KR20160130540A - Method for manufacturing quantum dot-optically transparent matrix complexes capable of adjusting luminance and quantum dot-polymer composite thereof - Google Patents
Method for manufacturing quantum dot-optically transparent matrix complexes capable of adjusting luminance and quantum dot-polymer composite thereof Download PDFInfo
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- KR20160130540A KR20160130540A KR1020150062410A KR20150062410A KR20160130540A KR 20160130540 A KR20160130540 A KR 20160130540A KR 1020150062410 A KR1020150062410 A KR 1020150062410A KR 20150062410 A KR20150062410 A KR 20150062410A KR 20160130540 A KR20160130540 A KR 20160130540A
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Abstract
Description
The present invention relates to a method for producing a quantum dot-nonabsorbing medium composite and a quantum dot-polymer composite produced thereby, and more particularly, to a method for producing a quantum dot-nonabsorbing medium complex by controlling the distance between quantum dots using a non- And a quantum dot-polymer composite produced thereby.
In general, when a material is reduced in size to nanometers, it has new physical properties that were not seen in the bulk state, as the materials become smaller and become nanometer-scale in size, the bulk / Is abnormally large.
Among such nanomaterials, there is a quantum dot (QD), which is a semiconductor material having a diameter of about 2 to 10 nm, which is smaller than a certain size. When the electron mobility in a bulk semiconductor material becomes more restrictive And is a material which exhibits a quantum confinement effect in which the emission wavelength is different from the bulk state. These quantum dots emit light from an excitation source and emit energy corresponding to their corresponding energy band gaps when they reach the energy excited state. Therefore, by adjusting the size of the quantum dots, it is possible to control the bandgap and obtain various wavelengths of energy, thereby exhibiting optical, electrical, and magnetic characteristics completely different from the original physical properties.
Such quantum dots are in recent years under investigation for use in a wide variety of applications including displays, solar energy conversion, molecular and cellular imaging, and the like.
As a related technology related to the quantum dot, there is a "quantum dot-matrix thin film" of Korean Patent Laid-Open No. 10-2013-0067137, which includes a plurality of quantum dots; An inorganic matrix in which a plurality of the quantum dots are embedded; And an interface layer located between the quantum dot and the inorganic matrix and surrounding the surface of the quantum dot.
The conventional quantum dots as well as the conventional quantum dots have characteristics of changing the emission color depending on the particle size as shown in Fig. 1, as well as being sensitive to the external environment and causing defects in heat resistance and chemical resistance .
The quantum dot solution exhibits optical properties that vary with concentration. In general, high-emitting quantum dots are produced by high-temperature pyrolysis. High crystallization due to high production temperature results in high light emission. The surface is stabilized with a hydrophobic ligand, which is applicable to particulate materials capable of being dispersed in a nonpolar organic solvent. However, when the concentration of the quantum dot solution is increased, the distance between the particles becomes closer to each other. As a result, distortion of the inherent luminescence property of the quantum dot occurs. Since the distance between the quantum dots is close to that of the high-concentration quantum dot solution, FRET (Forster Energy Transfer), which is commonly observed when two fluorescent materials are adjacent to each other, occurs, and the intensity of the quantum dot luminescence decreases and red- It is also observed.
Therefore, in a conventional system using quantum dot fluorescence, there is a problem that when the concentration of the quantum dots used is increased, the distance between the quantum dots becomes closer to each other, thereby decreasing the intrinsic luminescence intensity of the quantum dots and causing a red shift in the emission wavelength band. Therefore, there is a need to solve the problem of a system including such a quantum dot.
DISCLOSURE OF THE INVENTION In order to solve the problems of the prior art as described above, the present invention simplifies the manufacturing process while keeping spacers between the quantum dots to maintain the intrinsic luminescence of the quantum dots. By controlling the distance between the quantum dots, Transfer of the quantum dots is suppressed so that the inherent high light emission of the quantum dots is maintained and there is no spectrum distortion and the heat resistance and chemical resistance of the quantum dot containing complex are improved.
Other objects of the present invention will become readily apparent from the following description of the embodiments.
According to an aspect of the present invention, there is provided a method of forming a quantum dot in an optically transparent matrix material, which is an optically transparent medium and is solid at 100 DEG C or less and chemically reactive with quantum dots, A method of making a quantum dot-non-absorbing medium composite is provided.
The quantum dot may include any one of Si-based nanocrystals, II-VI group compound semiconductor nanocrystals, III-V group compound semiconductor nanocrystals, IV-VI group compound semiconductor nanocrystals and any of these compounds .
