CN111187610A - Composite quantum dot material, preparation method and display device thereof - Google Patents

Composite quantum dot material, preparation method and display device thereof Download PDF

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CN111187610A
CN111187610A CN201811529365.8A CN201811529365A CN111187610A CN 111187610 A CN111187610 A CN 111187610A CN 201811529365 A CN201811529365 A CN 201811529365A CN 111187610 A CN111187610 A CN 111187610A
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quantum dot
composite quantum
optical core
dot material
oxide
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李碧凤
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Shengsen Technology Co ltd
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Abstract

The invention provides a composite quantum dot material, which comprises the following components: an optical core; an inorganic ligand layer coated on a surface of the optical core, the inorganic ligand layer comprising at least one silicon oxide (SiOx) material; and a water oxygen barrier layer coated on the surface of the inorganic ligand layer; wherein, the water oxygen barrier layer is formed by stacking a laminated structure comprising at least one metal oxide in an irregular arrangement mode. In addition, a preparation method and application of the composite quantum dot material are also provided.

Description

Composite quantum dot material, preparation method and display device thereof
Technical Field
The present invention relates to a composite quantum dot material, a method for preparing the composite quantum dot material, and a display device using the composite quantum dot material, and more particularly, to a composite quantum dot material capable of improving the stability and the luminous efficiency of quantum dots, a method for preparing the composite quantum dot material, and a display device using the composite quantum dot material.
Background
Quantum dots have attracted considerable interest in the scientific and industrial fields due to their excellent optoelectronic properties since they have been fabricated. Compared with the traditional fluorescent material, the luminescent property of the quantum dot has the advantages of narrow half-peak width, small particles, no scattering loss, adjustable spectrum along with the size and the like, and is widely considered to have great application prospect in the fields of display, illumination, biological fluorescent labeling and the like.
A great deal of time and labor cost are invested in each unit to research the quantum dot material, so that the photoelectric performance of the quantum dot is continuously improved, and related applied elements appear successively.
Among them, application of quantum dots as a light emitting material to display devices is considered as an application field in which quantum dots first achieve a breakthrough. However, quantum dots as an excellent luminescent material still have many fundamental problems that have not been solved yet, and especially the stability problem of quantum dots is troubling many research units, which is one of the bottlenecks limiting the development of quantum dots field. Furthermore, the stability of quantum dots is also a great challenge in other application fields, such as solar cells, biomarkers, environmental pollution, and the like.
Disclosure of Invention
In view of the above-mentioned shortcomings in the prior art, the present invention is directed to a composite quantum dot material capable of improving the stability and the light emitting efficiency of quantum dots, a method for preparing the composite quantum dot material, and a display device using the composite quantum dot material.
Firstly, the invention provides a composite quantum dot material. The composite quantum dot material includes: an optical core; an inorganic ligand layer coated on the surface of the optical core, the inorganic ligand layer comprising at least one oxide of Silicon (SiO)x) A material; and a water oxygen barrier layer coated on the surface of the inorganic ligand layer. Wherein, the water oxygen barrier layer is formed by stacking a plurality of laminated structures comprising at least one metal oxide in an irregular arrangement mode.
Furthermore, the invention also provides a preparation method of the composite quantum dot material, which comprises the following steps: (A) providing an optical core and performing silanization treatment on the optical core; (B) adding a surfactant and a non-polar solvent to the silanized optical core; (C) adding a silicon-containing compound to make the surface of the optical core have at least one silicon oxide (SiO)x) A material; (D) adding an aqueous compound, wherein the aqueous compound and the silicon-containing compound are subjected to hydrolysis and condensation reaction to form an inorganic ligand layer; (E) mixing zinc acetate hydrate and ethanol and adding to the optical core coated with the inorganic ligand layer; and (F) soaking the optical core coated with the inorganic ligand layer in a sodium hydroxide (NaOH) -Ethanol (Ethanol) aqueous solution to form a composite quantum dot material.
The invention also provides another preparation method of the composite quantum dot material, which comprises the following steps: (G) providing an optical core and performing silanization treatment on the optical core; (H) adding a surfactant and a non-polar solvent to the silanized optical core; (I) adding a silicon-containing compound to make the surface of the optical core have at least one silicon oxide (SiO)x) A material; (J) adding an aqueous compound, said aqueous compound and saidThe silicon-containing compound is hydrolyzed and condensed to form an inorganic ligand layer; (K) adding Titanium isopropoxide (TTIP) or tetrabutyl titanate (TBOT) to the optical core coated with the inorganic ligand layer; and (L) soaking the optical core coated with the inorganic ligand layer in a water-alcohol solution to form a composite quantum dot material.
The invention also provides another preparation method of the composite quantum dot material, which comprises the following steps: (M) providing an optical core anchored to the inorganic oxide; (N) adding a non-polar solvent to the inorganic oxide containing at least one quantum dot; (O) adding a silicon-containing compound such that an inorganic ligand layer is formed on the surface of the optical core; (P) mixing zinc acetate monohydrate and ethanol and adding to the optical core coated with the inorganic ligand layer; and (Q) soaking the optical core coated with the inorganic ligand layer in a sodium hydroxide (NaOH) -Ethanol (Ethanol) aqueous solution to form a composite quantum dot material.
The invention also provides another preparation method of the composite quantum dot material, which comprises the following steps: (R) providing an optical core anchored to the inorganic oxide; (S) adding a nonpolar solvent to at least one quantum dot in the inorganic oxide; (T) adding a silicon-containing compound such that an inorganic ligand layer is formed on the surface of the optical core; (U) adding Titanium isopropoxide (TTIP) or tetrabutyl titanate (TBOT) to the optical core coated with the inorganic ligand layer; and (V) soaking the optical core coated with the inorganic ligand layer in a water-alcohol solution to form a composite quantum dot material.
Furthermore, the present invention further provides a composite quantum dot display device, comprising: a backlight source; at least one composite quantum dot material arranged on the backlight source; and a liquid crystal display module arranged on the backlight source containing at least one composite quantum dot material.
Wherein the at least one composite quantum dot material comprises: an optical core; an inorganic ligand layer coated on the surface of the optical core, the inorganic ligand layer comprising at least one oxide of Silicon (SiO)x) A material; andand the water oxygen barrier layer is coated on the surface of the inorganic ligand layer. Wherein, the water oxygen barrier layer is formed by stacking a laminated structure comprising at least one metal oxide.
The present invention further provides another composite quantum dot display device, including: the micro light-emitting source is an active micro LED crystal grain or a passive micro LED crystal grain; and at least one composite quantum dot material disposed on the micro-light-emitting source. Wherein the at least one composite quantum dot material comprises: an optical core; an inorganic ligand layer coated on the surface of the optical core, the inorganic ligand layer comprising at least one oxide of Silicon (SiO)x) A material; and a water oxygen barrier layer coated on the surface of the inorganic ligand layer. Wherein, the water oxygen barrier layer is formed by stacking a laminated structure comprising at least one metal oxide.
The foregoing summary of the invention is provided to introduce a basic description of several aspects and features of the present invention. This summary is not an extensive overview of the invention, and is intended to neither identify key or critical elements of the invention nor delineate the scope of the invention, but to present some concepts of the invention in a simplified form.
