KR101250859B1 - Quantum dots and Luminescent devices by using these - Google Patents

Quantum dots and Luminescent devices by using these Download PDF

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KR101250859B1
KR101250859B1 KR1020090038993A KR20090038993A KR101250859B1 KR 101250859 B1 KR101250859 B1 KR 101250859B1 KR 1020090038993 A KR1020090038993 A KR 1020090038993A KR 20090038993 A KR20090038993 A KR 20090038993A KR 101250859 B1 KR101250859 B1 KR 101250859B1
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core
shell
solution
trioctylphosphine
quantum dots
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KR20100120011A (en
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최경재
김경남
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/0805—Chalcogenides
    • C09K11/0811—Chalcogenides with zinc or cadmium
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
    • C09K11/881—Chalcogenides
    • C09K11/883—Chalcogenides with zinc or cadmium
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices

Abstract

본 발명은 양자점 핵을 비수계 용매에서 제조하고, 상기 제조된 양자점의 표면에 조성이 다른 양자점으로 껍질을 형성한 후 상기 양자점을 유기용매에 분산 후 이를 발광소자에 적용하기 위한 캡슐을 형성하고, 그 형성된 캡슐을 해당소자에 적층하여 발광소자를 구현하고자 하는 다층 양자점 및 그 다층 양자점을 적용한 발광소자에 관한 것이다. The present invention is to prepare a quantum dot nucleus in a non-aqueous solvent, to form a shell with a quantum dot having a different composition on the surface of the prepared quantum dot and then to disperse the quantum dot in an organic solvent to form a capsule for applying it to a light emitting device, The present invention relates to a multilayer quantum dot to form a light emitting device by laminating the formed capsule on a corresponding device, and a light emitting device to which the multilayer quantum dot is applied.

양자점, 다층 양자점, 발광소자, 나노 Quantum dots, multilayer quantum dots, light emitting device, nano

Description

다층 양자점 및 그 다층 양자점을 적용한 발광소자{Quantum dots and Luminescent devices by using these}Multilayer quantum dots and light emitting devices using the multilayer quantum dots {Quantum dots and Luminescent devices by using these}

본 발명은 다층 양자점 및 그 다층 양자점을 적용한 발광소자에 관한 것으로, 더욱 상세하게는 양자점 핵을 비수계 용매에서 제조하고, 상기 제조된 양자점의 표면에 조성이 다른 양자점으로 껍질을 형성한 후 상기 양자점을 유기용매에 분산 후 이를 발광소자에 적용하기 위한 캡슐을 형성하고, 그 형성된 캡슐을 해당소자에 적층하여 발광소자를 구현하는 것이다. The present invention relates to a multilayer quantum dot and a light emitting device to which the multilayer quantum dot is applied. More particularly, the quantum dot nucleus is prepared in a non-aqueous solvent, and the shell is formed of a quantum dot having a different composition on the surface of the quantum dot. After the dispersion in an organic solvent to form a capsule for applying it to the light emitting device, and to form the capsule to the corresponding device to implement a light emitting device.

양자점은 최근 10여년 동안 많은 연구와 발전을 이룬 물질로써, 양자 구속이라는 특이한 물리적 특성을 지닌다. 따라서, 양자점의 크기를 조절하면 밴드갭이 조절되어 다양한 파장의 에너지를 얻을 수 있게 된다. Quantum dots have been researched and developed in recent decades and have a unique physical property called quantum confinement. Therefore, by adjusting the size of the quantum dot is adjusted the band gap it is possible to obtain energy of various wavelengths.

기존의 양자점 합성방법은 CVD 등과 같은 기상증착법을 이용하여 제조되었다. 또한, 최근에는 유기 및 수용액에서 양자점 코어 및 쉘을 형성하는 방법이 많은 발전을 보이고 있으나, 이와 같은 방법은 제조방법이 기상증착법보다 싸고 용이 한 장점이 있으며, 이렇게 제조된 양자점을 발광소자에 응용한 문헌들이 나타나고 있다. Conventional quantum dot synthesis method was prepared by using a vapor deposition method such as CVD. In addition, in recent years, a method of forming a quantum dot core and a shell in organic and aqueous solutions has been developed, but such a method has an advantage that the manufacturing method is cheaper and easier than the vapor deposition method. Literature is emerging.

기존의 양자점을 이용하여 발광소자에 적용하기 위해서는 레진과 혼합하여 사용되어져야 하는데 이와 같은 방법은 양자점의 응집 및 효율감소를 보이는 단점이 있다. In order to apply to a light emitting device using a conventional quantum dot must be used in combination with the resin, such a method has a disadvantage that shows the aggregation and efficiency of the quantum dot.

본 발명은 발광효율이 좋고, 분산성을 높여주는 다층 양자점을 제조하고, 그 제조된 다층 양자점을 LED 칩 위에 적층하고 건조하며, 그 건조 적층된 LED 칩을 몰딩하여 발광소자를 제조함을 물론, 외부환경에 대한 반응성이 적어 발광소자 제조시 용이함을 주도록 함에 그 목적이 있다.The present invention manufactures a multi-layer quantum dot with good luminous efficiency, improves the dispersibility, laminates the manufactured multi-layer quantum dot on the LED chip and dried, and molding the dried stacked LED chip to manufacture a light emitting device, The purpose of the present invention is to provide ease in manufacturing a light emitting device due to its low reactivity to the external environment.

