KR101668480B1 - Surface treatment method for giving chemical resistance to quantum dot and quantum dot manufactured by the same - Google Patents
Surface treatment method for giving chemical resistance to quantum dot and quantum dot manufactured by the same Download PDFInfo
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- KR101668480B1 KR101668480B1 KR1020150117615A KR20150117615A KR101668480B1 KR 101668480 B1 KR101668480 B1 KR 101668480B1 KR 1020150117615 A KR1020150117615 A KR 1020150117615A KR 20150117615 A KR20150117615 A KR 20150117615A KR 101668480 B1 KR101668480 B1 KR 101668480B1
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Abstract
The present invention relates to a method for surface-treating an endothermic chemical resistance of a quantum dot, wherein a metal ion present on the surface of a quantum dot is replaced with a different kind of metal ion existing outside the quantum dot by a cation exchange reaction, Lt; / RTI >
According to the present invention, an inorganic shell coating is formed on a surface of a quantum dot in a simple and stable manner so as not to be influenced by an external environment, thereby having excellent chemical resistance and heat resistance, An inorganic layer having the nature of a buffer formed on the substrate may have a thickness that does not affect the luminescence property.
Description
TECHNICAL FIELD The present invention relates to a surface treatment method for imparting chemical resistance to a quantum dot and a quantum dot produced by the method, and more particularly, to a method for treating a surface of a quantum dot which is resistant to external environment, A surface treatment method and a quantum dot produced thereby.
In general, when a material is reduced in size to nanometers, it will have new physical properties not seen in the bulk state because the properties of materials change as the nanoscale and shape change.
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 the 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.
Conventional quantum dots as well as conventional quantum dots are synthesized at a high temperature using a high temperature pyrolysis method, and the higher the crystallinity, the higher the light emitting property. It has a hydrophobic property due to the presence of an alkyl chain on the surface of the particles, and thus has a characteristic of being dissolved only in a non-polar organic solvent.
Therefore, the quantum dot reacts sensitively to the external chemical environment due to the nano-sized small particles and the metal ions, together with the above-mentioned characteristics. Therefore, the luminescence is rapidly changed and the chemical resistance is poor. Resulting in poor heat resistance due to the surface being damaged and the luminescence being reduced rapidly. The lack of chemical resistance of the Qdots is evidence that the luminescence is reduced when the Qdot surface ligand substitution experiment is conducted. The quantum dots are not completely shielded from the external environment except the very thick CdS shell, and the inorganic shell coating is not complete and is affected by the external environment. Therefore, it was necessary to improve these disadvantages.
In order to solve the problems of the prior art as described above, the present invention provides a simple and stable inorganic shell coating on the surface of a quantum dot, so as not to be affected by the external environment, Chemical property and heat resistance, and has an inorganic layer having buffer characteristics formed at the outermost periphery of the quantum dots to have a thickness which does not affect the luminescence property.
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, metal ions existing on the surface of a quantum dots are subjected to a cation exchange reaction to form a heterogeneous metal ion existing outside the quantum dots A surface treatment method for imparting chemical resistance to the quantum dots is provided.
The substance exchanged with the different kind of metal ions has a larger atom or ion size than the metal ion on the surface of the quantum dots and has a lower band gap when replacing metal ions on the surface of the quantum dots Forming material.
When the outermost metal atom of the quantum dots is Zn, the material exchanged with the heterogeneous metal ions may include a part of Cd, Al, Ga (Gallium) and In (Indium).
Mixing the quantum dots into a solution containing the dissimilar metal ions and allowing the metal ions to exchange at the surface of the quantum dots at a temperature of 100 to 300 ° C; And cooling the quantum dot mixed solution after the metal ions have been exchanged, and then purifying the quantum dots with an organic solvent.
Octadecene (ODE) was added to the vessel so that the ligand was 5 to 100 mmol based on 10 mmol of CdO, and the 1-octadecene (ODE) was 10 To 2000 mL; Dissolving the CdO in a vacuum state at a temperature of 100 to 300 < 0 >C; Introducing a quantum dot into the solution in which the CdO is dissolved to exchange the metal ions of the surface of the quantum dot at a temperature of 100 to 300 ° C; And cooling the solution to purify the quantum dots with an organic solvent.
