KR101874811B1 - Apparatus of synthesizing quantum dot and process of synthesizing quantum dot - Google Patents

Apparatus of synthesizing quantum dot and process of synthesizing quantum dot Download PDF

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KR101874811B1
KR101874811B1 KR1020160009131A KR20160009131A KR101874811B1 KR 101874811 B1 KR101874811 B1 KR 101874811B1 KR 1020160009131 A KR1020160009131 A KR 1020160009131A KR 20160009131 A KR20160009131 A KR 20160009131A KR 101874811 B1 KR101874811 B1 KR 101874811B1
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core
quantum dot
precursor
shell
reaction
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KR20170089127A (en
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이경열
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(유)윈앤테크
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J14/00—Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • B82B3/0004—Apparatus specially adapted for the manufacture or treatment of nanostructural devices or systems or methods for manufacturing the same
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    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals

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Abstract

A precursor reaction unit having a reaction space in which a solution of a quantum dot (QD) precursor can be charged, and having a pump and a gas inlet; A core reaction unit for synthesizing a quantum dot core through a coil-shaped core mixing unit in which a solution of a quantum dot precursor injected from the precursor reaction unit and a synthesis solution for a core constituting a quantum dot are mixed; A shell reaction unit for synthesizing quantum dots of a core-shell structure through a coil-shaped shell mixing unit in which a quantum dot core synthesized in the core reaction unit and a synthesis solution for a shell constituting a quantum dot are mixed, and And a quantum dot synthesis method using the same.

Description

TECHNICAL FIELD [0001] The present invention relates to a quantum dot synthesizing apparatus and a quantum dot synthesizing method,

The present invention relates to quantum dot synthesis, and more particularly, to a device capable of synthesizing quantum dots having a uniform light emission distribution and a simple synthesis process, and a stable quantum dot synthesis method using the apparatus.

With the development of technology, nano-technology (NT), which is intended to synthesize so-called nanomaterials having a nanometer size and utilize nanomaterials in various industries, is attracting attention. When the size of a material is reduced to nanometers, nanotechnology researches and develops the properties of such nanomaterials, as it has various electrical and chemical properties that could not be seen with larger particles.

As the size of the material becomes smaller and the dimension of the material becomes lower, a quantum confinement effect that does not appear in general materials appears. Particularly, in the case of a zero-dimensional nano semiconductor material which is smaller than the de Broglie wavelength involved in all the particles having momentum, the band gap energy of the particle increases relatively as the size of the material decreases. Therefore, Various colors can be realized. Among these nanomaterials, Quantum Dot, which is a zero-dimensional semiconductor crystal material having a diameter of several tens of nanometers or less, is attracting attention as a material that can be applied to various industrial fields.

The quantum dots can accommodate a wider range of sunlight than conventional solar cells because they can absorb various wavelengths of sunlight depending on their size. Quantum dots are similar in size to proteins, which are the main molecules of living organisms, and can be used for drug diagnosis and biomaterials. In addition, quantum dots are also applied to electronic devices and displays because the color of emitted light changes according to size.

Since Qdots are chemically synthesized inorganic materials, they are stable, cost-effective, and have a longer life than organic light-emitting diodes (OLEDs) based on organic materials that can be decomposed by optical reaction. In addition, quantum dots have better color reproducibility than OLEDs and can compensate for the disadvantages of liquid crystal displays (LCDs). The full width at half maximum (FWHM) is about 20-30 nm, It has the advantage of excellent color purity because it is narrow. As a result, the quantum dot is attracting attention as a next-generation light emitting device in the display field.

As a method for synthesizing a quantum dot, an organometallic compound, which is a metal precursor constituting a quantum dot, is injected into a high-temperature solvent and thermally decomposed to obtain a metal ion concentration higher than a nuclear threshold, Solution synthesis methods that synthesize on a colloidal solution that grows nanocrystals through a thermodynamic process are generally adopted. Through the solution synthesis method, quantum dot synthesis can be classified into a precursor synthesis process, a core synthesis process, a shell synthesis process, and a precipitation process for synthesizing a quantum dot in an appropriate solution.

For example, Patent Document 1 proposes a quantum dot manufacturing apparatus for reacting a precursor solution with a solvent using an agitating means such as an impeller. However, in the case of the apparatus for producing quantum dots in Patent Document 1, it is difficult to control the quantum dot synthesis reaction time as desired. As a result, the reaction time for synthesizing the quantum dots may be prolonged. Further, when a magnetic stirrer is used, the quantum dots can not be uniformly synthesized throughout the reaction part. Therefore, the conventional quantum dot synthesizer and the quantum dot synthesized using the same have a problem of low stability and low quantum efficiency, and it is difficult to control the luminous efficiency of the quantum dot.

Korean Patent No. 10-1295543

It is an object of the present invention to simplify a quantum dot synthesis process, to induce quantum dot synthesis at a uniform temperature, And a quantum dot synthesis method.

Another object of the present invention is to provide a quantum dot synthesizer and a quantum dot synthesis method capable of synthesizing uniformly dispersed nano quantum dot particles to increase quantum efficiency and luminous efficiency thereby to synthesize quantum dots having improved sharpness.

According to an aspect of the present invention, there is provided a semiconductor device comprising: a precursor reaction unit having a reaction space in which a quantum dot (QD) precursor solution can be filled, the precursor reaction unit being heatable by a heat treatment unit; A core reaction unit for synthesizing a quantum dot core through a coil-shaped core mixing unit in which a quantum dot precursor solution injected from the precursor reaction unit and a quantum dot core synthesis solution are mixed; And a shell reaction unit for synthesizing quantum dots of a core-shell structure through a coil-shaped shell mixing unit in which a quantum dot core synthesized in the core reaction unit and a quantum dot shell synthesis solution are mixed.

The core reaction unit may include a first core reaction unit having a coil-shaped first core mixing unit thermally treated at a temperature ranging from 200 to 400 ° C so that the quantum-dot precursor solution reacts with the core synthesis solution, And a second core reaction portion having a coil-shaped second core mixing portion adjusted to a temperature ranging from 5 to 20 DEG C so as to cool the quantum dot core.

The shell reaction part includes a first shell reaction part having a coil-shaped first shell mixing part that is heat-treated at a temperature ranging from 200 to 300 ° C so that the quantum dot core and the shell synthesis solution react with each other, And a second shell reaction part having a coil-shaped second shell mixing part adjusted to a temperature ranging from 5 to 20 DEG C so as to cool the quantum dots of the shell structure.

For example, at least one of the quantum dot core and the quantum dot shell may be ZnS, ZnSe, ZnTe, CdS, CdSe, CdTe, HgS, HgTe, MgS, MgSe, MgTe, CaS, CaSe, CaTe, SrS, , BaS, BaSe, BaTe, GaN, GaP, GaAs, GaSb, InN, InP, InSb, Ge, Si and combinations thereof.

If necessary, one or more quantum dot buffer layers stacked between the quantum dot core and the quantum dot shell may be further synthesized in the shell reaction section.