상기 목적을 달성하기 위한 본 발명은 통상의 방법으로 제조된 코어/쉘 구조의 양자점을 유기용매에 분산 후 이를 발광소자에 적용하기 위한 캡슐을 형성하여 분산성 및 발광효율이 좋은 양자점으로 (코어/쉘)/용매/쉘 구조를 지닌 다층 양자점의 제조함과 동시에 이것을 다시 발광소자에 적층하여 발광소자를 구현하는 방법을 제공하는 것으로, 그 일 실시예로는 통상의 방법으로 제조된 CdTe/CdS(코어/쉘) 을 트리옥틸포스핀(Trioctylphosphine)에 분산시키고, TEOS, 증류수, 염산으로 제 조한 실리카 졸을 상기 트리옥틸포스핀에 분산된 코어/쉘 용액을 넣고 교반한 후 이 용액에 (3-Aminopropyl)트리에톡시실란(triethoxysilane) 용액을 넣고, 그 용액을 증류수와 트리톤(Triton) X-100이 혼합된 용액에 교반하는 상태에서 넣어 제조된 용액을 원심분리를 통하여 증류수를 제거한 후 진공건조기에서 건조하는 것으로 이루어지는 구성과, 상기 구성에 의해 제조된 다층 양자점 및 상기 다층 양자점을 LED 칩 위에 적용시켜 제조된 발광소자에 의한다. In order to achieve the above object, the present invention forms a capsule for dispersing a quantum dot of a core / shell structure manufactured by a conventional method in an organic solvent and then applying the same to a light emitting device. The present invention provides a method of manufacturing a multilayer quantum dot having a shell) / solvent / shell structure and stacking the same on a light emitting device to implement a light emitting device. In one embodiment, CdTe / CdS ( Core / shell) was dispersed in trioctylphosphine, and a silica / sol prepared with TEOS, distilled water, and hydrochloric acid was added to the trioctylphosphine, followed by stirring. Aminopropyl) triethoxysilane solution was added, and the solution was added to a solution mixed with distilled water and Triton X-100 in a state of stirring to remove distilled water by centrifugation. The multi-layer quantum dot and the multi-layer quantum dots produced by the configuration and the configuration formed by the dried in a vacuum dryer is due to the light-emitting device manufactured by applying on the LED chip.

상술한 바와 같은 본 발명은 장기간 동안 다양한 파장을 지님은 물론, 발광효율이 좋고, 분산성을 높여주는 효과가 있음은 물론, 상기의 방법으로 제조된 다층 양자점은 레진과 혼합을 할 경우, 다층 양자점들은 응집이 되는 현상을 보이나 그 내부에 있는 양자점은 용매에 단 분산된 형태로 고립되어 존재함으로써 발광효율의 감소가 없으며, 외부환경에 대한 반응성이 적어 발광소자 제조시 용이한 효과가 있다.As described above, the present invention has various wavelengths for a long time, has good luminous efficiency and improves dispersibility. Of course, when the multilayer quantum dots prepared by the above method are mixed with resin, the multilayer quantum dots They show a phenomenon of aggregation, but the quantum dots in the inside are isolated in a single dispersed form in the solvent so that there is no reduction in the luminous efficiency, and there is little reactivity to the external environment, thereby making it easy to manufacture a light emitting device.

본 발명은 양자점의 분산성을 높혀 발광효율을 향상시킨 것을 기본으로 하는 여러 껍질을 지니고 있는 다층 양자점으로, 기본 구조는 (코어/쉘)/용매/쉘 구조를 지니는 것이다.The present invention is a multi-layered quantum dot having several shells based on improved dispersibility of quantum dots to improve luminous efficiency, and the basic structure has a (core / shell) / solvent / shell structure.

본 발명에 따른 양자점은 II-VI족, III-V족 등으로 이루어진 코어 또는 코어 /쉘 구조를 지니는 것이 바람직하나, 이에 한정되는 것은 아니다. The quantum dot according to the present invention preferably has a core or core / shell structure composed of Group II-VI, Group III-V, and the like, but is not limited thereto.

본 발명의 양자점은 다양한 파장을 지니는 것으로 그것의 사용의 최종 발광소자의 쓰임에 따른 색상에 의존하는 것으로 양자점을 단독 혹은 여러 종을 혼합하여 사용하여 최종 발광소자의 색상을 조절한다. The quantum dots of the present invention have various wavelengths and depend on the color according to the use of the final light emitting device of the use thereof, and the color of the final light emitting device is adjusted by using quantum dots alone or in combination of several species.

본 발명의 발광소자용 양자점으로써 유기용매는 양자점의 분산성을 높이고, 외부환경에 대한 간섭을 적게 하여 양자점의 발광효율을 향상시키며, 장기간 그 특성을 유지하는 것이 특징이다. 상기 사용되어질 용매는 양자점의 분산성을 높혀주고 양자점에 영향을 주지 않는 것이 바람직하다. As the quantum dot for the light emitting device of the present invention, the organic solvent is characterized by increasing the dispersibility of the quantum dot, reducing interference with the external environment, improving the luminous efficiency of the quantum dot, and maintaining its characteristics for a long time. The solvent to be used preferably increases the dispersibility of the quantum dots and does not affect the quantum dots.

트리옥틸포스핀(Trioctylphosphine)과 같은 유기용매는 양자점의 분산성을 좋게 하여 발광효율을 증가시키는 것으로, 이와 같은 용매를 사용함이 바람직하나, 본 발명에서 사용되는 용매는 일 실시예이고 그에 한정되지는 않는다. Organic solvents such as trioctylphosphine (Trioctylphosphine) to improve the dispersibility of the quantum dots to increase the luminous efficiency, it is preferable to use such a solvent, but the solvent used in the present invention is an embodiment and is not limited thereto. Do not.

상기 용매에 분산된 양자점에 쉘을 입히는 최외각 쉘은 양자점이 분산된 용매를 나노 및 마이크로 단위의 쉘을 형성하는 것으로써, 빛 발광을 감소시키지 않는 형태로 제조되어 지는 것이 바람직하다. The outermost shell coating the shell on the quantum dots dispersed in the solvent is preferably formed in a form that does not reduce light emission by forming a shell of nano and micro units of the solvent in which the quantum dots are dispersed.