Drawings
FIG. 1 is a schematic diagram of a composite quantum dot material according to a preferred embodiment of the present invention;
FIG. 2 is a schematic diagram of a composite quantum dot material according to another preferred embodiment of the present invention;
fig. 3 is a flow chart of a method for preparing a composite quantum dot material according to a first preferred embodiment of the invention;
FIG. 4 is a flow chart of a method for preparing a composite quantum dot material according to a second preferred embodiment of the present invention;
fig. 5 is a flow chart of a method for preparing a composite quantum dot material according to a third preferred embodiment of the invention;
fig. 6 is a flow chart of a method for preparing a composite quantum dot material according to a fourth preferred embodiment of the invention;
FIG. 7A is an electrical representation of an inorganic ligand layer coating an optical core according to a preferred embodiment of the present invention;
FIG. 7B is an electrical representation of an inorganic ligand layer coating an optical core in accordance with a preferred embodiment of the present invention;
FIG. 7C is an electrical representation of an inorganic ligand layer coating an optical core in accordance with a preferred embodiment of the present invention;
FIG. 8A is an electron diagram of a composite quantum dot material with a water-oxygen barrier layer of titanium oxide according to a preferred embodiment of the present invention;
FIG. 8B is a diagram of a gold phase diagram of a composite quantum dot material with a water-oxygen barrier layer of titanium oxide according to a preferred embodiment of the present invention;
FIG. 8C is a diagram of a gold phase diagram of the water oxygen barrier layer of the composite quantum dot material of the preferred embodiment of the present invention being titanium oxide;
FIG. 9A is an electron diagram of a composite quantum dot material with zinc oxide as the water-oxygen barrier layer according to the preferred embodiment of the invention;
FIG. 9B is a diagram of a gold phase diagram of a zinc oxide barrier layer of the composite quantum dot material according to the preferred embodiment of the invention;
FIG. 9C is a diagram of a gold phase diagram of a zinc oxide barrier layer of the composite quantum dot material according to the preferred embodiment of the invention;
FIG. 10A is an electrical schematic of a composite quantum dot material according to another preferred embodiment of the present invention;
FIG. 10B is an electrical schematic diagram of a composite quantum dot material according to another preferred embodiment of the present invention;
FIG. 10C is an electrical schematic diagram of a composite quantum dot material according to another preferred embodiment of the present invention;
fig. 11 is a schematic view of a composite quantum dot light emitting diode (QD-LED) package structure according to a first embodiment of the present invention;
FIG. 12 is a schematic diagram of a composite quantum dot light emitting diode (QD-LED) package structure according to a second embodiment of the present invention;
fig. 13 is a schematic view of a composite quantum dot light emitting diode (QD-LED) package structure according to a third embodiment of the present invention;
FIG. 14 is a schematic view of a composite quantum dot LCD device according to an embodiment of the present invention;
FIG. 15A is a schematic view of a composite quantum dot LCD device according to another embodiment of the present invention;
FIG. 15B is a schematic view of a composite quantum dot LCD device according to still another embodiment of the present invention;
FIG. 16 is a schematic view of a composite quantum dot Micro light emitting diode (Micro LED) display device according to a first embodiment of the present invention;
FIG. 17 is a schematic view of a composite quantum dot Micro light emitting diode (Micro LED) display device according to a second embodiment of the present invention;
FIG. 18 is a schematic view of a composite quantum dot Micro light emitting diode (Micro LED) display device according to a third embodiment of the present invention;
FIG. 19 is a temperature test chart of the composite quantum dot material according to the preferred embodiment of the invention;
FIG. 20 is a water and oxygen blocking test chart of the composite quantum dot material according to the preferred embodiment of the present invention;
FIG. 21 is a water and oxygen blocking test chart of the composite quantum dot material according to the preferred embodiment of the invention;
fig. 22 is a comparison diagram of the color gamut of the composite quantum dot display device according to the preferred embodiment of the invention.
The reference numbers illustrate:
142. 142a, 142b, 142' … composite quantum dot material
421. 421a, 421b, 421c … optical core
431 … quantitative precursor
1001. 1001a, 1001b, 1001c … inorganic compound layer
2001 … Water oxygen Barrier layer
201 … laminated structure
52. 54 … Quantum dot liquid crystal display device
42 … liquid crystal display module
420 … glass substrate
422 … liquid crystal molecule layer
424 … thin-film transistor layer
32 … side light type backlight module
34 … direct type backlight module
320 … light guide plate
322 … reflective sheet
380 … frame
100 … backlight
100a, 100b, 100c … quantum dot light emitting diode
120 … base plate
122 … metal electrode
130 … light emitting diode chip
140 … wavelength converting film
144 … A photoresist layer
146 … composite photoresist layer
150 … barrier layer
151 … oxidized metal layer
160 … protective layer
170 … transparent colloid material
180 … Plastic electrode chip Carrier
190 … metal wire
200a, 200b, 200c … quantum dot micro LED display device
220 … LED chip
222 … first electrode
224 … second electrode
226 … light emitting layer
240 … micro-luminous source
260 … spacer layer
Detailed Description
Example (b): composite quantum dot material
First, please refer to fig. 1, which is a schematic diagram of a composite quantum dot material according to a preferred embodiment of the invention. As shown in fig. 1, the composite quantum dot material 142 of the preferred embodiment includes: an optical core 421, an inorganic compound layer 1001, and a water-oxygen barrier layer 2001.
Wherein the optical core 421 may be a quantum dot made of a semiconductor material, such as: group II-VI quantum dots (CdSe or CdS), group III-V quantum dots ((Al, In, Ga) P, (Al, In, Ga) As or (Al, In, Ga) N), group II-VI quantum dots having a shell-core structure (CdSe/ZnS), group III-V quantum dots having a shell-core structure (InP/ZnS), non-spherical group II-VI quantum dots having an alloy structure (ZnCdSeS), a combination of any two or more of the above.
The optical core 421 may also be a material having the chemical formula MAX3The perovskite quantum dot of (a), the perovskite quantum dot mainly comprises an organic-inorganic hybrid perovskite quantum dot, an all-inorganic perovskite quantum dot or a combination thereof. Wherein the cation M is organic methylamine ion, ethylamine ion, formamidine ion or inorganic cesium ion (Cs)+) (ii) a The metal ion A is divalent lead ion (Pb)2+) Tin (Sn)2+) Or germanium ion (Ge)2+) (ii) a The halide ion X is a chloride ion (Cl) belonging to a cubic, orthorhombic or tetragonal system-) Bromine ion (Br)-) Or iodide ion (I)-)。
Further, the all-inorganic perovskite quantum dot has a chemical general formula CsPbCl3Blue light all-inorganic perovskite quantum dot and CsPbBr3The green light all-inorganic perovskite quantum dot has a chemical general formula CsPb (I/Br)3The amber light all-inorganic perovskite quantum dot, the red light all-inorganic perovskite quantum dot with the chemical general formula CsPbI3 or the combination thereof. The composite quantum dot material 142 of the preferred embodiment can be excited by the first light to emit the second light with a wavelength different from that of the first light, and has excellent quantum efficiency and light wavelength conversion efficiency, and can exhibit a narrow-half-width light emission spectrum and excellent color purity, so that the light wavelength conversion effect is good, and the application thereof to a light emitting device can improve the light emitting efficiency thereof.
The quantum dots can be flexibly applied by changing the light emitting color (second light wavelength) according to the difference of the energy Band width (Band Gap) through the adjustment of the components and/or the sizes, such as the color gamut from blue, green to red; wherein, the quantum dots have nanometer size. In the preferred embodiment, the optical core 421 has a particle size of between 1 nanometer (nm) and 30 nm (e.g., 20 nm). However, the user may first determine the color of the photoluminescence of the optical core 421 and then determine the appropriate size of the optical core 421 according to the selected semiconductor material, which should not be construed as a limitation of the present invention.
Wherein the inorganic ligand layer 1001 is coated on the surface of the optical core 421, and the inorganic ligand layer 1001 comprisesAt least one oxide of Silicon (SiO)x) A material. In the preferred embodiment, the silicon oxide (SiO)x) The thickness of the material is between 1 nanometer (nm) and 1000 nm, such as 10 nm to 100 nm. Wherein the oxide of Silicon (SiO)x) The material may be silicon dioxide (SiO)2) Or silicon monoxide (SiO). Notably, silicon dioxide (SiO)2) The light transmittance of the quantum dot is high, the light extraction efficiency from at least one quantum dot is not reduced, the loss of a Ligand (Ligand) of the quantum dot can be reduced, the quantum efficiency is improved, and the photo-oxidation of the quantum dot can be prevented.