The quantum dot may include a CdSe / ZnS quantum dot, an InP / ZnS quantum dot, an alloy quantum dot, and a gradient quantum dot.
The inert matrix material may be a molecular material of an organic material or an organometallic compound, a particulate material of a metal oxide, or a mixture of the molecular material and the particulate material.
The molecular material may include a metal salt having an alkyl or aryl group.
The molecular material may include any one or combination of zinc stearate (ZnSt 2 ) and manganese stearate (MnSt 2 ).
The particulate material may include any one or combination of polymer beads, SiO 2 (Silica), and TiO 2 (Titania).
The polymer may be mixed with an inactive matrix material in which the plurality of quantum dots are dispersed.
The polymer may be a polydimethylsiloxane (PDMS) polymer.
The quantum dots and the inert matrix material may be mixed in an organic solvent in a dissolved or dispersed state.
The quantum dots and the inert matrix material may be in a powder state, and may be mixed and injected into the polymer solution.
The quantum dots and the inert matrix material may be mixed in an organic solvent in a dissolved or dispersed state.
The luminescence of the quantum dots can be controlled by further mixing of amines or thiols.
According to another aspect of the present invention, there is provided a quantum dot-polymer complex capable of controlling the luminance, which is produced by the method for producing a quantum dot-nonabsorbing medium composite according to an aspect of the present invention.
According to the method for producing a quantum dot-non-absorbing medium composite according to the present invention and the quantum dot-polymer composite produced thereby, a non-absorbing material is automatically formed when a substance is added or synthesized from the outside, It is possible to control the luminescence of quantum dots by adding substances such as amines and thiols and to control the distance between quantum dots by controlling the distance between quantum dots. Forster energy transfer is suppressed to maintain the inherent high light emission property of the quantum dot and to prevent spectrum distortion. When a heat resistant material such as silica is used as a spacer between quantum dots, the heat resistance of the quantum dot containing complex increases, When chemical-resistant materials such as silica are present between the water- It is a role to protect the quantum dot in the external environment, thereby improving the chemical resistance of the quantum dots comprises a polymer composite.
1 is an image showing a change in luminescent color according to a conventional quantum dot particle size.
2 is a view for explaining light emission intensity and red shift according to the distance between quantum dots according to the present invention.
3 is a view showing the case where the concentration of the quantum dot according to the present invention is controlled by a molecular material.
4 is an image showing quantum dot light emission in FIG.
5 is a view showing the case where the concentration of the quantum dots according to the present invention is controlled by a particulate material.
FIG. 6 is an image showing quantum dot light emission in FIG.
7 is an image showing luminescence of a quantum dot-polymer complex according to an embodiment of the present invention.
FIG. 8 is a diagram showing a sediment prediction structure of FIG. 4 according to the present invention.
The present invention is capable of various modifications and various embodiments, and specific embodiments are illustrated and described in detail in the drawings. It is to be understood, however, that the invention is not to be limited to the specific embodiments, but is to be understood to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention, And the scope of the present invention is not limited to the following examples.
Hereinafter, embodiments according to the present invention will be described in detail with reference to the accompanying drawings, wherein like or corresponding elements are denoted by the same reference numerals, and redundant explanations thereof will be omitted.
The method of manufacturing a quantum dot-non-depolarizing medium composite according to an embodiment of the present invention is a method of mixing quantum dots into an inactive matrix material which is an optically transparent medium and solid at 100 DEG C or less so as to be dispersed in large numbers, So that it is possible to control the luminance of the light emitting diode.
In the method of manufacturing a quantum dot-nonabsorbing medium composite according to the present invention, the quantum dots include Si-based nanocrystals, II-VI group compound semiconductor nanocrystals, III-V group compound semiconductor nanocrystals, IV- Of the present invention. Here, the II-VI group compound semiconductor nanocrystals may be CdS, CdSe, CdTe, ZnS, ZnSe, ZnTe, HgS, HgSe, HgTe, CdSeS, CdSeTe, CdSTe, PbSe, PbS, ZnSeS, ZnSeTe, ZnSTe, HgSeS, HgSeTe, HgSTe , CdZnSe, CdZnTe, CdHgS, CdHgSe, CdHgTe, HgZnS, HgZnSe, HggZnTe, CdZnSeS, CdZnSeTe, CdZnSTe, CdHgSeS, CdHgSeTe, CdHgSTe, HgZnSeS, HgZnSeTe and HgZnSTe. In addition, the III-V group compound semiconductor nanocrystals may be formed of a material selected from the group consisting of GaN, GaP, GaAs, AlN, AlP, AlAs, InN, InP, InAs, GaNP, GaNAs, GaPAs, AlNP, AlNAs, AlPAs, InNP, InNAs, InPAs, GaAlNP, GaAlPAs, GaInNP, GaInNAs, GaInPAs, InAlNP, InAlNAs, and InAlPAs.