최외각 쉘의 두께가 너무 두껍거나 혹은 쉘의 광 투광성이 없을 경우, 발광효율이 떨어져 바람직하지 않다. 최 외각 쉘로는 실리카나 고분자 등이 사용 가능하다. If the thickness of the outermost shell is too thick or the shell is not light transmissive, the luminous efficiency is poor, which is not preferable. As the outermost shell, silica or polymer can be used.

이렇게 제조된 다층 양자점은 레진과 혼합을 할 경우, 다층 양자점들은 응집이 되는 현상을 보이나 그 내부에 있는 양자점은 용매에 단 분산된 형태로 고립되어 존재함으로써 발광효율의 감소가 없으며, 외부환경에 대한 반응성이 적어 발광 소자 제조시 용이한 장점을 지니게 된다.When the multilayered quantum dots thus prepared are mixed with the resin, the multilayered quantum dots show a phenomenon of aggregation, but the quantum dots therein are isolated in the form of monodisperse in a solvent so that there is no decrease in luminous efficiency. It has a low reactivity and has an easy advantage in manufacturing a light emitting device.

이하 본 발명을 실시예를 통하여 상세하게 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail with reference to the following Examples.

[실시예 1] Example 1

1) CdTe/CdS(코어/쉘) 양자점 제조공정1) CdTe / CdS (core / shell) quantum dot manufacturing process

Cd(NO3)2·4H2O 0.4535g을 도데실아민(Dodecylamine)10g을 넣어서 녹인 후, 이에 Te 0.16g을 트리옥틸포스핀(Trioctylphosphine) 5g에 녹인 용액을 첨가하고 가열(160∼250℃)하여 도1a에 나타낸 바와 같은 CdTe 코어(11)를 제조한 다음 그 제조된 코어(11)를 클로로포름과 메탄올로 원심분리를 통하여 분리 및 세척한다. 0.4535 g of Cd (NO 3 ) 2 · 4H 2 O was dissolved in 10 g of dodecylamine, and then 0.16 g of Te was dissolved in 5 g of trioctylphosphine, followed by heating (160-250 ° C.). ) To prepare a CdTe core 11 as shown in Figure 1a, and then the prepared core 11 is separated and washed by centrifugation with chloroform and methanol.

상기와 같이하여 세척된 코어(11)에 도1b에 나타낸 바와 같은 CdS 쉘(12)을 형성하기 위하여 상기 제조된 코어(11)를 도데실아민 20g에 분산시킨 후, Cd(NO3)2·4H2O 0.907g과 황 0.198g을 트리옥틸포스핀 5g에 각각 녹인 후, 그 두 용액을 코어가 분산된 도데실아민 용액을 넣고 가열(160∼250℃)하여 CdTe 표면에 도1b에 나타낸 바와 같은 CdS 쉘(12)을 형성한다. After dispersing the prepared core 11 in 20 g of dodecylamine to form a CdS shell 12 as shown in FIG. 1B on the core 11 washed as described above, Cd (NO 3 ) 2. 0.907 g of 4H 2 O and 0.198 g of sulfur were dissolved in 5 g of trioctylphosphine, and the two solutions were added with a dodecylamine solution in which the core was dispersed, and heated (160 to 250 ° C.) as shown in FIG. 1B on the CdTe surface. The same CdS shell 12 is formed.

상기와 같이 제조된 코어/쉘 즉 양자점(10)을 클로로포름과 메탄올을 이용하여 원심분리를 통하여 분리 및 세척한다. 이렇게 세척된 양자점(10)을 투과전자현미경을 통하여 크기 및 형상을 조사한다.The core / shell quantum dot 10 prepared as described above is separated and washed by centrifugation using chloroform and methanol. The size and shape of the quantum dot 10 thus washed is examined through a transmission electron microscope.

2) CdTe/CdS/용매/실리카(코어/쉘/용매/최 외각 쉘) 다층 양자점 제조공정2) CdTe / CdS / solvent / silica (core / shell / solvent / outer shell) multilayer quantum dot manufacturing process

상기 도1b와 같이 제조된 CdTe/CdS 코어/쉘 즉 양자점(10)을 용매(21)인 트리옥틸포스핀 5g에 분산시킨 다음 TEOS 23ml, 증류수 2ml, 염산 0.2ml로 제조한 실 리카 졸(최 외각 쉘(22)) 5ml를 상기 트리옥틸포스핀에 분산된 코어/쉘 용액을 넣고 교반한다. The CdTe / CdS core / shell prepared as shown in FIG. 1B, that is, the quantum dot 10, was dispersed in 5 g of trioctylphosphine as a solvent 21, and then silica sol prepared with 23 ml of TEOS, 2 ml of distilled water, and 0.2 ml of hydrochloric acid (max. 5 ml of the outer shell 22) is added to the core / shell solution dispersed in the trioctylphosphine and stirred.

상기 용액에 (3-Aminopropyl)트리에톡시실란(triethoxysilane) 용액을 넣되, 증류수와 트리톤(Triton) X-100이 혼합된 용액을 교반하는 상태에서 넣는다. The solution (3-Aminopropyl) triethoxysilane (triethoxysilane) solution is added to the solution, distilled water and Triton (Triton) X-100 mixed solution is added while stirring.

상기와 같이하여 제조된 용액을 원심분리를 통하여 증류수를 제거한 후 진공건조기에서 건조하여 도2에 나타낸 바와 같이 다층 양자점(20)을 제조한다. 이와 같이 제조된 다층 양자점을 주사전자현미경 및 광스펙트럼 분석기를 통하여 이미지 및 발광 스펙트럼을 얻었다.The solution prepared as described above is removed by distillation through centrifugation and dried in a vacuum dryer to prepare a multilayer quantum dot 20 as shown in FIG. The multilayer quantum dots thus prepared were obtained by scanning electron microscope and light spectrum analyzer to obtain images and emission spectra.