According to another aspect of the present invention, there is provided a method of manufacturing a quantum dot precursor solution, comprising: reacting a precursor component capable of being heated by a heat treatment means with a quantum dot (QD) precursor component to obtain a quantum dot precursor solution; Introducing the quantum dot precursor solution synthesized in the precursor reaction part and a quantum dot core synthesis solution into a coil-shaped core mixing part located inside the coil reaction part to synthesize a quantum dot core; And introducing the synthesized quantum dot core and a quantum dot shell synthesis solution into a coil-shaped shell mixing portion located inside the shell reaction portion to synthesize quantum dots of the core-shell structure.

The step of synthesizing the quantum dot core may include the steps of injecting the quantum-dot precursor solution and the core synthesis solution into a coil-shaped first core mixing portion heat-treated at a temperature of 200 to 400 ° C, And cooling the quantum dot core by injecting the synthesized quantum dot core into a coil-shaped second core mixing portion controlled at a temperature ranging from 5 to 20 ° C.

The step of synthesizing the quantum dots of the core-shell structure may include the steps of injecting the quantum dot core and the shell synthesis solution into a coil-shaped first shell mixing portion heat-treated at a temperature of 200 to 300 ° C, And injecting the quantum dots of the core-shell structure synthesized through the mixing portion into the coil-shaped second shell mixing portion controlled at a temperature ranging from 5 to 20 ° C to cool the quantum dots of the core-shell structure .

At this time, in the step of synthesizing the quantum dots of the core-shell structure, one or more quantum dot buffer layers stacked between the quantum dot core and the quantum dot shell may be further synthesized.

The quantum dot manufacturing apparatus of the present invention includes a core reaction part having a coil-shaped mixing part, a core reaction part provided with a shell reaction part, and a shell reaction part. Therefore, in the case of adopting the quantum dot manufacturing apparatus of the present invention, quantum dots can be synthesized through a series of continuous processes from the production of the quantum dot precursor to the core synthesis and the shell synthesis.

It is possible to stir using a curved shape of a curved glass tube-shaped coil-shaped mixing part having a plurality of curved shapes, and the reaction time can be controlled according to the length of the curved glass tube, so that reaction time for synthesis of a quantum dot can be reduced. Further, since the core and the shell constituting the quantum dots can be uniformly dispersed by using the curved glass tube, it is possible to finally synthesize the quantum dots in which the core and the shell are uniformly dispersed.

As a result, the stability and quantum efficiency of the quantum dot produced by applying the quantum dot synthesizer according to the present invention can be maximized, and quantum dots having improved luminous efficiency and clarity can be synthesized.

1 is a view schematically showing a configuration of a quantum dot synthesizing apparatus according to an exemplary embodiment of the present invention.
2 is a schematic diagram schematically showing a configuration of a precursor reaction unit constituting a quantum dot synthesis apparatus according to an exemplary embodiment of the present invention.
3 is a schematic diagram schematically showing a configuration of a core and a shell reaction unit constituting a quantum dot synthesizing apparatus according to an exemplary embodiment of the present invention.
FIG. 4 is a photograph of a quantum dot synthesized according to an exemplary embodiment of the present invention, using a UV lamp. FIG.
5 is a graph showing a result of measuring PL (photoluminescence) intensity according to a wavelength band of a quantum dot synthesized according to an exemplary embodiment of the present invention.

The inventors of the present invention completed the present invention by studying a method capable of easily producing appropriate quantum dots according to need and synthesizing high quality quantum dots. Hereinafter, the present invention will be described in more detail with reference to the accompanying drawings when necessary.

1 is a view schematically showing a configuration of a quantum dot synthesizing apparatus according to an exemplary embodiment of the present invention. As shown in FIG. 1, a quantum dot (QD) synthesizer 100 according to the present invention includes a precursor reaction unit 200 having a reaction space in which a quantum dot precursor solution can be charged, a precursor reaction unit And a core / shell reaction unit 300 for synthesizing quantum dots by reacting a solution for synthesizing a core and a shell constituting a quantum dot. The quantum dots synthesized in the core / shell reaction unit 300 are accommodated in the storage unit 600 connected to the core / shell reaction unit 300, and can be applied to various fields such as a display light-emitting body.

The core / shell reaction unit 300 may be divided into a series of reaction units. The quantum dot precursor solution injected from the precursor reaction unit 200 and the quantum dot core synthesis solution are mixed to synthesize a quantum dot core. A core reaction unit 400 and a shell reaction unit 500 for synthesizing quantum dots of a core-shell structure by mixing a quantum dot core synthesized in the core reaction unit 400 and a quantum dot shell synthesis solution, have. The core reaction unit 400 and the shell reaction unit 500 may have coil-shaped core mixers 420 and 470 and coil-shell mixers 520 and 570, which may be curved glass tubes, Will be described later. If necessary, one or more quantum dot buffer layers stacked between the quantum dot core and the quantum dot shell in the shell reaction unit 500 may further be synthesized.

In connection with the present invention, the quantum dot produced by the synthesizing apparatus and the synthesizing method of the present invention is an inorganic semiconductor crystal having a particle diameter of approximately 1 to 1000 nm, preferably 1 to 30 nm, more preferably approximately 2 to 20 nm. Particles. ≪ / RTI > The quantum dot may be excited by light of a suitable wavelength band to emit light, and may be composed of one or more core surrounded by a shell of one or more layers. If necessary, one or more buffer layers may be formed between the core and the shell. In general, the band energy of a shell constituting a quantum dot is greater than the band energy of a core, and a shell close to the lattice constant or atomic spacing of the core substrate can be selected. In one exemplary embodiment, the quantum dot core and / or the quantum dot shell may be a ZnS, ZnSe, ZnTe, CdS, CdSe, CdTe, HgS, HgSe, HgTe, MgS, MgSe, MgTe, CaS, CaSe GaN, GaP, GaAs, GaSb, InN, InP, and InSb, which are III-V groups of the periodic table, Ge, Si, which is a Group IV of the periodic table, and combinations thereof For example, InGaAs, InGaP, ZnCdSe, SiGe), but the present invention is not limited thereto.

On the other hand, the quantum dot buffer layer that can be laminated between the quantum dot core and the quantum dot shell can be selected in consideration of the lattice constants of the core and the shell. For example, the quantum dot buffer layer may be selected from the group consisting of CdZnS, GaN, GaAs, InAs, InGaAs, GaP, InP, InGaP, GaAsP, InGaAsP and combinations thereof, but the present invention is not limited thereto.

The shapes of the respective reaction parts constituting the quantum dot synthesizing apparatus 100 according to the present invention will be described with reference to Figs. 2 and 3. Fig. 2 is a schematic diagram schematically showing a configuration of a precursor reaction unit constituting a quantum dot synthesis apparatus according to an exemplary embodiment of the present invention. The core / shell reaction part includes a cadmium selenide (CdSe) as a quantum dot core, a cadmium selenide (CdSe) as a buffer layer considering a lattice constant, and a cadmium zinc sulphide zinc sulfide, CdZnS), and a zinc sulfide (ZnS) as a quantum dot shell.