The quantum dot may be a Cd compound such as CdS, CdSe, CdTe, CdTe, etc., and the shell surrounding the core may be a Zn compound, for example, ZnS or ZnSe having a lattice parameter similar to that of the quantum dot core. Lt; RTI ID = 0.0 > CdSe / ZnS. ≪ / RTI >
The quantum dots may also include CdSe / ZnS quantum dots, InP / ZnS quantum dots, alloy quantum dots, and gradient quantum dots. Alloy quantum dots exist in alloy form between heterogeneous cation and anion. Gradient The quantum dot gradually changes linearly as the composition moves from the center of the quantum dot to the outer periphery.
The inactive matrix material may be a material that is non-absorbing (non-energy transferring) in the visible light region and used as a spacer between the quantum dots to control the distance between the quantum dots. For example, molecules of organic or organometallic compounds Or a particulate material of a metal oxide, or a mixture of the molecular material and the particulate material. The molecular material may include a metal salt having an alkyl or aryl group, for example, an alkyl acid metal salt or an aryl acid metal salt. For example. The alkyl acid metal salt may include any one or a combination of zinc stearate (ZnSt 2 ) and manganese stearate (MnSt 2 ). In addition, the particulate material may include any one or a combination thereof from the polymer beads, SiO 2 (Silica), TiO 2 (Titania).
2, when the distance between the quantum dots is adjusted using an inactive matrix, for example, ZnSt 2 , when the distance between the quantum dots QD is relatively close within the optical interaction limit region, as in a), the luminescence intensity is low In addition, when a red-shift of the emission wavelength band occurs largely and the distance between the quantum dots QD is relatively large in the optical interaction limit region as in a), as in b), the emission intensity When the distance between the quantum dots QD deviates from the optical interaction limit region as in c), there is no change in the luminescence intensity, and the red shift of the emission wavelength band is small . Therefore, the FRET phenomenon can be controlled by adjusting the distance between QDs.
As shown in FIG. 3, by adjusting the quantum dot concentration in the inactive matrix material to a molecular material such as ZnSt 2 , as shown in FIG. 4, a method of adjusting the distance between the solid-state quantum dots will be described. When irradiated with ultraviolet rays as in b) in the non-emitting state before, strong emission occurs. As shown in FIG. 5, by controlling the quantum dot concentration in the inert matrix material with a particulate material such as polymer beads, SiO 2 (Silica) or TiO 2 (Titania), ultraviolet irradiation In the non-light emitting state before, when the ultraviolet light is irradiated as in b), strong light emission is performed.
Meanwhile, the quantum dot-polymer complex capable of adjusting the luminescence according to the present invention may be mixed with a polymer in an inactive matrix material in which a plurality of quantum dots are dispersed. Here, the polymer may be a PDMS (polydimethylsiloxane) SYLGARD 184A and SYLGARD 184B, which are silicone polymers based on dimethylsiloxane of Dow Corning, were added to the dispersed inactive matrix material, and the inactive matrix materials, SYLGARD 184A and SYLGARD 184B, in which a large number of quantum dots were dispersed, : 0.01 to 50: 1, and they can be treated at a temperature of 25 to 200 ° C for 10 to 500 minutes. For example, 1 g of ZnSt 2 in which CdSe / ZnS quantum dots are dispersed, 45 g of SYLGARD 184A from Dow Corning, and 5 g of SYLGARD 184B are further mixed and treated at 120 ° C for 30 minutes, When irradiated with ultraviolet ray, it can be seen that it emits light.
In addition, yellow means quantum dots and ZnSt 2 color, because the quantum dots are red in the same condition and ZnSt 2 is white powder. This material is called a purification It is insoluble in CHCl 3 , which is a nonpolar solvent. 8, the quantum dots are partially dispersed in the ZnSt 2 lumps, and when the temperature of the solution is lowered to 100 ° C or lower, a precipitate having a unique color appears. In this process, The quantum dots are contained in ZnSt 2 , and the high luminescence properties of the precipitates are due to the fact that ZnSt 2 does not chemically and optically affect the surface of the quantum dots.
