CN109609116A - Quantum dot and quantum dots-polymer compound - Google Patents

Quantum dot and quantum dots-polymer compound Download PDF

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Publication number
CN109609116A
CN109609116A CN201811546485.9A CN201811546485A CN109609116A CN 109609116 A CN109609116 A CN 109609116A CN 201811546485 A CN201811546485 A CN 201811546485A CN 109609116 A CN109609116 A CN 109609116A
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quantum dot
core
shell
quantum
indium
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李鑫
李慧州
曹越峰
王允军
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Suzhou Xingshuo Nanotech Co Ltd
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Suzhou Xingshuo Nanotech Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/10—Encapsulated ingredients
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
    • C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/56—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing sulfur
    • C09K11/562—Chalcogenides
    • C09K11/565—Chalcogenides with zinc cadmium
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
    • C09K11/881—Chalcogenides
    • C09K11/883—Chalcogenides with zinc or cadmium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

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Abstract

This application discloses a kind of quantum dot and quantum dots-polymer compounds.The quantum dot includes: core；And the shell on the core is set；The core includes indium, phosphorus, zinc and Group VIA element, and the size of the core is not less than 2.5 nanometers.The quantum dot for the alloy core being made of at least four elements in indium, phosphorus, zinc and Group VIA element has smaller half-peak breadth and higher quantum yield.