The ligand may be an alkyl acid, an alkyl phosphonic acid, an alkyl phosphinic acid, an aryl acid, an aryl phosphate, or an aryl phosphate, which can react with a metal to form a metal salt. And may include any one of aryl phosphonic acid and aryl phosphinic acid.
According to another aspect of the present invention, there is provided a quantum dot produced by a method for surface-treating an applied chemical resistance of a quantum dot according to an aspect of the present invention.
According to the method for surface treatment of chemical resistance of a quantum dot according to the present invention and the quantum dots produced by the method, an inorganic shell coating can be easily and stably applied to the surface of a quantum dot, , Thereby having excellent chemical resistance and heat resistance, and an inorganic layer having a buffer nature formed at the outermost part of the quantum dots can have a thickness not affecting the luminescence.
Fig. 1 is a view for explaining a method of treating a surface of a quantum dot to impart chemical resistance according to the present invention.
Fig. 2 is a diagram for explaining the reason why the change in luminescence is small due to the chemical-resistance-imparted surface treatment method of a quantum dot according to the present invention.
Fig. 3 is a flowchart showing a method of treating a surface of a quantum dot to impart chemical resistance according to an embodiment of the present invention.
Fig. 4 is an image before and after the chemical-imparting surface treatment 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.
Fig. 1 is a view for explaining a surface treatment method for imparting chemical resistance to a quantum dot according to the present invention, which shows that a CdSe / ZnS quantum dot is surface-treated with Cd ions.
As shown in FIG. 1 (a), the method for surface treatment of chemical resistance of quantum dots according to the present invention is characterized in that metal ions present on the surfaces of quantum dots are present on the outside of quantum dots by cation exchange reaction Exchange with a different kind of metal ion. Here, the temperature at which the metal ions existing on the surface of the quantum dots are displaced to the different metal ions is the temperature at which the metal ions on the surface as described above and the metal ions other than the above- And may be a temperature range for allowing a cation exchange reaction.
A substance exchanged with a different kind of metal ion has a larger atom or ion size than the metal ion on the surface of the quantum dots and a substance which forms a layer having a lower band gap when the metal ion on the surface of the quantum dots is replaced As shown in FIG. 1 (b), when the outermost metal atom of the quantum dot is Zn, it may include a part of Cd, Al, Ga (Gallium), and In (Indium). For example, When the material is ZnS, the material formed by exchanging with a different kind of metal ion may be, for example, CdS or ZnSe. In addition, the quantum dot may be any one of Si-based nanocrystals, II-VI-based compound semiconductor nanocrystals, III-V-based compound semiconductor nanocrystals, IV-VI-based compound semiconductor nanocrystals, Nanocrystals. 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. In addition, the quantum dot may be a compound in which the core is a Cd compound such as CdS, CdSe, CdTe, CdTe, or the like, or an In compound such as InP, InN, InAs or the like, and the shell surrounding the core is a Zn compound, May be similar to ZnS or ZnSe. For example, the nanocrystal may include CdSe / ZnS nanocrystals as shown in FIG. 1, or nanoparticles of InP / ZnS as another example.
According to the method for surface treatment of chemical resistance of quantum dots according to the present invention as described above, an inorganic shell coating can be easily and surely formed, the internal size of particles can be prevented from being affected, The thickness of the monolayer is less than 1 monolayer while having the nature of a buffer at the outermost point of the quantum dots, so that the luminescence is not affected by the formation of a very thin inorganic film.
For example, as shown in FIG. 2A, when the quantum dot is CdSe / ZnS, a ZnS crystal lattice grows on the CdSe crystal lattice. When the ZnS crystal lattice grows to a certain thickness, for example, 1.7 mL or more As shown in FIG. 2 (b), when the quantum dots are produced by a chemical treatment-imparted surface treatment method of a quantum dot according to the present invention, for example, CdSe / ZnS / CdS is formed on a CdSe crystal lattice The ZnS crystal lattice grows and Cd larger than Zn is introduced into the outermost part of the quantum dots, thereby preventing cracks due to the increase in the ZnS thickness. This can be regarded as the presence of Cd at the position where the crack occurs, and as a result, cracks disappear on the crystal lattice, thereby suppressing lattice mismatch, minimizing energy loss, and improving luminescence. In addition, the phenomenon that the chemical substance penetrates into the space formed at the time of cracking to reduce the luminescence property is prevented by suppressing the occurrence of cracks as described above. Also for this reason, high temperature heat resistance is improved in the presence of oxygen, and the probability of attacking an external chemical substance due to high-density ligand binding is reduced. Here, CdS is not a shell of sufficient thickness and therefore does not affect the quantum dot emission wavelength.