The quantum dot-polymer composite capable of controlling the luminous efficiency according to the present invention may be such that the quantum dot and the passive matrix material are mixed in a state dissolved or dispersed in an organic solvent. As another example, the quantum dot and the passive matrix material may be in a powder state So that they can be mixed and injected into the polymer solution. The quantum dot may be a CdSe / ZnS quantum dot, InP / ZnS quantum dots, alloy (alloy) quantum dots, a gradient (gradient) quantum dots, organic solvents may be in CHCl 3, an inert matrix material may be a ZnSt 2. Also
Meanwhile, in the method of preparing the quantum dot-non-absorbing medium composite according to the present invention, the luminescence of the quantum dots can be controlled by further mixing of an amine and a thiol. That is, by adding an amine, the luminescence of the quantum dots can be increased, and the luminescence of the quantum dots can be reduced by the addition of thiol.
The quantum dot-polymer complex capable of adjusting the luminescence properties according to the present invention can be prepared by the above-described method for preparing a quantum dot-non-absorbing medium composite according to the present invention, The method for producing the quantum dot-non-absorbing medium composite according to the present invention will be described in more detail by way of example.
[Example 1]
1. CdSe quantum dot synthesis
0.4 mmol of CdO, 1 mmol of oleic acid and 10 ml of ODE were mixed and heated to 180 ° C. The mixture was degassed by lowering the temperature to 130 ° C. and then injected with 1 ml of TOP-Se at 300 ° C. 1M) and grown at 270 DEG C for 5 minutes, cooled to room temperature, and then purified with EtOH.
2. CdSe / ZnS quantum dot synthesis
The CdSe series quantum dots synthesized in the previous procedure were added to 10 mL of oleylamine in a ratio of 1: 0.0001 to 100 in terms of mass ratio to Zinc dimethyldithiocarbamate. The mixture was maintained at 200 ° C. for 30 minutes and then cooled to room temperature and purified with EtOH to obtain CdSe / ZnS quantum dots are synthesized.
3. Addition of ZnSt 2 to CdSe / ZnS quantum dots
All of the CdSe / ZnS quantum dots synthesized in the previous step are dissolved in 10 mL of CHCl 3 , and 1 g of ZnSt 2 is added to dissolve together, followed by spraying on the desired substrate and drying to obtain a highly luminous material. It can be confirmed that there is no difference in luminescence in comparison with the quantum dot-polymer complex solution of the present invention.
In situ generation of ZnSt 2 was carried out by using 0.4 mmol CdO, 4.0 mmol Zn (OAc) 2 , 17.6 mmol stearic acid and 10 ml of ODE in the case of gradient green QDs synthesis And the mixture is heated to 180 ° C. and then degassed by reducing the temperature to 130 ° C. Subsequently, TOP-Se and TOP-S mixture are injected at 300 ° C. (Se 0.4 mmol, S 4.0 mmol / 3 mL TOP). Then, it is grown at 270 ° C for 10 minutes, cooled to room temperature, and purified by using EtOH. In the case of the gradient red QDs synthesis, 0.4 mmol CdO, 4.0 mmol Zn (OAc) 2 , 17.6 mmol stearic acid and 10 ml of ODE were mixed and heated to 180 ° C. and then heated to 130 ° C. Deg.] C, TOP-Se and TOP-S are sequentially injected (Se 0.4 mmol, S 4.0 mmol / 3 mL TOP) at an interval of 10 s at 300 ° C. Then, it is grown at 260 ° C for 10 minutes, cooled to room temperature, and purified by EtOH to synthesize.
[Practical example 2] Quantum dot-silica co-precipitation
MEK dispersed silica such as MEK-ST (methyl ethyl ketone-based colloidal silica sol) (Nissan Chemical) was prepared. Then, the entirety of CdSe / ZnS synthesized above and 10 g of MEK-ST were mixed and then mixed with octylmine Add an amine. The dried product thereof has a strong luminescent performance and can ensure excellent luminescence without the surface treatment of silica.
[Practical Example 3] Quantum dot-silica co-precipitation
(WSN) was synthesized according to the known technology. After purification, it was surface-treated with methyl trimethoxysilane and adjusted to a concentration of 30 wt% and dispersed in MEK. Then, the entire CdSe / ZnS solution and 10 g of WSN Is mixed and dried. At this time, an amine such as octylmine can be added to improve the luminescence. The dried product thereof has a strong luminescent performance and can be surface-treated with silica only for mixing.
According to the method for producing a quantum dot-nonabsorbing medium composite according to the present invention and the quantum dot-polymer composite produced thereby, a non-absorbing material is automatically formed when an external substance is added or synthesized, By keeping the inherent luminous properties of the quantum dots by inserting them as spacers, the production process is simple, and it is possible to control the luminescent properties of quantum dots by addition of amines or thiols.
