 반응시켰다. 반응시킨 구리 분말이 용해된 폴리아믹산 절연체전구체 용액을 트리클로로에틸렌, 아세톤, 메탄올로 각각 5분간 초음파 세척한 기판상에 스핀코팅의 방법을 이용하여 얇게 성형하였다. 상기 기판을 100℃에서 30분 동안 중간열처리를 수행하였다. 중간 열처리를 수행한 기판을 단계적으로 가열하여 최고온도 400℃에서 1시간 동안 열처리한 후 상온까지 냉각시켜 구리산화물 양자점을 형성하였다. 도 2는 상기 방법에 의하여 형성된 구리 금속산화물 양자점의 투과전자현미경 사진이다. 상기 구리산화물의 양자점은 10 nm 이하의 크기로 균일하게 분포하고 있음을 확인할 수 있다.Copper powder with an average particle size of 4 μm and BPDA-PDA (Biphenyltetracarboxylic dianhydride-p-phenylenediamine) polyamic acid diluted in NMP solvent as an insulator precursor were mixed and stirred. The mixture was allowed to react for 24 hours at room temperature. The polyamic acid insulator precursor solution in which the reacted copper powder was dissolved was thinly formed on the substrate which was ultrasonically washed with trichloroethylene, acetone, and methanol for 5 minutes using a spin coating method. The substrate was subjected to an intermediate heat treatment at 100 ° C. for 30 minutes. The substrate subjected to the intermediate heat treatment was gradually heated, heat treated at a maximum temperature of 400 ° C. for 1 hour, and then cooled to room temperature to form a copper oxide quantum dot. 2 is a transmission electron micrograph of a copper metal oxide quantum dot formed by the above method. It can be seen that the quantum dots of the copper oxide are uniformly distributed in the size of 10 nm or less.
실시예 2 : 철 분말을 이용한 양자점의 형성Example 2 Formation of Quantum Dots Using Iron Powder
실시예 1에서와 동일한 방법으로 구리 분말 대신에 철 분말을 이용하여 양자점을 형성하였다. 도 3은 철산화물 양자점의 투과전자현미경 사진이다.Quantum dots were formed using iron powder instead of copper powder in the same manner as in Example 1. 3 is a transmission electron microscope photograph of iron oxide quantum dots.
실시예 3 : 망간 분말을 이용한 양자점의 형성Example 3 Formation of Quantum Dots Using Manganese Powder
실시예 1에서와 동일한 방법으로 구리 분말 대신에 망간 분말을 이용하여 양자점을 형성하였다. 도 4는 망간산화물 양자점의 투과전자현미경 사진이다.Quantum dots were formed using manganese powder instead of copper powder in the same manner as in Example 1. 4 is a transmission electron micrograph of a manganese oxide quantum dot.
실시예 4 : 열처리조건의 변화에 따른 양자점의 크기 및 밀도의 조절Example 4 Control of Size and Density of Quantum Dots with Changes in Heat Treatment Conditions
실시예 1에서와 동일한 방법으로 구리금속의 양자점을 형성하면서 열처리 조건을 변화시켜 구리 산화물 양자점을 형성하였다. 도 5a는 400℃에서 1시간 열처리 하여 형성한 구리산화물 양자점의 전자현미경 사진이다. 도 5b는 300℃에서 2시간 열처리 하여 형성한 구리산화물 양자점의 전자현미경 사진이다. 도 5a의 양자점의 밀도가 도 5b의 것보다 더 높은 것을 확인할 수 있다. 따라서, 금속산화물 양자점 형성시에 열처리 조건을 변화시키면 양자점의 크기 및 밀도를 조절할 수 있음을 확인하였다.Copper oxide quantum dots were formed by changing the heat treatment conditions while forming quantum dots of copper metal in the same manner as in Example 1. 5A is an electron micrograph of a copper oxide quantum dot formed by heat treatment at 400 ° C. for 1 hour. 5B is an electron micrograph of a copper oxide quantum dot formed by heat treatment at 300 ° C. for 2 hours. It can be seen that the density of the quantum dots of FIG. 5A is higher than that of FIG. 5B. Therefore, it was confirmed that the size and density of the quantum dots can be controlled by changing the heat treatment conditions at the time of forming the metal oxide quantum dots.