In addition, in the preferred embodiment, a water oxygen barrier layer 2001 is further coated on the surface of the inorganic ligand layer 1001, and the water oxygen barrier layer 2001 is formed by stacking the laminated structures 201 including at least one metal oxide in an irregular arrangement manner, so as to effectively reduce the influence of the inorganic ligand layer 1001, which may cause poor dispersion of the nano-structure of the quantum dot (optical core 421) in the cured polymer material. Wherein the at least one metal oxide is titanium oxide (TiO)2) Zinc oxide (ZnO), aluminum oxide (AlO)x) Or a combination thereof.
On the other hand, please refer to fig. 2, which is a schematic diagram of a composite quantum dot material according to another preferred embodiment of the invention. As shown in fig. 2, the composite quantum dot material 142' of the present another preferred embodiment includes: a quantity of precursor 431, an optical core 421, an inorganic ligand layer 1001, and a water oxygen barrier layer 2001.
The difference between the present embodiment and the composite quantum dot material 142 of fig. 1 is that the composite quantum dot material 142' of the present embodiment further includes a quantitative precursor 431, and the quantitative precursor 431 is an inorganic oxide, and in a possible implementation, the inorganic oxide may be a nano-sphere structure, and the material thereof may be at least one inorganic oxide, such as silicon dioxide (SiO) (i.e., SiO oxide)2) Silicon monoxide (SiO), or a combination thereof. In addition, please refer to FIG. 10A (scale size 15 nm), FIG. 10B (scale size 20 nm) and FIG. 10C (scale size 50 nm) at the same time, which are another preferred embodiment of the present invention (containing quantitative precursor)) An electrogram of the composite quantum dot material of (1). As shown in fig. 10A, 10B and 10C, an amination step is first performed on the quantitative precursor 431; upon completion, the optical core 421 may be anchored and grown on the dosing precursor 431, while the inorganic ligand layer 1001 is coated on the surfaces of the dosing precursor 431 and the optical core 421. Finally, the water oxygen barrier layer 2001 is further coated on the surface of the inorganic compound layer 1001 core to form the composite quantum dot material 142' of the present embodiment.
Example (b): preparation method of composite quantum dot material
Please refer to fig. 3, which is a flowchart illustrating a method for fabricating a composite quantum dot material according to a first preferred embodiment of the invention. As shown in fig. 3, the composite quantum dot material of the present invention can be prepared by the following steps: (A) providing an optical core and performing silanization treatment on the optical core; (B) adding a surfactant and a non-polar solvent to the silanized optical core; (C) adding a silicon-containing compound to make the surface of the optical core have at least one silicon oxide (SiO)x) A material; (D) adding an aqueous compound, wherein the aqueous compound and the silicon-containing compound are subjected to hydrolysis and condensation reaction to form an inorganic ligand layer; (E) mixing zinc acetate hydrate and ethanol and adding to the optical core coated with the inorganic ligand layer; and (F) soaking the optical core coated with the inorganic ligand layer in a sodium hydroxide (NaOH) -Ethanol (Ethanol) aqueous solution to form a composite quantum dot material.
In step (a) of the present embodiment, the optical core may be a quantum dot made of a semiconductor material, for example: group II-VI quantum dots (CdSe or CdS), group III-V quantum dots ((Al, In, Ga) P, (Al, In, Ga) As or (Al, In, Ga) N), group II-VI quantum dots having a shell-core structure (CdSe/ZnS), group III-V quantum dots having a shell-core structure (InP/ZnS), non-spherical group II-VI quantum dots having an alloy structure (ZnCdSeS), a combination of any two or more of the above.
The optical core may also be of the general chemical formula MAX3The perovskite quantum dot of (1), the perovskiteThe mineral quantum dots mainly comprise organic-inorganic hybrid perovskite quantum dots, all-inorganic perovskite quantum dots or a combination thereof. Wherein the cation M is organic methylamine ion, ethylamine ion, formamidine ion or inorganic cesium ion (Cs)+) (ii) a The metal ion A is divalent lead ion (Pb)2+) Tin (Sn)2+) Or germanium ions (Ge2 +); the halide ion X is a chloride ion (Cl) belonging to a cubic, orthorhombic or tetragonal system-) Bromine ion (Br)-) Or iodide ion (I)-). Further, the all-inorganic perovskite quantum dot has a chemical general formula CsPbCl3The blue light all-inorganic perovskite quantum dot has a chemical general formula CsPbBr3The green light all-inorganic perovskite quantum dot has a chemical general formula CsPb (I/Br)3The amber light all-inorganic perovskite quantum dot has a chemical general formula CsPbI3Or a combination thereof.
In step (B) of this example, the surfactant was Triton X-100(Triton X-100, C14H22O (C2H4O) n) or nonylphenol polyether-5 (Igepal CO-520); the non-polar solvent is Hexane (Hexane), Cyclohexane (Cyclohexane), Benzene (Benzene), Toluene (Toluene), Chloroform (Chloroform) or ethyl acetate (Ethylacetate).
In step (C) of this example, the silicon-containing compound is Tetraethylsilicate (TEOS), Tetramethylsilicate (TMOS), or 3-Aminopropyltriethoxysilane (APTES). Oxide of Silicon (SiO)x) The material may be silicon dioxide (SiO)2) Silicon monoxide (SiO), or a combination thereof.
In step (D) of this example, the aqueous compound was pure water (H)2O) or ammonia (NH)4OH) solution.
Referring to fig. 7A and 7B, which are electron micrographs (with a scale size of 20 nm) of an optical core coated with an inorganic ligand layer according to a preferred embodiment of the present invention, the preparation of the optical core 421a coated with the inorganic ligand layer 1001a can be completed through the steps (a) to (D) of the above-mentioned preparation method. First, as shown in fig. 7A, the scale size is 20 nm, it is evident from the figure that the size of the optical core 421a of the composite quantum dot material is about 5 nm, the thickness of the inorganic compound layer 1001a is about 3 nm, and the inorganic compound layer 1001a of the composite quantum dot material is coated with the single optical core 421 a; furthermore, as shown in fig. 7B, the scale size is also 20 nm, it is evident from the figure that the size of the optical core 421B of the composite quantum dot material is about 7 nm, the thickness of the inorganic compound layer 1001B is about 11.5 nm, and the inorganic compound layer 100B of the composite quantum dot material is also coated with the single optical core 421B. Therefore, the thickness of the inorganic ligand layer covering the optical core can be controlled by adjusting the concentrations of the solvents or compounds in the steps (A) to (D). In addition, referring to fig. 7C, which is an electrical diagram of the optical core coated by the inorganic ligand layer according to the preferred embodiment of the invention (with a scale size of 50 nm), the difference between fig. 7C and fig. 7A and 7B is that the inorganic ligand layer 1001C of the composite quantum dot material in fig. 7C can simultaneously coat multiple optical cores 421C.
Referring to fig. 8A, it is an electrical diagram of the water oxygen barrier layer of the composite quantum dot material of the preferred embodiment of the invention being titanium oxide. The composite quantum dot material 142a manufactured by the above manufacturing method includes: an optical core, an inorganic compound layer coated on the surface of the optical core, and a water-oxygen barrier layer coated on the surface of the inorganic compound layer, wherein the water-oxygen barrier layer is formed by stacking a laminated structure including at least one metal oxide in an irregular arrangement (refer to fig. 8A, the scale size is 100 nm). Wherein the optical core is quantum dot made of the semiconductor material or has a chemical general formula MAX3The perovskite quantum dots of (a); the inorganic ligand layer is silicon dioxide (SiO)2) Silicon monoxide (SiO), or a combination thereof; the at least one metal oxide is titanium oxide (TiO)2). Fig. 8B and 8C are gold phase diagrams of the composite quantum dot material with titanium oxide as the water-oxygen barrier layer, in which the fluorescent yellow portion in fig. 8B is a material containing silicon (Si) in the composite quantum dot material (with a scale of 15 nm), and the fluorescent green portion in fig. 8C is a material containing titanium (Ti) in the composite quantum dot material (with a scale of 15 nm).