2, the precursor reaction unit 200 according to an exemplary embodiment of the present invention includes four precursor reaction units 210, 220, 230, and 240. As shown in FIG. In one exemplary embodiment, a three-necked flask may be used as the first to fourth precursor reacting portions 210, 220, 230, and 240, and a precursor compound may be additionally injected for continuous reaction of the precursor. Each of the precursor reacting units 210, 220, 230, and 240 has reaction spaces 211a, 221a, 221a, and 231a through which the precursor solution can be charged. Each of the precursor reacting units 210, 220, 230 and 240 is configured so that a precursor for synthesizing quantum dots can be obtained by the heat treatment means 211b, 221b, 231b, and 241b. As the heat treatment means 211b, 221b, 231b, and 241b, a physical device such as a heater or a heating mantle may be used, and a heating medium such as oil is particularly preferably used. When these heating mediums are used, stable and accurate heat treatment can be performed, and it is possible to maintain a constant temperature.

The first to fourth precursor reacting parts 210, 220, 230, and 240 may further include stirring means 212, 222, 232 and 242 such as an impeller for reacting with the reaction spaces 211a, 221a and 231a , 241a. Agitation means 212, 222, 232 and 242 induce uniform dispersion and reaction between the precursors for synthesizing the precursor solution constituting the quantum dot core, buffer layer and / or cell.

The first to fourth precursor reacting units 210, 220, 230 and 240 include gas injection units 214, 224, 234 and 244 and pumps 216, 226, 236 and 246, respectively. An inert gas such as nitrogen gas, for example, moisture removed, is injected into the reaction part through the gas injection parts 214, 224, 234 and 244. Accordingly, it is possible to prevent oxidation of reactants to be charged in the reaction spaces 211a, 221a, 231a and 241a in the respective precursor reacting units 210, 220, 230 and 240, It is possible to provide the effect of inducing the reactants such as the precursor solution to pass smoothly through the first to fourth precursor reacting parts 210, 220, 230, and 240. At this time, the inert gas may be injected at a rate of about 0.2 L / min or more, for example, 0.2 to 2.0 L / min or more.

In addition, discharge valves 218, 228, 238 and 248 are provided at the lower ends of the first to fourth precursor reacting sections 210, 220, 230 and 240, and the discharge valves 218, 228, 238 and 248 Precursor transferring lines 250a, 250b, 250c, and 250d capable of injecting the precursor solution synthesized in the first to second precursor reacting parts 210, 220, 230, and 240 into the core / Respectively.

The first to fourth precursor reacting units 210, 220, 230, and 240 may include pumps 216, 226, 236, and 246, respectively, which may be, for example, vacuum pumps. By operating these pumps 216, 226, 236 and 246, the pressure in the reaction spaces 211a, 221a, 231a and 241a where the precursors are synthesized is maintained in a high-vacuum state of 10 -2 Torr or more, , 220, 230, and 240 can be removed. In addition, the reagents for synthesizing precursors in the first to fourth precursor reacting parts 210, 220, 230, and 240 may cause the reaction part 210 (210, 220, 230, , 220, 230, 240).

In one exemplary embodiment, each precursor that can constitute a quantum dot core, a buffer layer and / or a cell in the first to fourth precursor reacting sections 210, 220, 230, 240 can be synthesized. For example, a cadmium precursor is synthesized in the first precursor reaction unit 210, a selenium precursor is synthesized in the second precursor reaction unit 220, a zinc precursor is synthesized in the third precursor reaction unit 230, A sulfur precursor may be synthesized in the precursor reaction unit 240.

The first precursor reacting part 210 may be filled with a cadmium precursor solution such as cadmium salt, cadmium oxide, or organo cadmium. Examples of cadmium salts are those in which the anion is selected from the group consisting of acetateates or other carboxylates (for example, formates, decanates, and alkanates or alkanates, oxalates, maleates, adipates, etc.) Nitrates, nitrites, sulfates, sulfites, perchlorates, chlorates, carbonates, carbamates, substituted phosphates, and salts thereof. And substituted borates such as phosphates, fluorides, chlorides, bromides, iodides, hydroxides and tetrafluoroborates, including hexafluorophosphate. ≪ / RTI > borates. Although dimethylcadmium may be particularly used as the organic cadmium, other organic cadmiums, in which the organic moiety may be methyl ethylbutyl phenyl and combinations thereof, may also be used.

In one exemplary embodiment, the cadmium salt, for example, a cadmium precursor solution such as cadmium oleate, may be charged to the first precursor reacting portion 210. Specifically, cadmium oxide, oleic acid (OA), 1-octadecene (ODE) are added to the reaction space 211a of the first precursor reaction unit 210, And the cadmium precursor is synthesized in a nitrogen gas atmosphere introduced through the gas inlet 214. [ The first precursor reaction part 210 is heat-treated at a temperature of 160 to 180 ° C by using a heat treatment means 211b such as oil to obtain a cadmium precursor, and reacts the reaction product for 30 minutes or more before cooling.

In the second precursor reacting section 220, a selenium salt, for example, a selenium precursor solution such as a phosphine salt substituted with an alkyl group having 1 to 20 carbon atoms, such as trialkylphosphine selenium or selenium dioxide, have. For example, selenium and tri-n-octyl phosphine (TOP) are added to the reaction space 221a of the second precursor reaction part 220, And these reactants are stirred by stirring means 222. The selenium precursor is synthesized in a nitrogen gas atmosphere introduced through the gas inlet 224. The second precursor reacting part 220 is heat-treated at a temperature of 90-110 ° C by using a heat treatment means 221b such as oil to obtain a selenium precursor, and reacts the reaction product for 30 minutes or more before cooling.

In the third precursor reaction unit 230, a zinc precursor solution such as a zinc salt, a zinc oxide, and an organo zinc may be charged. Examples of zinc salts are those in which the anion is selected from the group consisting of acetateates or other carboxylates (e.g., formates, decanates, and alkanates or alkenates, oxalates, maleates, adipates, etc.) Nitrates, nitrites, sulfates, sulfites, perchlorates, chlorates, carbonates, carbamates, substituted phosphates, and salts thereof. And substituted borates such as phosphates, fluorides, chlorides, bromides, iodides, hydroxides and tetrafluoroborates, including hexafluorophosphate. ≪ / RTI > borates. Diethylzinc may particularly be used as the organic zinc, but other organic zinc, which may also be an organic moiety methyl, ethyl, butyl, phenyl and combinations thereof, may also be used.

In one exemplary embodiment, the zinc precursor solution, such as a zinc salt, such as zinc oleate, may be filled into the third precursor reacting portion 230. Specifically, zinc oxide, oleic acid (OA), and 1-octadecene (ODE) are added to the reaction space 231a of the third precursor reaction unit 230, To stir the reactants. Then, a zinc precursor is synthesized in a nitrogen gas atmosphere introduced through a gas inlet 234. The third precursor reaction part 230 is heat treated at a temperature of 270 to 330 ° C, preferably 280 to 320 ° C, using a heat treatment means 231b such as oil to obtain a zinc precursor, Allow to cool.