As shown in FIG. 3, the method for surface treatment of chemical resistance of a quantum dot according to an embodiment of the present invention is a method for treating a surface of a quantum dot by mixing quantum dots in a solution containing different kinds of metal ions, A step (S11) of allowing the metal ions to be exchanged on the surface, and a step (S12) of cooling the quantum dot mixed solution after the metal ions have been exchanged and then purifying the quantum dots with an organic solvent.
According to another embodiment of the present invention, there is provided a method for surface-treating a chemical resistance of a quantum dot, which comprises introducing CdO, a ligand and 1-octadecene (ODE) into a container, (ODE) of 10 to 2000 mL; dissolving the CdO in a vacuum state at a temperature of 100 to 300 DEG C; dissolving the CdO Introducing a quantum dot into a solution wherein the solution exchanges metal ions on the surface of the quantum dot at a temperature of 100 to 300 ° C; and cooling the solution to purify the quantum dots with an organic solvent have. Wherein the ligand is selected from the group consisting of an alkyl acid, an alkyl phosphonic acid, an alkyl phosphinic acid, an aryl phosphine, an aryl phosphine, And may include any one of aryl acid, aryl phosphonic acid, and aryl phosphinic acid. The structure and molecular weight of the material are not limited.
The quantum dot according to one embodiment of the present invention is a quantum dot produced by the method for surface treatment of chemical resistance of quantum dots according to the embodiments of the present invention as described above. And the description thereof will be omitted. Hereinafter, more specific examples will be described.
[Practical Example 1] Synthesis of Green Quantum Dot (QD)
Selenium and sulfur were dissolved in tri-n-octylphosphine to prepare a 1 M selenium solution (TOP-Se) and a 1 M sulfur (TOP-S) solution, both of which were chalcogenide standard solutions for red quantum dot synthesis. Then, 0.128 g (1.0 mmol) of cadmium oxide, 0.878 g (4.0 mmol) of zinc acetate, 6.34 mL (20.0 mmol) of oleic acid and 2.7 g (10 mmol) of cesium oxide were added to a 100 mL two neck round bottom flask ) Oleylamine, 10 mL of octadecin and heated to 180 DEG C until the solution became clear to obtain a metal precursor of cadmium oleate and zinc oleate. The water was then heated to 150 < 0 > C to remove the resulting water and degassed for 20 minutes. The temperature of the mixed solution was raised to 300 ° C, and 0.4 mL of a 1 M selenium solution (TOP-Se) and 3 mL of a 1 M sulfuric acid solution (TOP-S) were mixed at room temperature. In the subsequent growth step, the temperature was adjusted to 280 DEG C and the reaction was carried out for 10 minutes to obtain quantum dots.
[Practical Example 2] Synthesis of Yellow Quantum Dots (QD)
Se and S were dissolved in tri-n-octylphosphine to prepare 1M selenium solution (TOPSe) and 1M sulfur (TOPS) solution, which are standard solutions of chalcogenide for red quantum dot synthesis. Then add 0.128 g (1.0 mmol) of cadmium oxide, 0.634 mL (2.0 mmol) of oleic acid and 10 mL of octadecane to a 100 mL two neck round bottom flask and add 180 Lt; 0 > C to obtain a cadmium oleate metal precursor. The water was then heated in a vacuum to 150 DEG C to remove the generated water and degassed for 20 minutes. The temperature of the mixed solution was raised to 300 ° C and 2 mL of 1 M selenium solution (TOPSe) was injected. In the subsequent growth step, the temperature was adjusted to 280 ° C and the reaction was carried out for 12 minutes to obtain CdSe core quantum dots.
0.1 g of the above obtained CdSe Core QD is dissolved in 10 mL of ODE. The temperature of the reaction vessel was raised to 200 ° C under vacuum, and then the temperature was raised to 280 ° C after N 2 purging. Mix 1 mmol of Zinc stearate with 1 mL of TOP-S prepared above, and add 5 mL of TOP to dilute it (this is called a Zn-S precursor solution). Slowly drop the Zn-S precursor solution into the CdSe core QD / ODE solution using a syringe pump. After the reaction for 3 hours, the temperature of the reaction vessel is lowered to room temperature, EtOH is put into the vessel in an excessive amount, the quantum dots are precipitated, and the particles are recovered at 15,000 rpm using a centrifuge.