In addition, please refer to fig. 4, which is a flowchart illustrating a method for manufacturing a composite quantum dot material according to a second preferred embodiment of the invention. As shown in fig. 4, the composite quantum dot material of the present invention can also be prepared by: (G) providing an optical core and performing silanization treatment on the optical core; (H) adding a surfactant and a non-polar solvent to the silanized optical core; (I) adding a silicon-containing compound to make the surface of the optical core have at least one silicon oxide (SiO)x) A material; (J) adding an aqueous compound, wherein the aqueous compound and the silicon-containing compound are subjected to hydrolysis and condensation reaction to form an inorganic ligand layer; (K) adding Titanium isopropoxide (TTIP) or tetrabutyl titanate (TBOT) to the optical core coated with the inorganic ligand layer; and (L) soaking the optical core coated with the inorganic ligand layer in a water-alcohol solution to form a composite quantum dot material.
In step (G) of the present embodiment, the optical core may be a quantum dot made of a semiconductor material, for example: group II-VI quantum dots (CdSe or CdS), group III-V quantum dots ((Al, In, Ga) P, (Al, In, Ga) As or (Al, In, Ga) N), group II-VI quantum dots having a shell-core structure (CdSe/ZnS), group III-V quantum dots having a shell-core structure (InP/ZnS), non-spherical group II-VI quantum dots having an alloy structure (ZnCdSeS), a combination of any two or more of the above.
The optical core may also be of the general chemical formula MAX3The perovskite quantum dot of (a), the perovskite quantum dot mainly comprises an organic-inorganic hybrid perovskite quantum dot, an all-inorganic perovskite quantum dot or a combination thereof. Wherein the cation M is organic methylamine ion, ethylamine ion, formamidine ion or inorganic cesium ion (Cs)+) (ii) a The metal ion A is divalent lead ion (Pb)2+) Tin (Sn)2+) Or germanium ion (Ge)2+) (ii) a The halide ion X is a chloride ion (Cl) belonging to a cubic, orthorhombic or tetragonal system-) Bromine ion (Br)-) Or iodide ion (I)-). Further, the all-inorganic perovskite quantum dot has a chemical general formula CsPbCl3The blue light all-inorganic perovskite quantum dot has a chemical general formula CsPbBr3The green light all-inorganic perovskite quantum dot has a chemical general formula CsPb (I/Br)3The amber light all-inorganic perovskite quantum dot, the red light all-inorganic perovskite quantum dot with the chemical general formula CsPbI3 or the combination thereof.
In step (H) of this example, the surfactant was Triton X-100(Triton X-100, C14H22O (C2H4O) n) or nonylphenol polyether-5 (Igepal CO-520); the non-polar solvent is Hexane (Hexane), Cyclohexane (Cyclohexane), Benzene (Benzene), Toluene (Toluene), Chloroform (Chloroform) or ethyl acetate (Ethylacetate).
In step (I) of this example, the silicon-containing compound is Tetraethylsilicate (TEOS), Tetramethylsilicate (TMOS), or 3-Aminopropyltriethoxysilane (APTES). Oxide of Silicon (SiO)x) The material may be silicon dioxide (SiO)2) Silicon monoxide (SiO), or a combination thereof.
In step (J) of this example, the aqueous compound was pure water (H)2O) or ammonia (NH)4OH) solution.
Referring to fig. 9A, it is an electron micrograph (with a scale size of 100 nm) of zinc oxide as the water oxygen barrier layer of the composite quantum dot material according to the preferred embodiment of the invention. The composite quantum dot material 142b manufactured by the above manufacturing method includes: an optical core, an inorganic compound layer coated on the surface of the optical core, and a water-oxygen barrier layer coated on the surface of the inorganic compound layer, wherein the water-oxygen barrier layer is formed by stacking a laminated structure including at least one metal oxide in an irregular arrangement (refer to fig. 9A, the scale size is 100 nm). Wherein the optical core is quantum dot made of the semiconductor material or has a chemical general formula MAX3The perovskite quantum dots of (a); the inorganic ligand layer is silicon dioxide (SiO)2) Silicon monoxide (SiO), or a combination thereof; the at least one metal oxide is zinc oxide (ZnO). In addition, fig. 9B and 9C are gold phase diagrams of zinc oxide as the water oxygen barrier layer of the composite quantum dot material according to the preferred embodiment of the invention, wherein the fluorescent blue in fig. 9BThe color portion is a material containing silicon (Si) in the composite quantum dot material (the scale size is 250 nm), and the fluorescent yellow portion in fig. 9C is a material containing zinc (Zn) in the composite quantum dot material (the scale size is 250 nm).
Finally, the preparation method of the composite quantum dot material containing quantitative precursor is as follows. First, please refer to fig. 5, which is a flowchart illustrating a method for preparing a composite quantum dot material (containing a quantitative precursor) according to a third preferred embodiment of the invention. As shown in fig. 5, the preparation method comprises the steps of: (a) providing an optical core anchored to an inorganic oxide, and in possible implementations, the inorganic oxide can be a nanosphere structure; (b) adding a nonpolar solvent to at least one quantum dot grown on the inorganic oxide; (c) adding a silicon-containing compound to make the surface of the optical core have at least one silicon oxide (SiO)x) A material; and (d) forming an oxide (SiO) externally coated with the at least one siliconx) The material is a composite quantum dot material.
Wherein the surfactant is Triton X-100(Triton X-100, C14H22O (C2H4O) n) or nonylphenol polyether-5 (Igepal CO-520). Wherein the silicon-containing compound is tetraethyl silicate (TEOS), tetramethyl silicate (TMOS) or 3-Aminopropyltriethoxysilane (APTES).
In addition, referring to fig. 6, it is a flow chart of a method for preparing a composite quantum dot material (containing quantitative precursors) according to a fourth preferred embodiment of the invention. As shown in fig. 6, the preparation method comprises the steps of: (a') providing at least one amount of precursor, and performing an amination treatment on the at least one amount of precursor, wherein the at least one amount of precursor is an inorganic oxide, and the inorganic oxide is a nano-sphere structure; (b') providing at least one optical core; (c') adding a surfactant or a non-polar solvent such that the at least one optical core is formed on the surface of the at least one volume of precursor; (d') adding a silicon-containing compound such that the surface of the optical core has at least one silicon oxide (SiO)x) A material; and (e') forming an oxide (SiO) externally coated with the at least one siliconx) Material oneAnd (3) compounding the quantum dot material.
The amination treatment is a chemical unit process for introducing an amino group into an organic compound molecule, the amination not only can introduce one amino group into the organic compound, but also can replace two or three amino groups, and the amination treatment method mainly comprises two steps: reducing, namely reducing the compound containing the nitro; and aminolysis, in which an organic halide is directly reacted with ammonia to replace a halogen atom with an amine group. Wherein the surfactant is Triton X-100(Triton X-100, C14H22O (C2H4O) n) or nonylphenol polyether-5 (Igepal CO-520). Wherein the silicon-containing compound is tetraethyl silicate (TEOS), tetramethyl silicate (TMOS) or 3-Aminopropyltriethoxysilane (APTES).
The composite quantum dot material containing quantitative precursor prepared by the above method can refer to the electrical diagrams of fig. 10A, 10B and 10C.
Example (b): display device of composite quantum dot material
The composite quantum dot material can be applied to various light-emitting devices such as lighting lamps, light-emitting modules (front light modules and backlight modules) of display devices such as mobile phone screens and television screens, or panel pixels or sub-pixels of the display devices. Furthermore, when using a plurality of composite quantum dot materials with different compositions, i.e. a plurality of quantum dots with different light-emitting wavelengths, the emission spectrum of the light source is wider, and even the full spectrum (full spectrum) requirement can be achieved. Therefore, the composite quantum dot material can improve the color gamut of the display device and can also effectively improve the color purity and the color authenticity of the display device.