Description

Quantum dot and quantum dots-polymer compound
Technical field
This application involves field of nanometer material technology more particularly to a kind of quantum dots and quantum dots-polymer compound.
Background technique
Quantum dot is the semiconductor material with crystalline texture of a type of size with several nanometers, due to it Minimum size, quantum dot have big per unit volume surface area and quantum limitation effect can be presented, thus display with The different physics of block materials with same composition and chemical property.Different from block materials, quantum dot, which can have, to be referred to as The physical characteristic that intrinsic characteristic can still be controlled by changing its size.As a kind of luminescent material, quantum dot has hair The advantages that half-peak breadth is small, transmitting peak-to-peak value is controllable is penetrated, to be widely used and study.
Therefore, exploitation promotes optical property such as quantum efficiency, stability of photoluminescence or transmitting half-peak breadth of quantum dot etc. Technology it is most important for the development of quantum dot.
Summary of the invention
The application's is designed to provide a kind of quantum dot, to promote the optical property of quantum dot.
According to the one aspect of the application, a kind of quantum dot is provided, the quantum dot includes: core；And it is arranged described Shell on core；The core includes indium, phosphorus, zinc and Group VIA element, and the size of the core is not less than 2.5 nanometers.Quantum dot Core is the alloy core being made of four kinds of indium, phosphorus, zinc and at least one Group VIA element or more element, the i.e. centre of luminescence of quantum dot Without containing heavy metal element.Inventors have found that with the simple indium phosphide core being made of two kinds of indium, phosphorus elements or doping zinc member The size of the indium phosphide nuclear phase ratio of element, the alloy core that this four kinds or more elements are constituted is bigger, and luminous efficiency is higher.In order to reach To predetermined launch wavelength such as feux rouges or green light, the size of existing indium phosphide quantum dot core is typically small, and (such as less than 2 are received Rice), and it is entirely different with the prior art, and the size of quantum dot core is not less than 2.5 nanometers in the application.
In one embodiment, core is preferably dimensioned to be 2.5~4.5 nanometers.
In one embodiment, Group VIA element includes sulphur or selenium.I.e. core may be by four kinds of indium, phosphorus, zinc and sulphur element groups At being perhaps made of four kinds of indium, phosphorus, zinc and selenium elements and be perhaps made of five kinds of indium, phosphorus, zinc and selenium, sulphur elements or also wrap The case where including other elements doping.
In one embodiment, in core the molar ratio of Group VIA element and phosphorus in (1~4): 1.
In one embodiment, in core the molar ratio of zinc and indium in (1~4): 1.
In one embodiment, the molar ratio of indium and phosphorus is (0.8~1.2): (0.8~1.2) in core.When rubbing for indium and phosphorus You than for about 1:1 it is optimal.
In one embodiment, shell is the multilayered shell for including at least two shells, and two neighbouring layers have different from each other Composition.I.e. shell can be double shells, or three layers or the shell composition greater than three layers.
In one embodiment, shell includes two shells, and outermost shell is ZnS, and the shell close to the core is ZnSeS。
According to further aspect of the application, a kind of quantum dots-polymer compound is provided, comprising: polymeric matrix；With The quantum dot as described above of dispersion in a polymer matrix.
In one embodiment, polymeric matrix includes thiol-ene resin, (methyl) acrylate polymer, amino first Acid ester resin, epoxy resin, polyvinyl, organic siliconresin, or combinations thereof.
The utility model has the advantages that including the quantum for the alloy core being made of at least four elements in indium, phosphorus, zinc and Group VIA element Point has smaller half-peak breadth and higher quantum yield.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of quantum dot in the application one schematical embodiment.
Specific embodiment
Below in conjunction with the application embodiment, technical solutions in the embodiments of the present application is described in detail.It answers It is noted that described embodiment is only a part of embodiment of the application, rather than whole embodiments.
Fig. 1 is the structural schematic diagram of quantum dot in the application one schematical embodiment, and quantum dot 100 includes core 101, Core 101 includes indium, phosphorus, zinc and Group VIA element；And the shell 102 on core 101 is set.
Embodiment 1
The core of quantum dot is made of four kinds of indium, phosphorus, zinc and sulphur elements, and the shell of quantum dot is pair that ZnSe and ZnS is constituted Shell.Preparation process is as follows:
The octadecylene for weighing the indium acetate of 0.1mmol, the zinc stearate of 0.1mmol, the tetradecylic acid of 0.3mmol, 10ml, adds Enter into 100ml three-necked flask, 300 DEG C of heat preservations are heated under nitrogen exhaust condition.By three (trimethyl silicane) phosphines of 0.1mmol The mixed liquor of sulphur-tri octyl phosphine (0.1mmol/ml) of (being dispersed in the octadecylene of 1ml), 1ml is rapidly injected, and is reacted 1 hour The core solution of quantum dot is obtained afterwards.It is tested by high resolution transmission electron microscopy, the size of the core is about at 2.5 nanometers.
Reaction temperature is down to 150 DEG C, the zinc acetate of 1.5mmol is added, is vented 30min, is warming up to 260 DEG C, 1ml is added Selenium-tri octyl phosphine (0.1mmol/ml), reaction 20min, obtain being coated on the ZnSe shell on core, add 0.8ml sulphur-three Octyl phosphine (1mmol/ml) reacts 20min, obtains in the ZnS shell being coated on ZnSe shell.It is down to room after reaction Temperature is extracted three times with methanol, and is centrifuged with acetone precipitation, and precipitating is dissolved in toluene, and quantum dot is obtained.By surveying It tries, the emission peak of quantum dot is about at 531 nanometers in embodiment 1, and half-peak breadth is about at 45 nanometers, and quantum yield is about 45%.
Embodiment 2
The core of quantum dot is made of five kinds of indium, phosphorus, zinc, sulphur and selenium elements, and the shell of quantum dot is that ZnSe and ZnS is constituted Bivalve layer.Preparation process is as follows:
The octadecylene for weighing the indium acetate of 0.1mmol, the zinc stearate of 0.4mmol, the tetradecylic acid of 0.3mmol, 10ml, adds Enter into 100ml three-necked flask, 300 DEG C of heat preservations are heated under nitrogen exhaust condition.By three (trimethyl silicane) phosphines of 0.1mmol Sulphur-tri octyl phosphine (0.2mmol/ of selenium-tri octyl phosphine (0.2mmol/ml) of (being dispersed in the octadecylene of 1ml), 1ml, 1ml Ml mixed liquor) is rapidly injected, and reaction obtained the core solution of quantum dot after 1 hour.It is surveyed by high resolution transmission electron microscopy Examination, the size of the core is about at 4.5 nanometers.
Reaction temperature is down to 150 DEG C, the zinc acetate of 1.5mmol is added, is vented 30min, is warming up to 260 DEG C, 1ml is added Selenium-tri octyl phosphine (0.1mmol/ml), reaction 20min, obtain being coated on the ZnSe shell on core, add 0.8ml sulphur-three Octyl phosphine (1mmol/ml) reacts 20min, obtains in the ZnS shell being coated on ZnSe shell.It is down to room after reaction Temperature is extracted three times with methanol, and is centrifuged with acetone precipitation, and precipitating is dissolved in toluene, and quantum dot is obtained.By surveying It tries, the emission peak of quantum dot is about at 524 nanometers in embodiment 2, and half-peak breadth is about at 47 nanometers, and quantum yield is about 46%.
Comparative example 1
The core of quantum dot is made of three kinds of indium, phosphorus and zinc elements, and the shell of quantum dot is the bivalve that ZnSe and ZnS is constituted Layer.Preparation process is as follows:
The octadecylene for weighing the indium acetate of 0.1mmol, the zinc stearate of 0.1mmol, the tetradecylic acid of 0.3mmol, 10ml, adds Enter into 100ml three-necked flask, 300 DEG C of heat preservations are heated under nitrogen exhaust condition.By three (trimethyl silicane) phosphines of 0.1mmol (being dispersed in the octadecylene of 1ml) is rapidly injected, and reaction obtained the core solution of quantum dot after 1 hour.Electricity is transmitted by high-resolution Sub- microscope test, the size of the core is about at 1.7 nanometers.
Reaction temperature is down to 150 DEG C, the zinc acetate of 1.5mmol is added, is vented 30min, is warming up to 260 DEG C, 1ml is added Selenium-tri octyl phosphine (0.1mmol/ml), reaction 20min, obtain being coated on the ZnSe shell on core, add 0.8ml sulphur-three Octyl phosphine (1mmol/ml) reacts 20min, obtains in the ZnS shell being coated on ZnSe shell.It is down to room after reaction Temperature is extracted three times with methanol, and is centrifuged with acetone precipitation, and precipitating is dissolved in toluene, and quantum dot is obtained.By surveying It tries, the emission peak of quantum dot is about at 534 nanometers in embodiment 1, and half-peak breadth is about at 53 nanometers, and quantum yield is about 37%.
By above-described embodiment 1, embodiment 2 and comparative example 1 it is found that compared with containing indium, zinc and phosphorus in the core of quantum dot (comparative example 1) (is implemented when containing indium, zinc, sulphur and phosphorus (embodiment 1) in the core of quantum dot or containing indium, zinc, sulphur, selenium and phosphorus Example 2) in compare, half-peak breadth is respectively reduced by 53 nanometers as 45 nanometers and 47 nanometers, quantum yield by 37% increase separately for 45% and 46%.
Although inventor has done more detailed elaboration to the technical solution of the application and has enumerated, it should be understood that for For those skilled in the art, above-described embodiment is modified and/or the flexible or equivalent alternative solution of use is obvious , cannot all be detached from the essence of the application spirit, the term occurred in the application be used for elaboration to technical scheme and Understand, the limitation to the application can not be constituted.