In the fourth precursor reaction unit 240, a sulfide salt, for example, a phosphine salt substituted with an alkyl group having 1 to 20 carbon atoms, such as a trialkylphosphine sulfide salt, a 1-octadecene sulfide , ODES) can be charged with a sulfur precursor solution comprising an aliphatic or aromatic alkene sulfide salt having from 5 to 30 carbon atoms. For example, sulfur and ODE are added to and filled in the reaction space 241a of the fourth precursor reaction unit 240, and these reactants are stirred by the stirring means 242. [ Next, a sulfur precursor is synthesized in a nitrogen gas atmosphere introduced through a gas inlet 244. The fourth precursor reaction part 240 is heat-treated at a temperature of 110 to 130 ° C by using a heat treatment means 241b such as oil to obtain a sulfur precursor, and reacts the reaction product for at least 30 minutes before cooling.

2 illustrates a precursor reaction unit 200 including four reaction units 210, 220, 230, and 240 as an example. However, the number of reaction units constituting the precursor reaction unit 200 is not limited to the quantum dot And the structure of the quantum dots, the number of the precursor reacting portions may be varied, and the range of the heat treatment temperature applied to each precursor reaction portion may vary.

Next, the structure of the core / shell reaction unit 300 for synthesizing the quantum dots of the structure of the core-shell (optionally including the buffer layer between the core and the shell) using the precursor solution obtained through the precursor reaction unit 200 Will be described with reference to FIG. 3 is a schematic diagram schematically showing a configuration of a core and a shell reaction unit constituting a quantum dot synthesizing apparatus according to an exemplary embodiment of the present invention.

3, the core / shell reaction unit 300 includes a core reaction unit 300, a core reaction unit 300, and a core reaction unit 300. The core reaction unit 300 includes a core reaction unit 200, And a shell reaction unit 500 for synthesizing the quantum dots of the core-shell structure or the quantum dots of the core-buffer layer-shell structure by reacting the quantum dot core synthesized in the core reaction unit 400 with the quantum dot shell synthesis solution do.

The core reactor 400 includes a first core reactor 410, which may be a heating reactor that is heated to a high temperature so that the precursor solution supplied from the precursor reactor 200 (see FIG. 2) And a second core reaction unit 460, which may be a cooling reactor for cooling the quantum dot core synthesized in the first core reaction unit 410. The precursor solution synthesized in the precursor reaction unit 200 (see FIG. 2) is supplied to the first core reaction unit 410 (see FIG. 2) through a precursor supply line 412 connected to the precursor transfer lines 250a, 250b, 250c and 250d And the quantum dot core synthesis solution is supplied through the core injection unit 414 formed independently of the precursor supply line 412 to the coil-shaped first core mixer 420 of the first core reaction unit 410, Shaped first core mixing portion 420. The first core mixing portion 420 is formed in a shape.

In one exemplary embodiment, the quantum dot core synthesized in the first core reaction unit 410 may be a cadmium selenium compound (CdSe). At this time, the precursor solution supplied to the coil-shaped first core mixer 420 through the precursor supply line 412 flows through the cadmium oleate synthesized in the first precursor reactor 210 (see FIG. 2) and the second precursor reactor N-octylphosphine selenium (TOPSe), synthesized in WO-220, see Fig. 2). The quantum dot core synthesis solution injected into the coil-shaped first core mixer 420 through the core injector 414 may include one or more of octadecene (ODE), tri-n-octylphosphine oxide (TOPO) (OLA). ≪ / RTI >

The first core mixer 420 may be a glass tube having a curved shape in which the precursor solution supplied through the precursor supply line 412 and the core injector 414 is mixed with the core synthesis solution, . Accordingly, the precursor solution and the quantum dot core synthesis solution can be circulated through the coil-shaped first core mixer 420 while stirring. Circulation control valves 422 and 424 are respectively disposed at both ends of the coil-shaped first core mixer 420 to inject and circulate the precursor solution and the quantum-dot core synthesis solution into the coil-shaped first core mixer 420 . The entire length or inner diameter of the coil-shaped first core mixing portion 420 and the total amount of the precursor solution and the quantum-dot core synthesis solution in the coil-shaped first core mixing portion 420 due to the opening and closing of the circulation control valves 422 and 424 The quantum dot core of a desired wavelength band can be synthesized by controlling the circulation time, i.e., the reaction time.

With respect to the nanomaterial, when the size of the quantum dots becomes smaller than the radius of the exciton in which the electrons and the holes constituting the semiconductor material are coupled by the coulomb force, the movement of the electrons constituting the semiconductor material becomes a quantum A quantum confinement effect occurs. The quantum confinement effect shows discontinuous quantized energy levels. The quantum dots have a characteristic that the energy band gap (E g ) varies with size and shape. That is, as the size of the quantum dots decreases, the exciton transition energy increases. Therefore, by controlling the size of the quantum dots, the energy band gap can be widely changed over the visible ray region to the ultraviolet ray / infrared region. Generally, as the crystal growth time of the nanomaterial particles such as the quantum dots increases, the size of the quantum dots increases, the fluorescence color of the quantum dots changes from blue to red, and the absorption and fluorescence spectra move to a longer wavelength.

In the present invention, the length and inner diameter of the coil-shaped first core mixing portion 420, in which the precursor solution and the quantum-dot core synthesis solution are mixed and reacted, are adjusted and / or adjusted at both ends of the first coil- The particle size of the quantum dot core can be controlled by adjusting the opening and closing times of the circulation control valves 422 and 424.

For example, when the total amount of reactants such as the precursor solution supplied to the coil-shaped first core mixer 420 and the quantum-dot core synthesis solution is 500 mL, the inner diameter of the coil-shaped first core mixer 420 is The total length of the curved coil, which is the coil-shaped first core mixing portion 420, is approximately 70 to 130 cm, preferably approximately 1 to 5 cm, preferably 2 to 4 cm, more preferably 2.5 to 3.5 cm, May be 80 to 120 cm, and more preferably 90 to 110 cm. At this time, preferably, in the coil-shaped first core mixer 420, the reaction solution is mixed into the coil-shaped first core mixer 420 so that the reactant precursor solution and the quantum- To 70% by volume, preferably 40 to 60% by volume.

On the other hand, on the side of the first core reaction part 410, a first heating medium inlet line 432 for supplying a high-temperature heating medium, for example, heated oil to the outside of the coil-shaped first core mixing part 420, And a first heat medium discharge line 434 for discharging the heat medium circulated in the first core reaction part 410 to the outside. The temperature of the coil-shaped first core mixing portion 420 constituting the first core reaction portion 410 can be raised by the inflow and discharge of the heating medium. Accordingly, the quantum dot core can be synthesized by reacting the precursor solution introduced into the coil-shaped first core mixer 420 with the solution of the quantum dot core synthesis solution.