First, please refer to fig. 11, which is a schematic diagram of a composite quantum dot light emitting diode (QD-LED) package structure according to a first embodiment of the present invention. As shown in fig. 11, the composite quantum dot light emitting diode 100a is in a chip package form, and includes a substrate 120, a metal electrode 122, a light emitting diode chip 130, a wavelength conversion film 140, and a barrier layer 150(barrier layer), and both sides of the metal electrode 122, the light emitting diode chip 130, the wavelength conversion film 140, and the barrier layer 150(barrier layer) may be further respectively provided with a protective layer 160 made of a silicon-containing material (e.g., Silicone resin) for blocking permeation of moisture and oxygen. Wherein the barrier layer 150(barrier layer) is preferably selected from the group consisting of glass and silica gel; among them, glass is the most preferable. The periphery of the integrated composite quantum dot light emitting diode 100a can be further coated with a metal oxide layer 151 by using an atomic layer deposition system (ALD), and the metal oxide layer 151 can be made of an atomic-scale aluminum oxide material.
The composite quantum dot light emitting diode 100a is disposed at the bottom of the substrate 120. The metal electrode 122 is disposed above the substrate 120. The led chip 130 is disposed above the metal electrode 122 and electrically connected to the metal electrode 122. The wavelength conversion film 140 and the barrier layer 150(barrierlayer) are both disposed on the led chip 130, and the barrier layer 150 covers the wavelength conversion film 140, so as to prevent the wavelength conversion film 140 from being affected by heat energy generated when the led chip 130 emits light, and even damage the wavelength conversion film 140. The material of the barrier layer 150 is polymethyl methacrylate (PMMA), optical glass, plastic epoxy, Silicone resin (Silicone resin), or the like.
The wavelength conversion film 140 is a wavelength conversion film 140 having the composite quantum dot materials 142 and 142 '(please refer to fig. 1 or fig. 2), and the wavelength conversion film 140 may also be a composite wavelength conversion film 140 formed by mixing the composite quantum dot materials 142 and 142' with a transparent colloid material (not shown), where the transparent colloid material may be polymethyl methacrylate (PMMA), polyethylene terephthalate (PET), Polystyrene (PS), polyethylene (PP), nylon (PA), Polycarbonate (PC), epoxy resin (epoxy), Silicone resin (Silicone resin), Silicone rubber (Silicone), or a combination thereof.
The composite wavelength conversion film 140 may further include other fluorescent materials (not shown), such as inorganic fluorescent materials or organic fluorescent materials mixed with the quantum dot materials 142 and 142', and inorganic fluorescent materials, such as aluminate fluorescent powder (e.g., LuYAG, GaYAG, YAG, etc.), silicate fluorescent powder, sulfide fluorescent powder, nitride fluorescent powder, fluoride fluorescent powder, potassium fluosilicate (KSF) containing tetravalent manganese ions, and the like. The organic fluorescent material includes a single molecular structure, a multi-molecular structure, an Oligomer (Oligomer), and a Polymer (Polymer). The fluorescent material consists of a main crystal, a co-activator (a sensitizer) and an activator. The fluorescent material can be yellow, blue, green, orange, red or a combination thereof, such as yellow-orange and red-yellow nitride fluorescent powder, and the material of the fluorescent material is selected from organic fluorescent powder, fluorescent pigment, inorganic fluorescent powder, radioactive elements or a combination thereof.
In this embodiment, the method for manufacturing the wavelength conversion film 140 is as follows: firstly, step (a) is performed, and the composite quantum dot material is dispersed through a polar or non-polar solvent. And (B) uniformly mixing the dispersion liquid containing the composite quantum dot material and the transparent adhesive material, and placing the mixture in an oven for drying to form the composite quantum dot adhesive material. And (C) coating the composite quantum dot adhesive material on the transparent substrate by a doctor blade coating method or infiltrating the composite quantum dot adhesive material into the gap between the two transparent substrates by an infiltration method. And finally, executing the step (D), and carrying out glue material UV curing or thermosetting molding to finish the manufacture of the wavelength conversion film 140.
In this embodiment, another manufacturing method of the wavelength conversion film 140 is as follows: first, step (a) is performed to stack a plurality of nanospheres into a periodic or non-periodic stack structure. And (b) infiltrating a framework colloid into gaps of the stack structure, wherein the framework colloid is mixed with the composite quantum dot material. And (c) curing the skeleton colloid, and removing the plurality of nanospheres in the stack structure by using a depilling agent. Finally, step (d) is performed to complete the wavelength conversion film 140, wherein the wavelength conversion film 140 includes a periodic or aperiodic nano-spherical hole structure.
After step (d) is performed, if there is a need to increase the light intensity for more wavelength spectrum, step (e) may be performed, and the nano-spherical hole structure in the wavelength conversion film 140 is infiltrated with the composite quantum dot material.
The manufacturing method of the wavelength conversion film can also be realized through the following method: first, step (f) is performed to make a plurality of the composite quantum dot materials in a periodic or non-periodic stack structure. And (g) infiltrating a framework colloid into the gaps of the stack structure. And (h) executing the step (h) to solidify the framework colloid. Finally, step (i) is performed to complete the wavelength conversion film 140, which includes a plurality of composite quantum dot materials with periodicity or aperiodicity.
In another embodiment, the composite wavelength conversion film 140 is fabricated as follows: first, step (a1) is performed to stack a plurality of nanospheres into a periodic or non-periodic stack structure. Next, step (b1) is performed, a skeleton colloid is infiltrated into the gaps of the stack structure, and the skeleton colloid is mixed with the composite quantum dot material, the fluorescent material, the transparent colloid material, or the combination thereof. Then, step (c1) is performed to solidify the skeleton colloid and remove the plurality of nanospheres in the stack structure with a depilling agent. Finally, step (d1) is performed to complete the composite wavelength conversion film 140, wherein the composite wavelength conversion film 140 includes a periodic or aperiodic nano-spherical hole structure.
After step (d1) is performed, if there is a need to increase the light intensity for more wavelength spectrum, step (e1) can be performed, in which the nano-spherical hole structure in the composite wavelength conversion film 140 is infiltrated with the composite quantum dot material.
In the above two embodiments, the nano-spheres can be silicon dioxide (SiO)2) Polystyrene (PS), Polydimethylsiloxane (Polydimethylsiloxane), and polymethyl methacrylate (Polymethylmethacrylate) to form nanospheres having a diameter of 10 nm to 1000 nm.
The liquid skeleton colloid can be light-cured glue or heat-cured glue of mixed fluorescent materials, or pure light-cured glue or heat-cured glue. Still further, the material of the light-curable adhesive includes acrylate monomer, acrylate oligomer monomer, or a combination thereof. This embodiment is implemented using an acrylate monomer. The acrylate monomer may be selected from Tripropylene glycol diacrylate (TPGDA), neopentyl glycol diacrylate (NPGDA), Propoxylated neopentyl glycol diacrylate (PO-NPGDA), trimethylolpropane triacrylate (TMPTA), Ethoxylated trimethylolpropane triacrylate (EO-TMPTA), Propoxylated trimethylolpropane triacrylate (PO-TMPTA), Propoxylated glycerol triacrylate (Propoxylated glycerol triacrylate, TPPTA), pentaerythritol tetraacrylate (ethylene glycol diacrylate, pentaerythritol tetraacrylate), pentaerythritol tetraacrylate (ethylene glycol diacrylate, pentaerythritol tetraacrylate, pentaerythritol, and the acrylate (pentaerythritol) may be used as a pigment, a, Dipentaerythritol hexaacrylate (DPHA) or combinations thereof.
The mode of solidifying the framework colloid is different according to the type of the framework colloid. If the skeleton colloid is a photo-curing adhesive containing a photo-curing agent, external environmental factors such as ultraviolet rays and the like are applied for curing; otherwise, if the adhesive is a thermosetting adhesive, the adhesive is cured by heating in an oven, for example.