[Practical example 3] Red quantum dot (QD) synthesis
Se and S were dissolved in tri-n-octylphosphine to prepare a 1 M selenium solution (TOP-Se) and 1 M sulfur (TOP-S) solution, which are chalcogenide standard solutions for red quantum dot synthesis. Then, 0.128 g (1.0 mmol) of cadmium oxide, 0.878 g (4.0 mmol) of zinc acetate and 5.7 g (20.0 mmol) of stearic acid were added to a 100 mL two neck round bottom flask, 2.7 g (10 mmol) of oleylamine 10 mL of octadecine was added and heated to 180 ° C until the solution became clear to obtain a metal precursor of cadmium oleate and zinc oleate. The water was then heated to 150 < 0 > C to remove the resulting water and degassed for 20 minutes. The temperature of the mixed solution was raised to 300 ° C, 0.4 mL of 1 M selenium solution (TOP-Se) was injected, and 1 M sulfuric acid solution (TOP-S) was injected after 30 seconds. In the subsequent growth step, the temperature was adjusted to 280 DEG C and the reaction was carried out for 10 minutes to obtain quantum dots.
[Example 4] Synthesis of InP-ZnS
0.2 g of InCl 3 and 0.12 g of anhydrous ZnCl 2 are dissolved in olive oil (OLA), placed in a 100-mL 1-neck RBF and heated to 220 ° C. Then, the volatile material in the solution is removed by applying a medium intermediate vacuum, and the vessel is filled with nitrogen. Then dissolve 0.25 mL of Tris (dimethylamino) phosphine (P (DA) 3 ) in 1 mL of 1-octadecene. P (DA) 3 / ODE solution is injected into the In-Zn-OLA solution at 220 ° C and the temperature of the container is maintained at 220 ° C for 3 minutes. After 3 minutes, the vessel is separated from the heating mantle. When the temperature of the solution becomes 100 ° C or less, EtOH is poured to recover the InP-ZnS quantum dots. The recovered quantum dot emits green light.
[Example 5] High-speed cation exchange reaction
Prepare 100 mL 2-neck RBF, add 10 mmol of CdO and 22 mmol of oleic acid (OA) and fill with 50 mL of 1-octadecene (ODE). Then, while the vacuum is applied, raise the temperature of the solution to 200 ° C and maintain the condition for 12 hours to completely dissolve the CdO. 1 batch of the quantum dot prepared above (refined quantum dot) is filled, the temperature of the whole solution is raised to 220 ° C, and metal ion exchange existing on the surface is attempted at that temperature for 2 hours. Then, when the temperature of the solution drops to room temperature, the quantum dots are purified using excess EtOH.
[Example 6] Low rate cation exchange reaction
Prepare 100 mL 2-neck RBF, add 10 mmol of CdO and 21 mmol of stearic acid (SA), and fill with 50 mL of 1-octadecene (ODE). Then, while the vacuum is applied, raise the temperature of the solution to 200 ° C and maintain the condition for 12 hours to completely dissolve the CdO. 1 batch of the quantum dot prepared above (refined green quantum dot or InP-ZnS) is filled, the temperature of the whole solution is raised to 220 ° C, and the metal ion exchange existing on the surface is attempted at that temperature for 24 hours. Then, when the temperature of the solution drops to room temperature, the quantum dots are purified using excess EtOH.
The luminescence and chemical resistance of the quantum dot surface-treated by the above-described Example 3 and the quantum dot not subjected to the surface treatment were examined.
First, mercaptopropionic acid is dropped into a CHCl 3 solution in which a surface-treated quantum dot and a non-surface-treated quantum dot are dissolved according to the present invention. As a result, the luminescence of the quantum dots not subjected to the surface treatment was rapidly decreased, whereas the quantum dots subjected to the surface treatment according to the present invention did not greatly change the luminescence.