본 발명에 의해 형성되는 금속산화물 입자들은 다음의 표 1에 예시된 바와 같이, 반도체이므로 나노 반도체 양자점이 분산된 유전체는 광소자, 광전소자 등에 응용이 가능하다. 또한, 본 발명에서 제공되는 결과는 신기능을 구현할 수 있는 초고속 광신호 처리소자, 차세대 광자 변조기, 광검출기, 광자도파로 집적 소자, 고효율 정보통신 부품 등에 활용할 수 있고, 철 분말을 이용할 경우 γ-Fe2O3가 생성되므로 자기 매체 등 자성을 이용한 부품으로 이용이 가능할 것이다.As the metal oxide particles formed by the present invention are exemplified in Table 1 below, since the semiconductor is a semiconductor, the dielectric in which the nano semiconductor quantum dots are dispersed may be applied to an optical device, an optoelectronic device, and the like. In addition, the results provided in the present invention can be utilized for ultra-fast optical signal processing devices, next-generation photon modulators, photodetectors, photon waveguide integrated devices, high-efficiency information and communication components that can implement new functions, γ-Fe 2 Since O 3 is generated, it may be used as a magnetic component such as a magnetic medium.
이상에서 설명한 본 발명은, 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자에 있어서, 본 발명의 기술적 사상을 벗어나지 않는 범위내에서 다양한 치환, 변경이 가능하므로 전술한 실시예에 한정되는 것은 아니다.The present invention described above is not limited to the above-described embodiments, since various substitutions and changes can be made by those skilled in the art without departing from the technical spirit of the present invention. .
본 발명의 양자점 형성방법은 공정이 간단하여 경제적이고 분말의 크기에 관계없이 금속분말의 종류, 금속분말의 양, 열처리조건을 조절하여 양자점의 크기, 밀도 및 분포도를 용이하게 조절할 수 있고, 극미세 및 균일한 양자점을 용이하게 형성할 수 있다. 또한, 액체상을 도포하므로 다양한 도포방법이 사용 가능하여 대면적, 굴곡이 있는 면, 선택적인 면에도 도포가 가능하다. 상기와 같은 양자점은 반도체 성질을 가진 금속산화물을 이용하는 경우 반도체로서 이용 가능하다.The quantum dot forming method of the present invention is simple and economical to process and can easily control the size, density and distribution of the quantum dots by adjusting the type of metal powder, the amount of metal powder, heat treatment conditions irrespective of the size of the powder, and very fine And uniform quantum dots can be easily formed. In addition, since the liquid phase is applied, various coating methods can be used, so that it can be applied to a large area, a curved surface, and an optional surface. Such quantum dots can be used as a semiconductor when using a metal oxide having semiconductor properties.
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| KR100849418B1 (en) * | 2007-05-10 | 2008-08-01 | 한양대학교 산학협력단 | Fabrication method of copt nanoparticles |
| US8476055B2 (en) | 2006-05-22 | 2013-07-02 | Korea Advanced Institute Of Science And Technology | Method for preparing metal nanoparticle using metal binding protein |
| KR101413660B1 (en) * | 2012-04-13 | 2014-07-04 | 홍익대학교 산학협력단 | Quantum dot-polymer composite plate for light emitting diode and method for producing the same |
| WO2021235851A1 (en) * | 2020-05-20 | 2021-11-25 | 국방과학연구소 | Quantum dots containing molybdenum, nickel, and sulfur, and method for manufacturing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US8476055B2 (en) | 2006-05-22 | 2013-07-02 | Korea Advanced Institute Of Science And Technology | Method for preparing metal nanoparticle using metal binding protein |
| KR100849418B1 (en) * | 2007-05-10 | 2008-08-01 | 한양대학교 산학협력단 | Fabrication method of copt nanoparticles |
| KR101413660B1 (en) * | 2012-04-13 | 2014-07-04 | 홍익대학교 산학협력단 | Quantum dot-polymer composite plate for light emitting diode and method for producing the same |
| WO2021235851A1 (en) * | 2020-05-20 | 2021-11-25 | 국방과학연구소 | Quantum dots containing molybdenum, nickel, and sulfur, and method for manufacturing same |
| KR20210143673A (en) * | 2020-05-20 | 2021-11-29 | 국방과학연구소 | Quantum dot comprising molybdenum, nickel and sulfur and manufacturing method thereof |
| US11912917B2 (en) | 2020-05-20 | 2024-02-27 | Agency For Defense Development | Quantum dots containing molybdenum, nickel, and sulfur and method for manufacturing same |
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