[실시예 2][Example 2]

1) CdSe/ZnS(코어/쉘) 양자점 제조공정1) CdSe / ZnS (core / shell) quantum dot manufacturing process

CdO 0.0433g을 헥사데실아민(Hexadecylamine) 2.5g과 트리옥틸포스핀 옥사이드(Trioctylphosphine oxide) 5g이 혼합된 용액에 넣어서 녹인 후, Se 0.0359g을 트리옥틸포스핀 2.5g에 녹인 용액을 첨가하고 가열하여 도1a와 같은 CdSe 코어(11)를 제조한 다음 그 제조된 코어를 클로로포름과 메탄올을 이용하여 원심분리를 통하여 분리 및 세척한다. 0.0433 g of CdO was dissolved in a mixed solution of 2.5 g of hexadecylamine and 5 g of trioctylphosphine oxide, and then 0.0359 g of Se was dissolved in 2.5 g of trioctylphosphine. After preparing the CdSe core 11 as shown in FIG. 1A, the prepared core is separated and washed by centrifugation using chloroform and methanol.

상기 세척된 코어(11)에 도1b에 나타낸 바와 같은 ZnS 쉘(12)을 형성하기 위하여 코어(11)를 핵사데실아민(Hexadecylamine) 1.25g과 트리옥틸포스핀 옥사이드 2.5g에 분산시킨 후, Bis(trimethysilil)sulfate 0.124g과 디메틸아연(Dimethylzine) 0.35ml를 트리옥틸포스핀(Trioctylphosphine) 용액 3ml에 녹이 후 이용액을 코어가 분산된 용액에 넣고 가열(160∼250℃)하여 CdSe 표면에 Zns 쉘(12)을 형성한 다음 클로로포름과 메탄올을 이용하여 원심분리를 통하여 분리 및 세척한다. 이렇게 제조된 양자점을 투과전자현미경을 통하여 크기 및 형상을 조사한다.The core 11 was dispersed in 1.25 g of hexadecylamine and 2.5 g of trioctylphosphine oxide to form a ZnS shell 12 as shown in FIG. Dissolve 0.124 g of (trimethysilil) sulfate and 0.35 ml of dimethylzinc in 3 ml of trioctylphosphine solution, add the solution to the core-dispersed solution, and heat (160-250 ° C) to a Zns shell on the CdSe surface. 12) is formed and separated and washed by centrifugation using chloroform and methanol. The size and shape of the quantum dots thus prepared were examined through a transmission electron microscope.

2) CdSe/Zns/용매/실리카(코어/쉘/용매/최 외각 쉘) 다층 양자점 제조공정2) CdSe / Zns / Solvent / Silica (Core / Shell / Solvent / Outer Shell) Multilayer Quantum Dot Manufacturing Process

상기와 같이하여 제조된 CdSe/Zns 코어/쉘 즉 양자점(10)을 용매(21)인 트리옥틸포스핀(Trioctylphosphine) 2.5g을 분산시키고, TEOS 23ml, 증류수 2ml, 염산 0.2ml로 제조한 실리카 졸(최외각 쉘(22)) 2.5ml를 상기 트리옥틸포스핀에 분산된 코어/쉘 용액을 넣고 교반한다.Silica sol prepared by dispersing 2.5 g of trioctylphosphine (Trioctylphosphine), which is a solvent 21, of the CdSe / Zns core / shell, ie, the quantum dot 10 prepared as described above, was prepared with 23 ml of TEOS, 2 ml of distilled water, and 0.2 ml of hydrochloric acid. (Outer shell 22) 2.5 ml of the core / shell solution dispersed in the trioctylphosphine was added and stirred.

상기 용액에 (3-Aminopropyl)트리에톡시실란(triethoxysilane) 용액 넣되, 증류수와 트리톤(Triton) X-100이 혼합된 용액을 교반하는 상태에서 넣는다. 그리고 상기 제조된 용액을 원심분리를 통하여 증류수를 제거한 후 진공건조기에서 건조하여 다층 양자점(20)을 제조한다. The solution (3-Aminopropyl) triethoxysilane (triethoxysilane) solution is put into the solution, distilled water and Triton (Triton) X-100 mixed solution is added while stirring. Then, the prepared solution is removed by distillation through centrifugation and dried in a vacuum dryer to prepare a multilayer quantum dot (20).

이렇게 제조된 다층 양자점을 주사전자현미경 및 광스펙트럼 분석기를 통하여 이미지 및 발광 스펙트럼을 얻었다.The multilayer quantum dots thus prepared were obtained by scanning electron microscope and light spectrum analyzer to obtain images and emission spectra.

[실시예 3][Example 3]

코어/쉘/용매/최 외각 쉘(고분자) 다층 양자점 제조 및 발광소자 제조공정 Core / shell / solvent / outer shell (polymer) multilayer quantum dot manufacturing and light emitting device manufacturing process

실시예 1과 2에서 제조된 코어/쉘 양자점을 트리옥틸포스핀 5g에 분산하고, 이 용액을 폴리비닐알콜 3.2g이 녹아있는 증류수에 넣고 교반 후, 붕산 3.2g을 녹여 놓은 용액에 넣어 (코어/쉘)/용매/고분자 다층 양자점을 형성하고, 이것을 원심분리를 통하여 수분을 제거하고 한다. The core / shell quantum dots prepared in Examples 1 and 2 were dispersed in 5 g of trioctylphosphine, and the solution was added to distilled water in which 3.2 g of polyvinyl alcohol was dissolved and stirred, and then, 3.2 g of boric acid was dissolved in a solution (core) / Shell) / solvent / polymer multilayer quantum dots, which are then centrifuged to remove moisture.