For example, when a cadmium selenium compound (CdSe) is to be synthesized as a quantum dot core according to one exemplary embodiment, the precursor solution and the precursor solution in the first core- The precursor solution and the quantum dot core synthesis solution are mixed in the coil-shaped first core mixer 420 for 60 minutes or less, preferably 30 minutes or less, for 200 minutes or less, so that the quantum- 400 ° C, preferably 200 to 300 ° C.

The size of the synthesized quantum dot particles can be controlled according to the reaction temperature and the reaction time described above, so that the emission spectrum of the quantum dot can be controlled. As the reaction temperature and / or reaction time become longer, the quantum dot core particles grow and the wavelength of the emission spectrum changes according to the particle size. When the reaction temperature and / or the reaction time is less than the above-mentioned range, the growth of the quantum dot core may not occur. If the reaction temperature and / or the reaction time exceed the above-mentioned range, the quantum dot particles become very large, There is no problem.

When the quantum dot core is synthesized by mixing and reacting the precursor solution and the quantum dot core synthesis solution, the circulation control valve 426 located downstream of the first coil mixer 420 is opened and closed. Accordingly, the quantum dot core heated to a high temperature is discharged from the first core reaction section 410 through the first core discharge line 426 connected downstream of the coil-shaped first core mixing section 420. The first core discharge line 426 is connected to the core inflow line 462 through the valve 450 and the core inflow line 462 is connected to the second coil reacting section 460 And is connected to the core mixing section 470. Shaped second core mixing portion 460 on the side of the second core reaction portion 460 so that the quantum dot core flowing into the coil-shaped second core mixing portion 470 in the second core reaction portion 460 can be cooled. A coolant inflow line 482 for supplying a coolant such as cooling water to the outside of the second core reaction part 470 and a coolant discharge line 484 for discharging the coolant circulated inside the second core reaction part 460 to the outside have. The temperature of the coil-shaped second core mixing portion 470 constituting the second core reaction portion 460 can be controlled by the inflow and discharge of the coolant. For example, the temperature of the coil-shaped second core mixing portion 470 may be lowered to 5 to 20 ° C by the inflow of a coolant to cool the quantum dot core introduced from the first core reaction portion 410.

Next, the shell reaction unit 500, which can be continuously connected to the core reaction unit 400, will be described. The shell reaction unit 500 includes a first shell reaction unit 510, which may be a reaction unit for heating a high-temperature heat treatment so that the quantum-dot-core solution supplied from the core reaction unit 400 can react with the quantum- And a second shell reaction unit 560, which may be a cooling reactor for cooling the quantum dot shell synthesized in the first shell reaction unit 510.

The quantum dot core solution synthesized in the core reaction unit 400 is supplied to the first core reaction unit 460 through the core discharge line 476 connected to the downstream side of the coil-shaped second core mixing unit 570 located inside the second core reaction unit 460, And is supplied to the shell reaction unit 510. The core discharge line 476 is connected to the core supply line 512 through a valve 490 and the core supply line 512 is connected to a coiled first shell mixer 520, respectively. Meanwhile, the quantum dot shell synthesis solution is injected into the coil-shaped first shell mixing portion 520 of the first shell reaction portion 510 through the shell injection portion 514 formed independently of the core supply line 512.

In one exemplary embodiment, the quantum dot shells synthesized in the first shell reacting section 510 may be zinc sulfide (ZnS). At this time, the quantum dot shell synthesis solution injected into the coil-shaped first shell mixing portion 520 through the shell injection portion 514 may be ODES synthesized in the fourth precursor reaction portion 240 (see FIG. 2). If necessary, a quantum dot buffer layer synthesis solution stacked one or more layers between the quantum dot core and the quantum dot shell may be injected through the shell injection section 514 to form one or more buffer layers between the quantum dot core and the quantum dot shell. For example, the quantum-dot buffer layer synthesis solution may include cadmium oleate synthesized in the first precursor reaction unit 210 (see FIG. 2), zinc oleate synthesized in the third precursor reaction unit 230 (see FIG. 2), 1-octadecene ) And oleylamine (OLA).

The first core-mixer 420, in which the quantum-dot core solution supplied and injected through the core supply line 512 and the shell injection unit 514 are mixed with the quantum-point shell synthesis solution, . Accordingly, the quantum dot core solution supplied through the core supply line 512 and the quantum dot shell solution injected through the shell injection unit 514 can be circulated through the coil-shaped first shell mixer 520 do. Circulation control valves 522 and 524 are positioned at both ends of the coil-shaped first shell mixing section 520 for injection and circulation of the quantum dot core solution and the quantum dot shell synthesis solution into the coil-shaped first shell mixing section 520 have. The entire length or inner diameter of the coil-shaped first shell mixing portion 520 and the quantum dot core solution and the quantum dot shell synthesis solution in the coil-shaped first shell mixing portion 520 due to the opening and closing of the circulation control valves 522 and 524 It is possible to synthesize a quantum dot core having a desired wavelength band by controlling the circulation time of the quantum dot, i.e., the reaction time.

According to one exemplary embodiment, the length and inner diameter of the coil-shaped first shell mixing portion 520 in which the quantum dot core solution and the quantum dot shell synthesis solution are mixed and reacted can be adjusted and adjusted, The particle size of the quantum dot core can be controlled by adjusting the opening and closing times of the circulation control valves 522 and 524 disposed at both ends of the unit 520. [

For example, when the total amount of reactants such as the quantum dot core solution and the quantum dot shell synthesis solution fed into and injected into the coil-shaped first shell mixer 520 is 500 mL, the inner diameter of the coil- 1 to 5 cm, preferably 2 to 4 cm, and more preferably 2.5 to 3.5 cm, and the total length of the curved coil as the coil-shaped first shell mixing portion 520 is approximately 70 to 130 cm, 80 to 120 cm, and more preferably 90 to 110 cm. At this time, preferably, in the coil-shaped first shell mixer 520, these reaction solutions are mixed in the coil-shaped first core mixer 520 so that the quantum-dot core solution and the quantum- 30 to 70% by volume, preferably 40 to 60% by volume.

On the other hand, on the side of the first shell reaction part 510, a second heating medium inlet line 532 for supplying a high-temperature heating medium, for example, heated oil to the outside of the coil-shaped first shell mixing part 420, And a second heat medium discharge line 534 for discharging the heat medium circulated inside the first shell reaction part 410 to the outside. The temperature of the coil-shaped first shell mixing portion 520 constituting the first shell reaction portion 510 can be raised by the inflow and discharge of the heating medium. Accordingly, the quantum dot shell can be synthesized by reacting the quantum dot core solution introduced into the coil-shaped first shell mixing portion 520 with the quantum dot shell synthesis solution. As described above, when necessary, the quantum dot core solution and the quantum dot buffer synthesis solution may react first to form a quantum dot buffer layer of one or more layers before synthesizing the quantum dot shell.