Claims (10)

1. a kind of quantum dot, the quantum dot include:
Core；And the shell on the core is set；
The core includes indium, phosphorus, zinc and Group VIA element, and the size of the core is not less than 2.5 nanometers.
2. quantum dot according to claim 1, which is characterized in that the size of the core is 2.5~4.5 nanometers.
3. quantum dot according to claim 1, which is characterized in that the Group VIA element includes sulphur or selenium.
4. quantum dot according to claim 1, which is characterized in that in the core, the molar ratio of Group VIA element and phosphorus is (1 ~4): 1.
5. quantum dot according to claim 1, which is characterized in that in the core, the molar ratio of zinc and indium is in (1~4): 1.
6. quantum dot according to claim 1, which is characterized in that in the core, the molar ratio of indium and phosphorus be (0.8~ 1.2): (0.8~1.2).
7. quantum dot according to claim 1, which is characterized in that the shell is the multilayered shell for including at least two shells, Neighbouring two layer of at least two shell has composition different from each other.
8. quantum dot according to claim 1, which is characterized in that the shell includes two shells, and outermost shell is ZnS, the shell close to the core are ZnSe or ZnSeS.
9. a kind of quantum dots-polymer compound, comprising:
Polymeric matrix；With
Dispersion in the polymer matrix such as quantum dot of any of claims 1-8.
10. quantum dots-polymer compound according to claim 9, which is characterized in that the polymeric matrix includes sulphur Alcohol-olefine resin, (methyl) acrylate polymer, carbamate resins, epoxy resin, polyvinyl, organosilicon tree Rouge, or combinations thereof.
CN201811546485.9A 2018-12-18 2018-12-18 Quantum dot and quantum dots-polymer compound Pending CN109609116A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11279874B2 (en) 2020-05-04 2022-03-22 National Tsing Hua University Quantum dot
WO2022111520A1 (en) * 2020-11-24 2022-06-02 苏州星烁纳米科技有限公司 Indium-oxygen cluster, preparation method therefor, quantum dot prepared therefrom and preparation method for quantum dot

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN105051153A (en) * 2013-03-15 2015-11-11 纳米技术有限公司 Group iii-v/zinc chalcogenide alloyed semiconductor quantum dots

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Publication number Priority date Publication date Assignee Title
CN105051153A (en) * 2013-03-15 2015-11-11 纳米技术有限公司 Group iii-v/zinc chalcogenide alloyed semiconductor quantum dots

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JENNIFER K. MOLLOY等: "Sensitisation of visible and NIR lanthanide emission by InPZnS quantum dots in bi-luminescent hybrids", 《CHEM. COMMUN.》 *
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11279874B2 (en) 2020-05-04 2022-03-22 National Tsing Hua University Quantum dot
WO2022111520A1 (en) * 2020-11-24 2022-06-02 苏州星烁纳米科技有限公司 Indium-oxygen cluster, preparation method therefor, quantum dot prepared therefrom and preparation method for quantum dot

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Application publication date: 20190412