상기와 같이하여 제조된 코어/쉘/용매/최 외각 쉘(고분자) 다층 양자점이 완전히 고형화되기 전에 주사기와 같은 것으로 압출성형을 통하여 LED 칩 위에 일정한 크기로 주입하여 칩 위에 적층한 후 건조한다. 이와 같이하여 다층 양자점이 적층된 칩은 에폭시로 몰딩하여 램프를 제조한다.The core / shell / solvent / outer shell (polymer) multilayer quantum dots prepared as described above are injected into a predetermined size on an LED chip by extrusion molding, such as a syringe, before being completely solidified, stacked on the chip, and dried. In this way, the chip in which the multilayered quantum dots are stacked is molded by epoxy to manufacture a lamp.

[실시예 4]Example 4

상기 실시예 1과 2에서 제조된 다층 양자점을 단독 혹은 2가지를 혼합하여 원하는 색으로 조절하고, 그 다층 양자점들을 주제와 경화제로 구성된 에폭시와 혼합한 후 이것을 LED 칩 위에 적층한 후 그 다층 양자점이 적층된 칩을 에폭시로 몰딩하여 램프를 제조한다.The multilayer quantum dots prepared in Examples 1 and 2 were adjusted to a desired color by mixing only one or two, mixed the multilayer quantum dots with epoxy composed of a main agent and a curing agent, and laminated them on the LED chip, and then the multilayer quantum dots The laminated chip is molded with epoxy to make a lamp.

상술한 바와 같이 제조된 다층 양자점 및 그 다층 양자점이 적층된 발광소자는 장기간 동안 다양한 파장을 지님은 물론, 발광효율이 좋고, 분산성을 높여주는 장점이 있다.The multilayer quantum dots manufactured as described above and the light emitting device in which the multilayer quantum dots are stacked have various wavelengths for a long time, as well as good luminous efficiency and improved dispersibility.

또한 상기의 방법으로 제조된 다층 양자점은 레진과 혼합을 할 경우, 다층 양자점들은 응집이 되는 현상을 보이나 그 내부에 있는 양자점은 용매에 단 분산된 형태로 고립되어 존재함으로써 발광효율의 감소가 없으며, 외부환경에 대한 반응성이 적어 발광소자 제조시 용이한 장점을 지니게 된다. In addition, when the multilayer quantum dots manufactured by the above method are mixed with the resin, the multilayer quantum dots show a phenomenon of aggregation, but the quantum dots therein are isolated in a single dispersed form in a solvent so that there is no decrease in luminous efficiency. It is easy to manufacture a light emitting device because it is less reactive to the external environment.

도 1a는 본 발명의 다층 양자점을 형성하는 양자점의 코어 확대도이고,1A is an enlarged view of a core of a quantum dot forming a multilayer quantum dot of the present invention,

도 1b는 본 발명의 다층 양자점을 형성하는 양자점의 확대도이며,1B is an enlarged view of a quantum dot forming a multilayer quantum dot of the present invention,

도 2는 본 발명에 의해서 제조된 다층 양자점의 확대도이고, 2 is an enlarged view of a multilayer quantum dot manufactured by the present invention,

도 3a는 본 발명에 따른 제1실시예의 양자점 투과전자현미경 사진이고,3A is a quantum dot transmission electron microscope photograph of a first embodiment according to the present invention;

도 3b는 본 발명에 따른 제2실시예의 양자점 투과전자현미경 사진이며, Figure 3b is a quantum dot transmission electron micrograph of a second embodiment according to the present invention,

도 4a는 실시예 1에 의하여 제조된 코어/쉘/용매/최 외각 쉘 구조의 다층 양자점의 주사전자현미경 사진이고,4A is a scanning electron micrograph of a multilayer quantum dot of a core / shell / solvent / outer shell structure prepared according to Example 1,

도 4b는 실시예 2에 의하여 제조된 코어/쉘/용매/쉘 구조의 다층 양자점의 주사전자현미경 사진이며, 4B is a scanning electron micrograph of a multilayer quantum dot of a core / shell / solvent / shell structure prepared according to Example 2,

도 5a는 실시예 1에 의하여 제조된 코어/쉘/용매/쉘 구조의 다층 양자점의 발광스텍트럼이고,5A is a light emission spectrum of a multilayer quantum dot of a core / shell / solvent / shell structure prepared according to Example 1,

도 5b는 실시예 2에 의하여 제조된 코어/쉘/용매/쉘 구조의 다층 양자점의 발광스텍트럼이며, 5B is a light emission spectrum of a multilayer quantum dot of a core / shell / solvent / shell structure prepared in Example 2,

도 6은 실시예 3에 의하여 제조된 코어/쉘/용매/쉘 구조의 다층 양자점을 혼합한 것의 발광스텍트럼이고, 6 is a light emission spectrum of a mixture of multilayer quantum dots of a core / shell / solvent / shell structure prepared in Example 3,

도 7은 실시예 4에 의하여 제조된 LED의 발광사진이다. 7 is a light-emitting photograph of the LED manufactured by Example 4.