For example, a case is described in which cadmium zinc sulfide (CdZnS) is formed as a quantum dot buffer layer according to one exemplary embodiment, and then zinc sulfide (ZnS) is synthesized as a quantum dot shell. The quantum dot core solution (for example, CdSe) synthesized in the core reaction part 400 and the quantum dot buffer layer synthesis solution react first in the coil-shaped first shell mixing part 520 of the first shell reaction part 510, The quantum dot core solution and the quantum dot buffer layer synthesis solution can be reacted at a temperature of 200 to 300 DEG C for 60 minutes or less, preferably 30 minutes or less, in the coil-shaped first shell mixing portion 520 so as to form a buffer layer have. In this case, the quantum dot buffer layer may be stacked by one or more layers, for example, from 1 to 5 layers. When the quantum dot buffer layer is formed, the quantum dot shell synthesis solution is injected into the coil-shaped first shell mixing portion 520 through the shell supply line 512 and is injected into the coil-shaped first shell mixing portion 520 for 200 minutes or less, preferably 200 minutes or less, To 300 < 0 > C. Similar to the quantum dot buffer layer, the quantum dot shell may be formed of one or more layers, for example, one to five layers of quantum dot shells may be laminated.

The size of the synthesized quantum dot particles can be controlled according to the reaction temperature and the reaction time described above, so that the emission spectrum of the quantum dot can be controlled. As the reaction temperature and / or reaction time become longer, the quantum dot core particles grow and the wavelength of the emission spectrum changes according to the particle size. When the reaction temperature and / or the reaction time is less than the above-mentioned range, the growth of the quantum dot core may not occur. If the reaction temperature and / or the reaction time exceed the above-mentioned range, the quantum dot particles become very large, There is no problem.

When the quantum dot buffer layer and the quantum dot shell are synthesized by mixing and reacting the quantum dot core solution and the quantum dot shell synthesis solution and optionally the quantum dot buffer synthesis solution, the circulation control valve 526 located downstream of the coil- Respectively. Accordingly, the quantum dot shell heated at a high temperature is discharged from the first shell reaction portion 510 through the shell discharge line 526 connected downstream of the coil-shaped first shell mixing portion 520. The shell discharge line 526 is connected to the shell inlet line 562 through a valve 550 and the shell inlet line 562 is connected to the coil shaped second shell mix 560 disposed within the second shell reaction section 560. [ (570). The second shell reacting section 560 is provided so as to cool the quantum dot core-shell (quantum dot core-buffer layer-shell, if necessary) that flows into the coil-shaped second shell mixing section 570 in the second shell reaction section 560 A second coolant inflow line 582 for supplying a coolant, for example, cooling water, to the outside of the coil-shaped second shell mixing portion 570 on the side of the second shell reaction portion 560, And a second refrigerant discharge line 584 for discharging the refrigerant to the outside. The temperature of the coil-shaped second shell mixing portion 570 constituting the second shell reaction portion 560 can be adjusted by the inflow and discharge of the coolant. For example, the temperature of the coil-shaped second shell mixing portion 570 is lowered to 5 to 20 占 폚 by the inflow of the refrigerant, and the quantum dots of the core-shell structure introduced from the first shell reaction portion 510 - buffer layer - quantum dots of the shell structure).

The quantum dots of the core-shell structure cooled in the second shell reaction part 560 are discharged to the outside through the quantum dot discharge line 576 connected to the downstream side of the coil-shaped second cell mixing part 570. The valve 590 may be located in the quantum dot discharge line 576 to control the discharge of the cooled quantum dots through the quantum dot discharge line 576. The emitted quantum dots will be processed by particle size distribution so that only quantum dots of appropriate size can be separated.

3, a syringe pump is connected between the precursor supply line 412 and the core injection portion 414 and / or between the core supply line 512 and the shell injection portion 514 to form a precursor solution, The quantum dot core synthesis solution and / or the quantum dot buffer layer or the shell synthesis solution can be continuously supplied and injected into the first shell reaction part 410 by a predetermined amount.

Although not shown in the drawings, the first core reaction unit 410, the second core reaction unit 460, the first shell reaction unit 510, and the second shell reaction unit 560 may include a pump such as a vacuum pump So that the pressure of these reaction parts before the quantum dot core, the buffer layer and / or the shell are synthesized can be maintained in a high-vacuum state of 10 -2 Torr or more. Accordingly, moisture and impurities in the reaction parts 410, 460, 510, and 560 can be removed, and a solution for synthesizing the quantum dot core / buffer layer and / or shell can be removed from the reaction parts 410, 460, , These solutions can be rapidly introduced into the reaction parts 410, 460, 510, and 560 due to the pressure difference between the inside and the outside of the reaction part.

A fluid sensor or a pressure sensor (not shown) is disposed on the front and rear surfaces of the first core reaction unit 410, the second core reaction unit 460, the first shell reaction unit 510 and the second shell reaction unit 560, Not shown), so that it can be confirmed that the reaction solution flows in, and the reaction solution can be configured not to flow backward.

In addition, the reactors 410, 460, 510, and 560 each include a gas injection unit (not shown) when required, and an inert gas such as nitrogen gas from which water is removed is supplied to the reactors 410, 460, And the like. The reactants injected into the reactors 410, 460, 510, and 560 can be prevented from being oxidized, and the reactants can be formed in the reactors 410, 460, 510, and 560, (420, 470, 520, 570). At this time, the inert gas may be injected at about 0.2 L / min or more, for example, at 0.2 to 2.0 L / min or more.

At this time, a gas supply line (not shown) for introducing nitrogen gas into the reaction part for heating, such as the first core reaction part 410 and the first shell reaction part 510, is operated at a temperature substantially from room temperature to 400 ° C It is possible to minimize the change in the characteristics of the reaction solution due to the temperature of the nitrogen gas when the nitrogen gas contacts the reaction solution. The gas supply line (not shown) for introducing the nitrogen gas into the cooling reaction unit, such as the second core reaction unit 420 and the second shell reaction unit 520, It may be surrounded by 20 ℃ or less.

Hereinafter, the present invention will be described in more detail with reference to exemplary embodiments. However, the present invention is not limited to the technical idea described in the following embodiments.

Materials Used

The material for synthesizing the precursor, core, buffer and shell for synthesizing the quantum dots was a reagent of mode Sigma-Aldrich. Specifically, cadmium oxide (SKU 202894), oleic acid (OA, SKU 364528), 1-octadecene (ODE, SKU O806), selenium (SKU 209643) Octyl phosphine (TOP, SKU 117854), zinc oxide (SKU 205532), sulfur (S, SKU 213292), tri-n-octyl phosphine oxide, TOPO, SKU 346187) and oleylamine (OLA, SKU 07805) were used.