When the material of the plurality of nano-spheres is silicon compound, the de-sphering agent is hydrofluoric acid (HF). The plurality of nanospheres in the stacked structure can be removed without corroding the framework colloid. When the plurality of nano-spheres are high molecular polymers, the sphere removing agent is an organic solvent to achieve the purpose.
In this embodiment, the steps of the led chip 130 process can be divided into an upstream, a midstream and a downstream, where the upstream includes forming a substrate (e.g., sapphire substrate, ceramic substrate, metal substrate, etc.), a single crystal rod (e.g., GaN, GaAs, GaP, etc.), a single crystal wafer, a structural design, and an epitaxial chip, the midstream includes metal evaporation, photo etching, thermal processing, and dicing, and the downstream packaging includes Flip-chip (Flip-chip), Surface Mount Device (SMD), and chip package (CSP).
In this embodiment, the wavelength conversion film 140 of the composite quantum dot light emitting diode 100a and the composite quantum dot materials 142 and 142' included in the composite wavelength conversion film 140 can be excited by the first light emitted from the light emitting diode chip 130 to emit the second light with a wavelength different from that of the first light, and have excellent quantum efficiency, and can exhibit a half-width-at-half-maximum emission spectrum and excellent color purity, so that the light wavelength conversion effect is excellent, and the light emission effect can be improved when applied to a backlight. The led chip 130 emitting the first light is emitted by a blue led chip or an ultraviolet led chip.
Please refer to fig. 12, which is a schematic diagram of a composite quantum dot light emitting diode (QD-LED) package structure according to a second embodiment of the present invention. As shown in fig. 12, the plastic electrode chip carrier 180 (connected by metal wires 190) of the composite quantum dot led 100b is provided with an led chip 130. And form a cup-shaped structure by surrounding the protection layer 160 to block the penetration of moisture and oxygen; and a transparent gel material 170 is filled therein. The transparent colloidal material 170 may be Polymethylmethacrylate (PMMA), Polyethyleneterephthalate (PET), Polystyrene (PS), polyethylene (PP), nylon (PA), Polycarbonate (PC), epoxy resin (epoxy), silicone resin (silicone), silicone (silicone), or a combination thereof. In the embodiment of fig. 12, the transparent colloid material 170 is Silicone resin (Silicone resin); and a wavelength conversion film 140 or a composite wavelength conversion film 140 sandwiched by the barrier layer 150 is disposed on the protective layer 160 and the transparent colloid material 170. The periphery of the integrated composite quantum dot light emitting diode 100a can be further coated with a metal oxide layer 151 by using an atomic layer deposition system (ALD), and the metal oxide layer 151 can be made of an atomic-scale aluminum oxide material.
Please refer to fig. 13, which is a schematic diagram of a composite quantum dot light emitting diode (QD-LED) package structure according to a third embodiment of the present invention. As shown in fig. 13, the plastic electrode chip carrier 180 of the composite quantum dot light emitting diode 100c is provided with a light emitting diode chip 130 (connected through a metal wire 190). And form a cup-shaped structure by surrounding the protection layer 160 to block the penetration of moisture and oxygen; and filled with a transparent colloidal material 170 mixed with the composite quantum dot material 142, 142'. The transparent colloid material 170 may be Polymethylmethacrylate (PMMA), polyethylene terephthalate (PET), Polystyrene (PS), polyethylene (PP), nylon (PA), Polycarbonate (PC), epoxy resin (epoxy), Silicone resin (Silicone resin), Silicone (Silicone), or a combination thereof. The periphery of the integrated composite quantum dot light emitting diode 100a can be further coated with a metal oxide layer 151 by using an atomic layer deposition system (ALD), and the metal oxide layer 151 can be made of an atomic-scale aluminum oxide material.
Fig. 14 is a schematic view of a composite quantum dot liquid crystal display device according to an embodiment of the invention. As shown in fig. 14, the composite quantum dot lcd device 52 includes a side-light type backlight module 32 and an lcd module 42, and the side-light type backlight module 32 includes a frame 380, a backlight source 100 and a light guide plate 320. In this embodiment, the backlight source 100 is a composite quantum dot light emitting diode (QD-LED)100a, 100b, or 100c shown in fig. 11 to 13, and the light emitting direction of the backlight source 100 faces the light incident side of the light guide plate 320, and the backlight module 32 further has at least one reflector 322 for concentrating the light emitted from the backlight source 100 to the light guide plate 320, and the light is emitted to the liquid crystal display module 42 above the light emitting side of the light guide plate 320.
Fig. 15A is a schematic view of a composite quantum dot liquid crystal display device according to another embodiment of the invention. As shown in fig. 15A, the composite quantum dot lcd device 54 includes a direct-type backlight module 34 and an lcd module 42, and the direct-type backlight module 34 includes a frame 380 and a backlight source 100. In this embodiment, the backlight source 100 is any one of the composite quantum dot light emitting diodes 100a, 100b or 100c shown in fig. 11 to 13 or a blue Light Emitting Diode (LED), the light emitting direction of the backlight source 100 faces the liquid crystal display module 42, and the frame 380 further has at least one reflective sheet 322 for concentrating the light emitted from the backlight source 100 to the liquid crystal display module 42, and the light is emitted from the liquid crystal display module 42.
The lcd module 42 includes a glass substrate 420 disposed above the edge-lit backlight module 32 or the direct-lit backlight module 34, a thin film transistor layer 424 disposed between the glass substrate 420 and the edge-lit backlight module 32 or the direct-lit backlight module 34, and a liquid crystal molecule layer 422 disposed between the glass substrate 420 and the thin film transistor layer 424.
Fig. 15B is a schematic view of a composite quantum dot liquid crystal display device according to still another embodiment of the invention. As shown in fig. 15B, the composite quantum dot lcd device 54 includes a direct-type backlight module 34, an lcd module 42, and a wavelength conversion layer 140 or a composite wavelength conversion layer 140, where the direct-type backlight module 34 includes a frame 380 and a backlight source 100. In this embodiment, the backlight source 100 may also be a composite quantum dot light emitting diode (QD-LED)100a, 100b, or 100c or a blue Light Emitting Diode (LED) as shown in fig. 11 to 13, and the light emitting direction of the backlight source 100 faces the liquid crystal display module 42, and the frame 380 further has at least one reflective sheet 322 for concentrating the light energy emitted from the backlight source 100, and then emitting the light energy to the liquid crystal display module 42 through the wavelength conversion layer 140 or the composite wavelength conversion layer 140, and the light energy is emitted from the liquid crystal display module 42. The difference between this embodiment and fig. 15A is that the backlight source 100 of the direct-type backlight module 34 may further have the wavelength conversion layer 140 or the composite wavelength conversion layer 140 (see fig. 11 and 12).
The lcd module 42 includes a glass substrate 420 disposed above the edge-lit backlight module 32 or the direct-lit backlight module 34, a thin film transistor layer 424 disposed between the glass substrate 420 and the edge-lit backlight module 32 or the direct-lit backlight module 34, and a liquid crystal molecule layer 422 disposed between the glass substrate 420 and the thin film transistor layer 424.
In addition, please refer to fig. 16, which is a schematic diagram of a composite quantum dot Micro light emitting diode (Micro LED) display device according to a first embodiment of the present invention. As shown in fig. 16, a composite quantum dot Micro light emitting diode (Micro LED) display device 200a includes a Micro light source 240, the Micro light source 240 is an active light emitting diode die or a passive light emitting diode die, and at least one composite quantum dot material 142 coated on a surface of the Micro light source. Wherein the at least one composite quantum dot material 142 comprises an optical core; an inorganic ligand layer coated on the surface of the optical core (see FIG. 1), the inorganic ligand layer comprising at least one silicon oxide (SiO)x) A material; and a water oxygen barrier layer coated on the surface of the inorganic ligand layer. Wherein, the water oxygen barrier layer is formed by stacking a laminated structure comprising at least one metal oxide.