Claims (12)

(a) CdTe/CdS(코어/쉘) 양자점 혹은 CdSe/ZnS(코어/쉘) 양자점을 유기 용매인 트리옥틸포스핀(Trioctylphosphine)에 분산시키는 단계;(a) dispersing CdTe / CdS (core / shell) quantum dots or CdSe / ZnS (core / shell) quantum dots in trioctylphosphine, an organic solvent; (b) TEOS, 증류수 및 염산으로 제조한 실리카 졸을 상기 유기 용매에 분산된 코어/쉘 용액에 넣고 교반하는 단계;(b) adding a silica sol prepared from TEOS, distilled water and hydrochloric acid into a core / shell solution dispersed in the organic solvent and stirring; (c) 상기 용액에 (3-Aminopropyl)트리에톡시실란(triethoxysilane) 용액을 넣는 단계;(c) adding a (3-Aminopropyl) triethoxysilane solution to the solution; (d) 상기 단계 (c)의 결과물에 증류수와 트리톤(Triton) X-100이 혼합된 용액을 교반하는 상태에서 넣는 단계;(d) adding distilled water and Triton X-100 mixed solution to the resultant of step (c) while stirring; (e) 상기 단계 (d)에서 제조된 용액을 원심분리를 통하여 증류수를 제거하는 단계; 및(e) removing distilled water by centrifuging the solution prepared in step (d); And (f) 상기 단계 (e)의 결과물을 진공건조기에서 건조하는 단계;로 이루어지는 방법으로 다층 양자점을 제조하고, 상기 다층 양자점은 코어/쉘/용매/최 외각 쉘 형태를 가지며, 상기 CdTe/CdS(코어/쉘) 양자점 혹은 CdSe/ZnS(코어/쉘) 양자점은 다층 양자점을 형성하는 최 외곽 쉘의 내부 용매에 분산된 상태로 분포된 것을 특징으로 하는 발광소자용 다층 양자점 제조방법.(f) drying the resultant of step (e) in a vacuum dryer; to prepare a multilayer quantum dot, the multilayer quantum dot has a core / shell / solvent / outermost shell form, the CdTe / CdS ( Core / shell) Quantum dots or CdSe / ZnS (core / shell) quantum dots is a method of manufacturing a multilayer quantum dot for a light emitting device, characterized in that distributed in the state dispersed in the inner solvent of the outermost shell forming a multilayer quantum dot. (a) CdTe/CdS(코어/쉘) 양자점 혹은 CdSe/ZnS(코어/쉘) 양자점을 유기 용매인 트리옥틸포스핀(Trioctylphosphine) 5g에 분산시키는 단계;(a) dispersing CdTe / CdS (core / shell) quantum dots or CdSe / ZnS (core / shell) quantum dots in 5 g of trioctylphosphine, an organic solvent; (b) TEOS 23 ml, 증류수 2 ml 및 염산 0.2 ml로 제조한 실리카 졸 5 ml를 상기 유기 용매 트리옥틸포스핀에 분산된 코어/쉘 용액을 넣고 교반하는 단계;(b) adding 5 ml of a silica sol prepared with 23 ml of TEOS, 2 ml of distilled water, and 0.2 ml of hydrochloric acid to a core / shell solution dispersed in the organic solvent trioctylphosphine; (c) 상기 용액에 (3-Aminopropyl)트리에톡시실란(triethoxysilane) 용액을 넣는 단계;(c) adding a (3-Aminopropyl) triethoxysilane solution to the solution; (d) 상기 단계 (c)의 결과물에 증류수와 트리톤(Triton) X-100이 혼합된 용액을 교반하는 상태에서 넣는 단계;(d) adding distilled water and Triton X-100 mixed solution to the resultant of step (c) while stirring; (e) 상기 단계 (d)에서 제조된 용액을 원심분리를 통하여 증류수를 제거하는 단계; 및(e) removing distilled water by centrifuging the solution prepared in step (d); And (f) 상기 단계 (e)의 결과물을 진공건조기에서 건조하는 단계;로 이루어지는 방법으로 다층 양자점을 제조하고, 상기 다층 양자점은 코어/쉘/용매/최 외각 쉘 형태를 가지며, 상기 CdTe/CdS(코어/쉘) 양자점 혹은 CdSe/ZnS(코어/쉘) 양자점은 다층 양자점을 형성하는 최 외곽 쉘의 내부 용매에 분산된 상태로 분포된 것을 특징으로 하는 발광소자용 다층 양자점 제조방법.(f) drying the resultant of step (e) in a vacuum dryer; to prepare a multilayer quantum dot, the multilayer quantum dot has a core / shell / solvent / outermost shell form, the CdTe / CdS ( Core / shell) Quantum dots or CdSe / ZnS (core / shell) quantum dots is a method of manufacturing a multilayer quantum dot for a light emitting device, characterized in that distributed in the state dispersed in the inner solvent of the outermost shell forming a multilayer quantum dot. 삭제delete 삭제delete 제1항 또는 제2항에 있어서, 상기 최 외각 쉘은 실리카 또는 고분자로 구성된 것을 특징으로 하는 발광소자용 다층 양자점 제조방법.The method of claim 1 or 2, wherein the outermost shell is made of silica or a polymer. (a) CdTe/CdS(코어/쉘) 양자점 또는 CdSe/ZnS(코어/쉘) 양자점 중 어느 하나의 양자점을 트리옥틸포스핀(Trioctylphosphine)에 분산시키는 단계;(a) dispersing quantum dots of either CdTe / CdS (core / shell) quantum dots or CdSe / ZnS (core / shell) quantum dots in trioctylphosphine; (b) 상기 단계 (a)의 결과물을 폴리비닐알콜이 녹아있는 증류수에 넣고 교반하는 단계;(b) putting the resultant of step (a) into distilled water in which polyvinyl alcohol is dissolved and stirring; (c) 상기 단계 (b)의 결과물을 붕산을 녹여 놓은 용액에 넣어 코어/쉘/용매/최 외각 쉘(고분자) 다층 양자점을 형성하는 