Example 1: Quantum dot CdSe / CdZnS (x) / ZnS (y) synthesis with an emission wavelength of 500 nm

(1) Synthesis of precursor

A precursor for synthesizing quantum dots was added to each precursor reaction part constituting the precursor reaction part 200 as shown in FIG. 0.432 g of cadmium oxide, 8.25 mL of oleic acid (OA) and 24.25 mL of 1-octadecene (ODE) were added to the first precursor reacting portion 210. 0.43 g of selenium (Se) and 5.50 mL of tri-n-octylphosphine (TOP) were added to the second precursor reaction portion (220). 0.50 g of zinc oxide (ZnO), 15.05 mL of OA and 44.26 mL of ODE were added to the third precursor reacting part 230 and 0.294 g of sulfur (S) and 91.81 mL of ODE were added to the fourth precursor reaction part 240 . Each precursor reaction part was agitated at 1000 rpm or more using a stirrer and a vacuum pump was operated to maintain the pressure inside the reaction part of each precursor at 10 -2 Torr or more, The impurities were volatilized. After maintaining the pressure and temperature for more than 30 minutes, the oil heater was operated to heat each reaction part. At this time, the operation of the vacuum pump was stopped, and nitrogen gas from which moisture was removed was injected into each of the precursor reaction parts at 0.2 L / min or more. The first precursor reaction unit 210 is maintained at 170 ° C, the second precursor reaction unit 220 is maintained at 100 ° C, and the third precursor reaction unit 220 is maintained at 100 ° C so that nitrogen gas is simultaneously injected into each precursor reaction unit, The precursor reaction unit 230 was heated at 300 ° C. and the fourth precursor reaction unit 240 was heated at 120 ° C. for 30 minutes using an oil heater. 32.50 mL of cadmium oleate was obtained from the first precursor reacting section 210 and 5.50 mL of tri-n-octylphosphine selenium (TOPSE) was obtained from the second precursor reacting section 220. 59.30 mL of zinc oleate was obtained in the third precursor reacting portion 230 and 91.80 mL of 1-octadecene sulfide (ODES) was obtained in the fourth precursor reacting portion 240.

(2) Quantum dot core synthesis

The precursor solution is transferred to the first core reaction part 410 provided with the coil-shaped curved glass tube mixer which can be heat-treated by the oil heater by opening the cock (discharge valve) in the lower part of the reaction part after reacting for 30 minutes each , The core synthesis solution and the precursor reactant were mixed to synthesize the CdSe core. Specifically, 4.80 mL of a cadmium oleate precursor solution synthesized in the first precursor reacting section 210 was injected into the first core mixer 420 of the first core reaction section 410, 24.0 mL of ODE, 3.30 mL of TOPO (90%), and 9.0 mL of OLA (70%) were injected into the coil-shaped first core mixer 420 through the solution inlet for the core, and the circulation control valve was closed. The temperature of the oil circulated around the coil-shaped first core mixer 420 is adjusted to 220 ° C so that the quantum dot core having the emission wavelength of 480 nm can be stably synthesized, and a separate reaction for the precursor solution and the core synthesis solution The precursor solution and the core solution were directly circulated without giving a holding time so that the quantum dot core was synthesized. When the quantum dot core having a desired wavelength is made, the second core reaction unit 460, in which the valve is opened so that the nano-sized quantum dot core can be deposited by the temperature difference, and oil or water maintained at 10 to 15 ° C is circulated outside the coil, The quantum dot core synthesized by the above method was transferred. The quantum dot core synthesized in the second core reaction section 460 is cooled until the temperature of the refrigerant is stabilized.

(3) Quantum dot synthesis of core-shell structure

After the temperature of the refrigerant is stabilized in the second core reactor 460, the valve of the second core reactor 420 is opened to supply the quantum dot core solution to the first shell reactor 510 heated by the oil heater at 230 ° C And injected into the coil-shaped first shell mixer 520. The quantum dot core solution was injected into the first shell reaction part 510. To synthesize the quantum dot buffer layer, 95.0 mL of ODE, 19.0 mL of OLA, 1.95 mL of cadmium oleate synthesized in the first precursor reaction part 210, 3.85 mL of zinc oleate synthesized in the precursor reaction unit 230 is injected into the coil-shaped curved surface shell mixer 520 of the first shell reaction unit 510 through the solution inlet, and the first shell reaction unit 510) was adjusted to 270 DEG C to form a buffer layer. After 15 minutes have elapsed from the introduction of the synthesis solution for forming the buffer layer, 5.85 mL of 1-octadecene sulfide (ODES) synthesized in the fourth precursor reaction part 240 is introduced into the first shell reaction part 510, To form a quantum dot shell on the surface of the core and buffer layer. When the quantum dot shell is formed, the valve is opened to transfer the reactant to the second shell reaction part 560 cooled at 10 to 15 ° C so that the synthesized core-shell can be precipitated. When the temperature of the refrigerant is stabilized, And the particles were separated to obtain a quantum dot of 100 mL.

Example 2: Quantum dot CdSe / CdZnS (x) / ZnS (y) synthesis with emission wavelength 520 nm

CdSe core having an emission wavelength of 500 nm was prepared by allowing the precursor solution and the core synthesis solution to react at a temperature of 220 ° C for 1 minute in the first core reaction section. To form a buffer layer, 2.1 mL of cadmium oleate and 4.2 mL of zinc oleate And the procedure of Example 1 was repeated except that 6.2 mL of ODES was used to synthesize the shell to obtain a quantum dot of 100 mL.

Example 3: Quantum dot CdSe / CdZnS (x) / ZnS (y) synthesis with emission wavelength of 540 nm

CdSe core having an emission wavelength of 520 nm was prepared by allowing the precursor solution and the core synthesis solution to react at 220 DEG C for 5 minutes in the first core reaction part. To form a buffer layer, 2.5 mL of cadmium oleate and 4.5 mL of zinc oleate And the procedure of Example 1 was repeated except that 6.8 mL of ODES was used to synthesize the shell to obtain a quantum dot of 100 mL.

Example 4: Quantum dot CdSe / CdZnS (x) / ZnS (y) synthesis with emission wavelength of 560 nm

CdSe core having an emission wavelength of 540 nm was prepared by reacting the precursor solution and the core synthesis solution at a temperature of 220 캜 for 15 minutes in the first core reaction part. To form a buffer layer, 2.8 mL of cadmium oleate and 5.2 mL of zinc oleate And the procedure of Example 1 was repeated except that 8.2 mL of ODES was used to synthesize the shell to obtain a quantum dot of 100 mL.

Example 5: Quantum dot CdSe / CdZnS (x) / ZnS (y) synthesis with emission wavelength of 580 nm

CdSe core having an emission wavelength of 560 nm was prepared by reacting the precursor solution and the core synthesis solution in a first core reaction portion at a temperature of 270 ° C without holding time. To form a buffer layer, 3.4 ml of cadmium oleate and 6.2 ml of zinc oleate And the procedure of Example 1 was repeated except that 9.5 mL of ODES was used to synthesize the shell to obtain a quantum dot of 100 mL.

Example 6: Quantum dot CdSe / CdZnS (x) / ZnS (y) synthesis at an emission wavelength of 600 nm

CdSe core having an emission wavelength of 580 nm was prepared by allowing the precursor solution and the core synthesis solution to react at a temperature of 270 캜 for 10 minutes in the first core reaction part. To form a buffer layer, 4.5 ml of cadmium oleate, 8.2 ml of zinc oleate , And the procedure of Example 1 was repeated except that 12 mL of ODES was used to synthesize the shell to obtain a quantum dot of 100 mL.