Wherein the optical core may be a quantum dot made of a semiconductor material, such as: group II-VI quantum dots (CdSe or CdS), group III-V quantum dots ((Al, In, Ga) P, (Al, In, Ga) As or (Al, In, Ga) N), group II-VI quantum dots having a shell-core structure (CdSe/ZnS), group III-V quantum dots having a shell-core structure (InP/ZnS), non-spherical group II-VI quantum dots having an alloy structure (ZnCdSeS), a combination of any two or more of the above.
The optical core may also be of the general chemical formula MAX3The perovskite quantum dot of (a), the perovskite quantum dot mainly comprises an organic-inorganic hybrid perovskite quantum dot, an all-inorganic perovskite quantum dot or a combination thereof. Wherein the cation M is organic methylamine ion, ethylamine ion, formamidine ion or inorganic cesium ion (Cs)+) (ii) a The metal ion A is divalent lead ion (Pb)2+) Tin (Sn)2+) Or germanium ion (Ge)2+) (ii) a The halide ion X is a chloride ion (Cl) belonging to a cubic, orthorhombic or tetragonal system-) Bromine ion (Br)-) Or iodide ion (I)-)。
Wherein the oxide of Silicon (SiO)x) The material may be silicon dioxide (SiO)2) Or silicon monoxide (SiO). The at least one metal oxide is titanium oxide (TiO)2) Zinc oxide (ZnO), aluminum oxide (AlO)x) Or a combination thereof.
In the present embodiment, the micro light-emitting source 220 includes an led chip 220 and a plurality of spacer layers 260, the at least one composite quantum dot material 142 is disposed on the light-emitting side of the led chip 220, and more specifically, the at least one composite quantum dot material 142 is coated on the light-emitting side surface of the led chip 220 at intervals, and the plurality of spacer layers 260 are disposed between the led chip 220 and the at least one composite quantum dot material 142 at intervals. The led chip 220 is a vertical led chip, and includes a first electrode 222, a second electrode 224, and a P-type semiconductor layer, a light emitting layer 226 and an N-type semiconductor layer sequentially disposed between the first electrode 222 and the second electrode 224, wherein the light emitted from the led chip 220 is located on the same side as the first electrode 222.
In this embodiment, at least one composite quantum dot material 142 is coated on the surface of the Micro light-emitting source by an atomization coating method, in which the at least one composite quantum dot material 142 is mixed with a glue material (e.g., silica gel) and then uniformly coated on the surface of the Micro light-emitting source 240, and the color required by a single light-emitting diode chip 220 is automatically aligned and coated on the light-emitting diode chip 220 by using an atomization coating machine, thereby achieving a full-color Micro light-emitting diode (Micro LED) display device.
Fig. 17 is a schematic view of a quantum dot Micro light emitting diode (Micro LED) display device according to a second embodiment of the invention. As shown in fig. 17, a composite quantum dot Micro light emitting diode (Micro LED) display device 220b includes a Micro light source 240, the Micro light source 240 is an active light emitting diode die or a passive light emitting diode die, and at least one composite quantum dot material 142 coated on a surface of the Micro light source 240. Wherein the at least one composite quantum dot material packageIncludes an optical core; an inorganic ligand layer coated on the surface of the optical core, the inorganic ligand layer comprising at least one oxide of Silicon (SiO)x) A material; and a water oxygen barrier layer coated on the surface of the inorganic ligand layer. The water oxygen barrier layer is formed by stacking a laminated structure including at least one metal oxide (refer to fig. 1).
The difference between this embodiment and the composite quantum dot Micro light emitting diode (Micro LED) display device 200a of fig. 16 is that a Photoresist layer 144, such as a Photoresist Mask (PRM), a barrier layer (barrier layer) or a combination thereof, is further disposed between the Micro light emitting source 240 and the at least one composite quantum dot material 142. The material of the photoresist layer 144 is polymethyl methacrylate (PMMA), or other photoresist materials such as positive photoresist phenolic resin (or epoxy resin), negative photoresist polyisoprene rubber (or inverse photoresist), etc.; the photoresist layer 144 may be the wavelength conversion film 140 or the composite wavelength conversion film 140 described in fig. 9 and 10.
In the present embodiment, a full-color Micro light emitting diode (Micro LED) display device is obtained by performing a spray coating process of converting two wavelengths of green light and red light to form a photoresist layer 144 between the Micro light source 240 and the at least one composite quantum dot material 142 by using an atomization spray coating and a photolithography process.
Please refer to fig. 18, which is a schematic diagram of a composite quantum dot Micro light emitting diode (Micro LED) display device according to a third embodiment of the present invention. As shown in fig. 18, a composite quantum dot Micro light emitting diode (Micro LED) display device 200c includes a Micro light source 240, the Micro light source 240 is an active light emitting diode die or a passive light emitting diode die, and at least one composite quantum dot material 142 coated on a surface of the Micro light source 240. Wherein the at least one composite quantum dot material comprises an optical core; an inorganic ligand layer coated on the surface of the optical core, the inorganic ligand layer comprising at least one oxide of Silicon (SiO)x) A material; and a water oxygen barrier layer coated on the substrateOn the surface of the organic body layer. Wherein, the water oxygen barrier layer is formed by stacking a laminated structure comprising at least one metal oxide.
The difference between the present embodiment and the composite quantum dot Micro light emitting diode (Micro LED) display device 200b of fig. 17 is that the at least one composite quantum dot material 142 may further form a composite photoresist layer 146 with a photoresist material. The photoresist material is polymethyl methacrylate (PMMA), or other photoresist materials such as positive photoresist phenolic resin (phenol-formaldehyde resin) or epoxy resin (epoxy resin), negative photoresist polyisoprene rubber (polyisoprene rubber), and reverse photoresist; the composite photoresist layer 146 may also be the wavelength converting film 140 or the composite wavelength converting film 140 described in fig. 9 and 10.
In the embodiment, a full-color Micro light emitting diode (Micro LED) display device is achieved by using a spin coating process and a yellow photolithography process, and since the composite quantum dot material 142 of the present invention can be mutually soluble in a non-polar solution, the toluene solubility can be adjusted by using a methyl methacrylate (PMMA) electronic resist, and the composite resist layer 146 of the composite quantum dot material mixed with the methyl methacrylate (PMMA) can be adjusted by using the method, so as to improve the adhesion. The composite photoresist layer 146 is then coated on the micro-light source 240 by spin coating, and addressed deposition of quantum dot material is formed by photolithography.
Results of the experiment
Finally, the composite quantum dot material of the present invention is encapsulated in a light emitting diode element (as shown in fig. 11 to 13), and subjected to heat resistance and water and oxygen resistance experiments. First, please refer to fig. 19, which is a temperature test chart of the composite quantum dot material according to the preferred embodiment of the invention. As shown in fig. 19, during the heating process (solid line portion in the figure), the light emitting diode device and the conventional light emitting diode device packaged with the composite quantum dot material of the present invention both decrease the light emitting intensity with the increase of the temperature. On the other hand, during the cooling process (shown in dashed lines), the conventional led device is cooled from about 150 degrees celsius to 20 degrees celsius, and the light intensity of the led device is only restored to twenty percent of the original intensity; however, the light emitting diode device packaged with the composite quantum dot material of the present invention can recover the light emitting intensity to eighty percent of the original intensity under the condition that the temperature is also reduced from about 150 ℃ to 20 ℃. As described above, the composite quantum dot according to the present invention is not destroyed even in a high-temperature environment, and can effectively maintain the emission intensity of the light-emitting element.