Also, in FIG. 4, as shown in FIG. 4 (a), the quantum dots not subjected to the surface treatment show low luminous properties, but the quantum dots surface-treated according to the present invention as shown in FIG. Here, before the surface treatment refers to a quantum dot raw solution obtained by synthesis, and after the surface treatment refers to a case of a quantum dot obtained through Cd-alkyl acid and having a surface metal substituted with Cd. It can be seen that the luminescence after the surface treatment is increased by 10% or more, while the under room light means that the under-room light is photographed by a camera under a fluorescent lamp.
According to the method for surface treatment of chemical resistance of quantum dots according to the present invention and the quantum dots produced by the method, an inorganic shell coating can be easily and stably applied to the surface of a quantum dots, So that it has excellent chemical resistance and heat resistance and an inorganic layer having a buffer nature formed at the outermost part of the quantum dots can have a thickness not affecting the luminescence.
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 and scope of the present 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 (7)
Octadecene (ODE) was added to the vessel so that the ligand was 5 to 100 mmol based on 10 mmol of CdO, and the 1-octadecene (ODE) was 10 To 2000 mL;
Dissolving the CdO in a vacuum state at a temperature of 100 to 300 < 0 >C;
Introducing a quantum dot into the solution in which the CdO is dissolved to exchange the metal ions of the surface of the quantum dot at a temperature of 100 to 300 ° C; And
And cooling the solution to purify the quantum dots with an organic solvent:
Of the surface of the quantum dot.
The material exchanged with the different kind of metal ions is,
The surface of the quantum dots is subjected to chemical resistance imparting treatment of the quantum dots, which is a material which has a larger atom or ion size than the metal ions on the surface of the quantum dots and forms a layer having a lower band gap, Way.
The material exchanged with the different kind of metal ions is,
Wherein the quantum dots include a part of Cd, Al, Ga (Gallium) and In (indium) when the outermost metal atom of the quantum dots is Zn.
The ligand,
Alkyl phosphonic acid, alkyl phosphinic acid, aryl acid, aryl phosphonic acid (which is capable of forming a metal salt by reacting with a metal), alkyl phosphonic acid, alkyl phosphinic acid, aryl acid, aryl phosphonic acid phosphonic acid, and aryl phosphinic acid. < Desc / Clms Page number 24 >
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| WO2021216941A3 (en) * | 2020-04-24 | 2021-12-02 | The Government Of The United States Of America, As Represented By The Secretary Of The Navy | Cu2-xs/pbs core/shell nanocrystals |
| US11603493B2 (en) | 2019-10-17 | 2023-03-14 | Samsung Electronics Co., Ltd. | Core shell quantum dot, production method thereof, and electronic device including the same |
| US11692136B2 (en) | 2019-10-17 | 2023-07-04 | Samsung Electronics Co., Ltd. | Core shell quantum dot, production method thereof, and electronic device including the same |
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| US10246638B1 (en) * | 2017-11-20 | 2019-04-02 | eLux, Inc. | Quantum dot light emitting diode (LED) with suppressed photobrightening |
| CN115181561A (en) * | 2021-04-02 | 2022-10-14 | 纳晶科技股份有限公司 | Nanocrystalline composition, preparation method and application thereof |
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| KR20130004739A (en) * | 2011-07-04 | 2013-01-14 | 홍익대학교 산학협력단 | Method of forming cis/zns core/shell quantum dots by solvothermal method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11603493B2 (en) | 2019-10-17 | 2023-03-14 | Samsung Electronics Co., Ltd. | Core shell quantum dot, production method thereof, and electronic device including the same |
| US11692136B2 (en) | 2019-10-17 | 2023-07-04 | Samsung Electronics Co., Ltd. | Core shell quantum dot, production method thereof, and electronic device including the same |
| US11987739B2 (en) | 2019-10-17 | 2024-05-21 | Samsung Electronics Co., Ltd. | Core shell quantum dot, production method thereof, and electronic device including the same |
| US11999887B2 (en) | 2019-10-17 | 2024-06-04 | Samsung Electronics Co., Ltd. | Core shell quantum dot, production method thereof, and electronic device including the same |
| WO2021216941A3 (en) * | 2020-04-24 | 2021-12-02 | The Government Of The United States Of America, As Represented By The Secretary Of The Navy | Cu2-xs/pbs core/shell nanocrystals |
| US11732186B2 (en) | 2020-04-24 | 2023-08-22 | The Government Of The United States Of America, As Represented By The Secretary Of The Navy | Core/shell nanocrystals with copper sulfide cores and lead sulfide shells |
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