단계;(c) adding the resultant of step (b) to a solution of boric acid to form a core / shell / solvent / outer shell (polymer) multilayer quantum dot; (d) 상기 단계 (c)의 결과물을 원심분리를 통하여 수분을 제거한 후 그 수분이 제거된 코어/쉘/용매/최 외각 쉘(고분자) 다층 양자점이 완전히 고형화되기 전에 LED 칩 위에 원하는 크기로 적층하고 건조하는 단계; 및(d) The resultant of step (c) is centrifuged to remove moisture, and then the core / shell / solvent / outer shell (polymer) multilayered quantum dots from which the moisture is removed are laminated to the desired size on the LED chip before it is completely solidified. And drying; And (e) 상기 단계 (d)의 건조 적층된 LED 칩을 몰딩하여 램프를 제조하는 단계;로 이루어진 것을 특징으로 하는 발광소자 제조방법.(e) molding a dry stacked LED chip of step (d) to manufacture a lamp. 제6항에 있어서, 상기 CdTe/CdS(코어/쉘) 양자점 또는 CdSe/ZnS(코어/쉘) 양자점 중 어느 하나의 양자점을 트리옥틸포스핀(Trioctylphosphine) 5g에 분산시키고, 이 용액을 폴리비닐알콜 3.2g이 녹아있는 증류수에 넣고 교반한 후, 붕산 3.2g을 녹여 놓은 용액에 넣어 코어/쉘/용매/최 외각 쉘(고분자) 다층 양자점을 형성한 것임을 특징으로 하는 발광소자 제조방법.The quantum dot of any one of the CdTe / CdS (core / shell) quantum dots or CdSe / ZnS (core / shell) quantum dots are dispersed in 5 g of trioctylphosphine (Trioctylphosphine), the solution is polyvinyl alcohol A method of manufacturing a light emitting device, characterized in that 3.2g of distilled water is dissolved and stirred, and then 3.2g of boric acid is added to a dissolved solution to form a core / shell / solvent / outer shell (polymer) multilayer quantum dot. 상기 제6항의 방법으로 제조된 발광소자.A light emitting device manufactured by the method of claim 6. 상기 제1항의 방법으로 제조된 다층 양자점을 원하는 색으로 조절하고, 그 조절된 다층 양자점을 에폭시와 혼합한 후 그 혼합물을 LED 칩 위에 적층하고 건조하며, 그 건조 적층된 LED 칩을 몰딩하여 램프를 제조하는 것을 특징으로 하는 발광소자 제조방법. The multilayer quantum dots prepared by the method of claim 1 are adjusted to a desired color, the controlled multilayer quantum dots are mixed with epoxy, the mixture is laminated on the LED chip and dried, and the dried laminated LED chip is molded to form a lamp. Light emitting device manufacturing method characterized in that the manufacturing. 상기 제9항의 방법으로 제조된 발광소자.A light emitting device manufactured by the method of claim 9. 제1항 또는 제2항에 있어서, 상기 CdTe/CdS(코어/쉘) 양자점은 (ⅰ) Cd(NO3)2· 4H2O 0.4535 g을 도데실아민(Dodecylamine)10 g을 넣어서 녹인 다음, 이에 Te 0.16 g을 트리옥틸포스핀(Trioctylphosphine) 5 g에 녹인 용액을 첨가하고 가열(160∼250℃)하여 CdTe 코어(11)를 제조한 다음 상기 제조된 코어(11)를 클로로포름과 메탄올로 원심분리를 통하여 분리 및 세척하는 단계; 및 (ⅱ) 상기 단계 (ⅰ)의 세척된 코어(11)를 도데실아민 20 g에 분산시킨 후, Cd(NO3)2· 4H2O 0.907 g과 황 0.198 g을 트리옥틸포스핀 5 g에 각각 녹인 후, 상기 두 용액을 코어가 분산된 도데실아민 용액에 넣고 가열(160∼250℃)하여 CdTe 표면에 CdS 쉘(12)을 형성한 다음, 클로로포름과 메탄올을 이용하여 원심분리를 통하여 분리 및 세척하는 단계;를 포함하는 방법으로 제조하고, The method according to claim 1 or 2, wherein the CdTe / CdS (core / shell) quantum dot (iii) dissolve 0.4535 g of Cd (NO 3 ) 2 · 4H 2 O with 10 g of dodecylamine, To this, 0.16 g of Te was dissolved in 5 g of trioctylphosphine (Trioctylphosphine), and heated (160 to 250 ° C.) to prepare a CdTe core (11). Separating and washing through separation; And (ii) dispersing the washed core 11 of step (iii) in 20 g of dodecylamine, followed by 0.907 g of Cd (NO 3 ) 2 .4H 2 O and 0.198 g of sulfur, 5 g of trioctylphosphine. After dissolving in each, the two solutions were placed in a dodecylamine solution in which the core was dispersed to form a CdS shell (12) on the surface of CdTe by heating (160 ~ 250 ℃), and then centrifuged with chloroform and methanol Is prepared by a method comprising; and separating and washing; 상기 CdSe/ZnS(코어/쉘) 양자점은 (ⅲ) CdO 0.0433 g을 헥사데실아민(Hexadecylamine) 2.5 g과 트리옥틸포스핀 옥사이드(Trioctylphosphine oxide) 5 g이 혼합된 용액에 넣어서 녹인 다음, Se 0.0359 g을 트리옥틸포스핀 2.5 g에 녹인 용액을 첨가하고 가열하여 CdSe 코어(11)를 제조하고, 상기 제조된 코어를 클로로포름과 메탄올을 이용하여 원심분리를 통하여 분리 및 세척하는 단계; 및 (ⅳ) 상기 단계 (ⅲ)의 세척된 코어(11)를 핵사데실아민(Hexadecylamine) 1.25 g과 트리옥틸포스핀 옥사이드 2.5 g에 분산시킨 다음, 비스(트리메틸실일)설페이트(Bis(trimethysilil)sulfate) 0.124 g과 디메틸아연(Dimethylzine) 0.35 ml를 트리옥틸포스핀(Trioctylphosphine) 용액 3 ml에 녹인 후 상기 용액을 코어가 분산된 용액에 넣고 가열(160∼250℃)하여 CdSe 표면에 Zns 쉘(12)을 형성한 다음 