In addition, by controlling the distance between the quantum dots, it is possible to suppress the generation of FRET, thereby maintaining the intrinsic fluorescence of the quantum dot and preventing the spectrum distortion.
Further, when a heat resistant material such as silica is used as a spacer between quantum dots, the heat resistance of the quantum dot containing composite can be increased.
In addition, when the same chemical resistant material such as silica is present between the quantum dots, the substance plays a role of protecting the quantum dots in the external chemical environment, so that the chemical resistance of the quantum dots containing complex can be improved.
Although the present invention has been described with reference to the accompanying drawings, it is to be understood that various changes and modifications may be made without departing from the spirit of the invention. Therefore, the scope of the present invention should not be limited to the described embodiments, but should be determined by the scope of the appended claims and equivalents thereof.
Claims (13)
The quantum dots include,
A nanocrystal of Si-based nanocrystals, II-VI-based compound semiconductor nanocrystals, III-V-based compound semiconductor nanocrystals, IV-VI-based compound semiconductor nanocrystals, and nanocrystals of any of these compounds. ≪ / RTI >
The quantum dots include,
Wherein the quantum dot comprises a CdSe / ZnS quantum dot, an InP / ZnS quantum dot, an alloy quantum dot, and a gradient quantum dot.
Wherein the inert matrix material comprises
A method of producing a quantum dot-non-absorbing medium composite, which is a molecular material of an organic material or an organic metal compound, a particulate material of a metal oxide, or a mixture of the molecular material and the particulate material.
The molecular material may be,
A metal salt having an alkyl or aryl group.
The molecular material may be,
A method for producing a quantum dot-non-mucosal matrix composite comprising any one of or a combination of zinc stearate (ZnSt 2 ) and manganese stearate (MnSt 2 )
The particulate material may be,
Method of producing a composite light-medium biheup - either or, the quantum dot including the combination thereof from the polymer beads, SiO 2 (Silica), TiO 2 (Titania).
Wherein the polymer is mixed with the inactive matrix material in which the plurality of quantum dots are dispersed.
The polymer may be,
PDMS (polydimethylsiloxane) family of polymers. A method for preparing a quantum dot-nonabsorbent matrix composite capable of controlling the luminance.
Wherein the quantum dot and the passive matrix material are doped with
To be mixed in a state dissolved or dispersed in an organic solvent.
Wherein the quantum dot and the passive matrix material are doped with
In a powder state so as to be introduced into a polymer solution to be mixed therewith.
Wherein the luminescence properties of the quantum dots are controlled by further mixing an amine or a thiol.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200001764A (en) * | 2018-06-28 | 2020-01-07 | (주)디씨티 | Quantum dot complex and method for manufacturing the same |
| KR20200001765A (en) * | 2018-06-28 | 2020-01-07 | (주)디씨티 | Photo-curable resin composition and quantum dot sheet comprising the same |
| KR20200020141A (en) * | 2018-08-16 | 2020-02-26 | (주)디씨티 | Led package including quantum dot |
| KR20200020139A (en) * | 2018-08-16 | 2020-02-26 | (주)디씨티 | Nanophosphor sheet |
| KR20200042873A (en) * | 2018-10-16 | 2020-04-24 | 연세대학교 산학협력단 | Multi-states Photoresponsive Polymer-QD Nanocomposite by Multiple Optical Switches |
| US10680144B2 (en) | 2017-06-05 | 2020-06-09 | Samsung Electronics Co., Ltd. | Quantum dot glass cell and light-emitting device package including the same |
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| US10680144B2 (en) | 2017-06-05 | 2020-06-09 | Samsung Electronics Co., Ltd. | Quantum dot glass cell and light-emitting device package including the same |
| KR20200001764A (en) * | 2018-06-28 | 2020-01-07 | (주)디씨티 | Quantum dot complex and method for manufacturing the same |
| KR20200001765A (en) * | 2018-06-28 | 2020-01-07 | (주)디씨티 | Photo-curable resin composition and quantum dot sheet comprising the same |
| KR20200020141A (en) * | 2018-08-16 | 2020-02-26 | (주)디씨티 | Led package including quantum dot |
| KR20200020139A (en) * | 2018-08-16 | 2020-02-26 | (주)디씨티 | Nanophosphor sheet |
| KR20200042873A (en) * | 2018-10-16 | 2020-04-24 | 연세대학교 산학협력단 | Multi-states Photoresponsive Polymer-QD Nanocomposite by Multiple Optical Switches |
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