Fig. 20 and 21 are schematic diagrams illustrating a water-blocking oxygen test of the composite quantum dot material according to the preferred embodiment of the invention. As shown in fig. 20, the experiment was conducted on a well-known light emitting diode element, a light emitting diode element in which the optical core is coated with the inorganic ligand layer of the present invention, and a light emitting diode element in which the composite quantum dot material of the present invention (including the optical core made of quantum dots, the inorganic ligand layer made of silicon oxide, and the water-oxygen barrier layer made of titanium oxide) is encapsulated, wherein the environment of the burning was a high-temperature and high-humidity environment in which the temperature is 60 degrees celsius and the relative humidity is 90%. As is apparent from the figure, the well-known led device has a light intensity maintenance rate of only ten percent of the original intensity at about 50 hours of the experiment; the light-emitting diode element provided with the inorganic ligand layer coated optical core still keeps the luminous intensity maintenance rate of fifty percent of the original intensity at about 100 hours of the experiment; surprisingly, even after the light-emitting diode element packaged with the composite quantum dot material is tested in the high-temperature high-humidity environment for 100 hours, the maintenance rate of the luminous intensity still has ninety-five percent of the original intensity, and the light-emitting diode element has the effects of water and oxygen resistance and high temperature resistance.
Fig. 21 also shows a conventional led device, a led device in which the optical core is covered with the inorganic ligand layer of the present invention, and a led device in which the composite quantum dot material of the present invention (including the optical core made of quantum dots, the inorganic ligand layer made of silicon oxide, and the water-oxygen barrier layer made of titanium oxide) is encapsulated, and the burning environment is changed to a general environment with a temperature of 25 degrees celsius and a relative humidity of 50%. As is apparent from the figure, the conventional led device has a luminous intensity maintenance rate of only twenty-five percent of the original intensity at about 1000 hours of the experiment; the luminous intensity maintaining rate of the LED element provided with the inorganic ligand layer coating the optical core is kept to be fifty percent of the original intensity at about 1000 hours of the experiment; it is also surprising that the led device packaged with the composite quantum dot material of the present invention has a luminous intensity maintenance rate of ninety five percent of the original intensity even after the led device is tested in the high temperature and high humidity environment for 1000 hours.
Finally, please refer to fig. 22, which is a color gamut comparison diagram of the composite quantum dot display device according to the preferred embodiment of the invention. In the present invention, the light emitting diode device encapsulated with the composite quantum dot material of the present invention is further applied to a liquid crystal display device (refer to fig. 14, 15A and 15B), as shown in fig. 22, the spectrum of the composite quantum dot (liquid crystal) display device of the present invention is further subjected to rec.2020 color gamut calculation, and it is found that the color gamut of the composite quantum dot (liquid crystal) display device of the present invention is about 90% (NTSC > 130%) (solid line triangle area in fig. 20), and is about 70% (NTSC > 90%) (dotted line triangle area in fig. 20) compared with the known wide color gamut display device, so that the rec.2020 color gamut of the quantum dot display device of the present invention is improved by nearly 1.3 times.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the invention, which is covered by the present invention even though the invention is briefly changed or modified according to the claims and the description.

Claims (22)

1. A preparation method of a composite quantum dot material is characterized by comprising the following steps:
(A) providing at least one optical core linked to a quantity of precursor;
(B) adding a surfactant or a non-polar solvent such that the at least one optical core is formed on the surface of the quantitative precursor structure;
(C) adding a silicon-containing compound to make the surface of the optical core have at least one oxide of silicon; and
(D) forming a composite quantum dot material coated with the oxide material of the at least one silicon.
2. The method for preparing the composite quantum dot material according to claim 1, wherein the surfactant is triton X-100 or nonylphenol polyether-5.
3. The method of claim 1, wherein the silicon-containing compound is tetraethyl silicate, tetramethyl silicate, or 3-aminopropyltriethoxysilane.
4. A composite quantum dot material, comprising:
a quantity of precursor being at least one inorganic oxide;
an optical core formed on the surface of the quantitative precursor;
an inorganic ligand layer coated on the surface of the optical core, the inorganic ligand layer comprising at least one oxide material of silicon; and
a water oxygen barrier layer coated on the surface of the inorganic ligand layer;
wherein, the water oxygen barrier layer is formed by stacking a laminated structure comprising at least one metal oxide.
5. The composite quantum dot material of claim 4, wherein the optical core is of the general chemical formula MAX3And M is a cation, a is a metal ion, and X is a halide ion.
6. The composite quantum dot material of claim 5, wherein the perovskite quantum dot is an organic-inorganic hybrid perovskite quantum dot or an all-inorganic perovskite quantum dot.
7. The composite quantum dot material of claim 4, wherein the at least one silicon oxide material is silicon dioxide, silicon monoxide, or a combination thereof.
8. The composite quantum dot material of claim 4, wherein the at least one metal oxide is titanium oxide, zinc oxide, aluminum oxide, or a combination thereof.
9. The composite quantum dot material of claim 4, wherein the at least one inorganic oxide is silica, silicon monoxide, or a combination thereof.
10. A preparation method of a composite quantum dot material is characterized by comprising the following steps:
providing an optical core and performing silanization treatment on the optical core;
adding a surfactant and a non-polar solvent to the silanized optical core; and
a silicon-containing compound is added such that the optical core surface has at least one silicon oxide material.
11. The method of claim 10, wherein step (D) is further performed after step (C) by adding an aqueous compound, and the aqueous compound and the silicon-containing compound undergo hydrolysis and condensation reactions to form an inorganic ligand layer.
12. The method of claim 11, wherein a step (E) of mixing zinc monoacetate hydrate and ethanol is further performed after the step (D) and adding to the optical core coated with the inorganic ligand layer.
13. The method of claim 11, wherein a step (E') of adding titanium isopropoxide or tetrabutyl titanate to the optical core coated with the inorganic ligand layer is further performed after the step (D).
14. The method of claim 12, wherein step (E) is further followed by step (F) of immersing the optical core coated with the inorganic ligand layer in an aqueous solution of sodium hydroxide-ethanol to form a composite quantum dot material.
15. The method of claim 13, wherein a step (F ') of immersing the optical core coated with the inorganic ligand layer in an aqueous-alcoholic solution is further performed after the step (E') to form a composite quantum dot material.
16. A composite quantum dot material, comprising:
an optical core;
an inorganic ligand layer coated on the surface of the optical core, the inorganic ligand layer comprising at least one oxide material of silicon; and
a water oxygen barrier layer coated on the surface of the inorganic ligand layer;
wherein, the water oxygen barrier layer is formed by stacking a laminated structure comprising at least one metal oxide.
17. The composite quantum dot material of claim 16, wherein the optical core is of the general chemical formula MAX3And M is a cation, a is a metal ion, and X is a halide ion.
18. The composite quantum dot material of claim 17, wherein the perovskite quantum dot is an organic-inorganic hybrid perovskite quantum dot or an all-inorganic perovskite quantum dot.
19. The composite quantum dot material of claim 16, wherein the at least one silicon oxide material is silicon dioxide, silicon monoxide, or a combination thereof.
20. The composite quantum dot material of claim 16, wherein the at least one metal oxide is titanium oxide, zinc oxide, aluminum oxide, or a combination thereof.
21. A composite quantum dot display device, comprising:
a backlight source;
at least one composite quantum dot material arranged on the backlight source; and
the liquid crystal display module is arranged on the at least one composite quantum dot material;
wherein the at least one composite quantum dot material comprises:
an optical core;
an inorganic ligand layer coated on the surface of the optical core, the inorganic ligand layer comprising at least one oxide material of silicon; and
a water oxygen barrier layer coated on the surface of the inorganic ligand layer;
wherein, the water oxygen barrier layer is formed by stacking a laminated structure comprising at least one metal oxide.
22. A composite quantum dot display device, comprising:
the micro light-emitting source is an active micro LED crystal grain or a passive micro LED crystal grain; and
at least one composite quantum dot material coated on the micro-luminous source;
wherein the at least one composite quantum dot material comprises:
an optical core;
an inorganic ligand layer coated on the surface of the optical core, the inorganic ligand layer comprising at least one oxide material of silicon; and
a water oxygen barrier layer coated on the surface of the inorganic ligand layer;
wherein, the water oxygen barrier layer is formed by stacking a laminated structure comprising at least one metal oxide.
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