클로로포름과 메탄올을 이용하여 원심분리를 통하여 분리 및 세척하는 단계;를 포함하는 방법으로 제조하는 것을 특징으로 하는 발광소자용 다층 양자점 제조방법.The CdSe / ZnS (core / shell) quantum dots (ⅲ) 0.0433 g of CdO was dissolved in a solution of 2.5 g of hexadecylamine and 5 g of trioctylphosphine oxide, and then dissolved 0.0359 g of Se. Adding a solution dissolved in 2.5 g of trioctylphosphine and heating to prepare a CdSe core (11), and separating and washing the prepared core by centrifugation using chloroform and methanol; And (iii) dispersing the washed core 11 of step (iii) in 1.25 g of Hexadecylamine and 2.5 g of trioctylphosphine oxide, followed by bis (trimethysilil) sulfate. ) 0.124 g and 0.35 ml of dimethylzine were dissolved in 3 ml of trioctylphosphine solution, and the solution was added to a core-dispersed solution and heated (160 to 250 ° C.) to a Zns shell (12). Forming a) and then separating and washing through centrifugation using chloroform and methanol; manufacturing method of a multi-layer quantum dot for a light emitting device comprising a. 제6항에 있어서, 상기 CdTe/CdS(코어/쉘) 양자점은 (ⅰ) Cd(NO3)2· 4H2O 0.4535 g을 도데실아민(Dodecylamine)10 g을 넣어서 녹인 다음, 이에 Te 0.16 g을 트리옥틸포스핀(Trioctylphosphine) 5 g에 녹인 용액을 첨가하고 가열(160∼250℃)하여 CdTe 코어(11)를 제조한 다음 상기 제조된 코어(11)를 클로로포름과 메탄올로 원심분리를 통하여 분리 및 세척하는 단계; 및 (ⅱ) 상기 단계 (ⅰ)의 세척된 코어(11)를 도데실아민 20 g에 분산시킨 후, Cd(NO3)2· 4H2O 0.907 g과 황 0.198 g을 트리옥틸포스핀 5 g에 각각 녹인 후, 상기 두 용액을 코어가 분산된 도데실아민 용액에 넣고 가열(160∼250℃)하여 CdTe 표면에 CdS 쉘(12)을 형성한 다음, 클로로포름과 메탄올을 이용하여 원심분리를 통하여 분리 및 세척하는 단계;를 포함하는 방법으로 제조하고, According to claim 6, wherein the CdTe / CdS (core / shell) quantum dots (ⅰ) dissolve 0.4535 g of Cd (NO 3 ) 2 · 4H 2 O by adding 10 g of dodecylamine, Te 0.16 g Was added to a solution of 5 g of trioctylphosphine (Trioctylphosphine) and heated (160 ~ 250 ℃) to prepare a CdTe core (11) and then the core (11) was separated by centrifugation with chloroform and methanol And washing; And (ii) dispersing the washed core 11 of step (iii) in 20 g of dodecylamine, followed by 0.907 g of Cd (NO 3 ) 2 .4H 2 O and 0.198 g of sulfur, 5 g of trioctylphosphine. After dissolving in each, the two solutions were placed in a dodecylamine solution in which the core was dispersed to form a CdS shell (12) on the surface of CdTe by heating (160 ~ 250 ℃), and then centrifuged with chloroform and methanol Is prepared by a method comprising; and separating and washing; 상기 CdSe/ZnS(코어/쉘) 양자점은 (ⅲ) CdO 0.0433 g을 헥사데실아민(Hexadecylamine) 2.5 g과 트리옥틸포스핀 옥사이드(Trioctylphosphine oxide) 5 g이 혼합된 용액에 넣어서 녹인 다음, Se 0.0359 g을 트리옥틸포스핀 2.5 g에 녹인 용액을 첨가하고 가열하여 CdSe 코어(11)를 제조하고, 상기 제조된 코어를 클로로포름과 메탄올을 이용하여 원심분리를 통하여 분리 및 세척하는 단계; 및 (ⅳ) 상기 단계 (ⅲ)의 세척된 코어(11)를 핵사데실아민(Hexadecylamine) 1.25 g과 트리옥틸포스핀 옥사이드 2.5 g에 분산시킨 다음, 비스(트리메틸실일)설페이트(Bis(trimethysilil)sulfate) 0.124 g과 디메틸아연(Dimethylzine) 0.35 ml를 트리옥틸포스핀(Trioctylphosphine) 용액 3 ml에 녹인 후 상기 용액을 코어가 분산된 용액에 넣고 가열(160∼250℃)하여 CdSe 표면에 Zns 쉘(12)을 형성한 다음 클로로포름과 메탄올을 이용하여 원심분리를 통하여 분리 및 세척하는 단계;를 포함하는 방법으로 제조하는 것을 특징으로 하는 발광소자 제조방법.The CdSe / ZnS (core / shell) quantum dots (ⅲ) 0.0433 g of CdO was dissolved in a solution of 2.5 g of hexadecylamine and 5 g of trioctylphosphine oxide, and then dissolved 0.0359 g of Se. Adding a solution dissolved in 2.5 g of trioctylphosphine and heating to prepare a CdSe core (11), and separating and washing the prepared core by centrifugation using chloroform and methanol; And (iii) dispersing the washed core 11 of step (iii) in 1.25 g of Hexadecylamine and 2.5 g of trioctylphosphine oxide, followed by bis (trimethysilil) sulfate. ) 0.124 g and 0.35 ml of dimethylzine were dissolved in 3 ml of trioctylphosphine solution, and the solution was added to a core-dispersed solution and heated (160 to 250 ° C.) to a Zns shell (12). Forming a) and then separating and washing by centrifugation using chloroform and methanol; manufacturing method comprising a light emitting device.
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