Example 7: Quantum dot CdSe / CdZnS (x) / ZnS (y) synthesis with an emission wavelength of 620 nm

CdSe core having an emission wavelength of 590 nm was prepared by allowing the precursor solution and the core synthesis solution to react at a temperature of 270 캜 for 20 minutes in the first core reaction part. To form a buffer layer, 5.8 mL of cadmium oleate, 10.2 mL And the procedure of Example 1 was repeated except that 16.2 mL of ODES was used to synthesize the shell, thereby obtaining a quantum dot of 100 mL.

Example 8: Quantum dot luminescence characteristics

The luminescence characteristics were measured for quantum dots synthesized in Examples 1 to 7 respectively. FIG. 4 is a photograph of the quantum dots synthesized in Example 1 using a UV lamp, and FIG. 5 is a graph showing a result of measuring PL intensity according to the wavelength band of the quantum dots synthesized in Example 1. FIG. As shown in the figure, the quantum dots synthesized using the device of Example 1 had excellent luminescence efficiency and it was confirmed that quantum dots with good color purity were synthesized according to the desired emission wavelength band.

Although the present invention has been described based on the exemplary embodiments and examples of the present invention, the scope of rights of the present invention is not limited to the technical ideas described in the above embodiments and examples. Those skilled in the art will appreciate that various modifications and changes may be made without departing from the scope of the present invention as defined by the appended claims. It will be apparent, however, that the appended claims are intended to cover all such modifications and changes as fall within the true scope of the invention.

100: Quantum dot synthesizer 200: Precursor reaction part
300: core / shell reaction part 400: core reaction part
410: first core reacting part 420: coil-shaped first core mixing part
460: second core reaction part 470: coil-shaped second core mixing part
500: Shell reaction part 510: First shell reaction part
520: coil-shaped first shell mixing portion 560: second shell reaction portion
570: coil-shaped second shell mixing portion

Claims (10)

A first precursor reaction part to a fourth precursor reaction part, each of which has a reaction space in which a quantum dot (QD) precursor solution can be filled, and which can be heated by a heat treatment device, And a second precursor reacting section which is heat-treated at a temperature of 90 to 110 ° C, respectively, are used to synthesize the first precursor and the second precursor of the quantum dot core, respectively, and the third precursor reacting section, which is heat- The precursor reaction unit and the fourth precursor reaction unit, which are thermally treated at a temperature of 110 to 130 ° C, include a precursor reaction unit for synthesizing the first precursor and the second precursor of the quantum dot shell, respectively;
A quantum dot core precursor solution injected from each of the first and second precursor reacting portions, and a mixed solution of 1-octadecene, tri-n-octylphosphine oxide and oleylamine A core reaction part for synthesizing a quantum dot core through a coil-shaped core mixing part in which a quantum dot core synthesis solution is mixed;
A quantum dot core synthesized in the core reaction unit and a quantum dot core synthesized in the core reaction unit are independently mixed with a quantum dot shell synthesis solution supplied from the third and fourth precursor reaction units, And a shell reaction unit for synthesizing the quantum dots of the core-shell structure through a portion of the core-shell structure.
The method according to claim 1,
The core reaction unit includes a first core reaction unit having a coil-shaped first core mixing unit thermally treated at a temperature ranging from 200 to 400 ° C so that the quantum-dot core precursor solution and the quantum-dot core synthesis solution react with each other, And a second core reaction part having a coil-shaped second core mixing part adjusted to a temperature ranging from 5 to 20 ° C so as to cool the quantum dot core synthesized in the second core reaction part.
The method according to claim 1,
The shell reaction part includes a first shell reaction part having a coil-shaped first shell mixing part which is heat-treated at a temperature ranging from 200 to 300 ° C so that the quantum dot core and the quantum dot shell synthesis solution react with each other, And a second shell reaction part having a coil-shaped second shell mixing part adjusted to a temperature ranging from 5 to 20 캜 so as to cool the quantum dots of the core-shell structure.
4. The method according to any one of claims 1 to 3,
Wherein the quantum dot core is a cadmium selenium compound (CdSe), and the quantum dot shell is zinc sulfide (ZnS).
4. The method according to any one of claims 1 to 3,
In the shell reaction unit, one or more quantum dot buffer layers stacked between the quantum dot core and the quantum dot shell are further synthesized.
(QD) precursor solution may be respectively filled in the reaction chamber, and the precursor reaction unit including the first precursor reaction unit through the fourth precursor reaction unit, which can be heated by the respective heat treatment units, is reacted with the quantum dot precursor component The first precursor reaction part being thermally treated at a temperature of 160 to 180 DEG C and the second precursor reaction part being heat-treated at a temperature of 90 to 110 DEG C may be formed by synthesizing a first precursor and a second precursor of the quantum- And a fourth precursor reacting part which is heat-treated at a temperature of from 270 to 330 ° C. and a fourth precursor reacting part which is heat-treated at a temperature of from 110 ° C. to 130 ° C. synthesizes the first precursor and the second precursor of the quantum dot shell to obtain a solution of a quantum dot precursor ;
A quantum dot core precursor solution synthesized in each of the first and second precursor reacting portions and a solution of a mixed solution of 1-octadecene, tri-n-octylphosphine oxide and oleylamine Forming a quantum dot core by injecting a quantum dot synthesis solution in a core-like core mixer located inside the core reaction section;
The quantum dot core solution synthesized in the core reaction unit and the quantum dot synthesis solution supplied respectively from the third and fourth precursor reaction units independently of the quantum dot core synthesized in the core reaction unit are placed in the shell reaction unit Shaped shell mixing portion to form a quantum dot of the core-shell structure.

The method according to claim 6,
The step of synthesizing the quantum dot core comprises the steps of injecting the quantum-dot core precursor solution and the quantum-dot core synthesis solution into a coil-shaped first core mixing portion heat-treated at a temperature of 200 to 400 ° C, And cooling the quantum dot core by injecting the quantum dot core synthesized through the first core portion into a coil-shaped second core mixing portion controlled at a temperature ranging from 5 to 20 ° C.
The method according to claim 6,
The step of synthesizing the quantum dots of the core-shell structure comprises the steps of injecting the quantum dot core and the quantum dot shell synthesis solution into a coil-shaped first shell mixing portion heat-treated at a temperature of 200 to 300 ° C, And a step of injecting the quantum dots of the core-shell structure synthesized through the shell mixing portion into a coil-shaped second shell mixing portion controlled at a temperature ranging from 5 to 20 ° C to cool the quantum dots of the core- Synthesis method.
9. The method according to any one of claims 6 to 8,
Wherein the quantum dot core is a cadmium selenium compound (CdSe), and the quantum dot shell is zinc sulfide (ZnS).
9. The method according to any one of claims 6 to 8,
Wherein one or more quantum dot buffer layers stacked between the quantum dot core and the quantum dot shell are further synthesized in synthesizing quantum dots of the core-shell structure.
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