CN105219380A - A kind of high quality colloid is without the synthetic method of cadmium quantum dot - Google Patents
A kind of high quality colloid is without the synthetic method of cadmium quantum dot Download PDFInfo
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Abstract
The invention discloses the synthetic method of a kind of high quality without cadmium quantum dot, copper source, indium source, sulphur source are dissolved in whiteruss, be heated to 100-150 DEG C, obtain body fluid before copper indium, vacuumize, repeatedly nitrogen injection, under atmospheric environment or under inert atmosphere protection, continue to be heated to 180-260 DEG C, insulation, obtains core quantum dot solution; Be dissolved in whiteruss by zinc source, be heated to 100-200 DEG C, obtain body fluid before zinc, at such a temperature, body fluid before zinc is injected core quantum dot solution, is warming up to 180-260 DEG C, insulation, obtains quantum dot solution with core-shell structure; By quantum dot solution with core-shell structure purifying, obtain nuclear shell structure quantum point finished product.The present invention adopts cheapness, nontoxic, and the whiteruss of stable chemical nature is as non-coordinating solvent, and preparation is without cadmium quantum dot.Due to the chemical property that whiteruss is stable, have isolated effect very well for the moisture in air and oxygen, this preparation process also can be carried out under air ambient, has greatly saved the cost of vacuum environment.
Description
Technical field
The present invention relates to the preparing technical field of semiconductor nano material, concrete a kind of high quality colloid is without the synthetic method of cadmium quantum dot.
Background technology
Quantum dot is a kind of inorganic nanocrystal, and the size due to nanocrystal is less than the Exciton Bohr Radius of body material, and electronics and hole are by quantum confinement, and quasi-continuous energy band structure becomes discrete energy levels structure.Due to exciting of external energy, comprise optical, electrical and other rays, the electronics in quantum dot by valence to conduction band, valence band leaves hole, hole in the electronics on conduction band of transition and valence band forms electron-hole pair (i.e. exciton), and the electronics on conduction band can transit to valence band again, and transition process may be nonradiative transition, namely in the mode of lattice vibration, allowing electronics get back to valence band, also may be radiative transition, namely can with in the process of valence band in transition, release photon, namely luminous.Because quantum confinement is relevant with the size of nanocrystal, therefore, the band gap width of quantum dot also receives the impact of size, that is photon energy, the emission wavelength of the transition release of electronics all receive the impact of the size of quantum dot, the dimensional effect of Here it is quantum dot.Dimensional effect allows the luminescence of quantum dot obtain continuously adjustable spectrum by the size changing nanocrystal, has great application in illumination and display field.
At present, CdSe quantum dots emmission spectrum visible-range in the continuously adjustabe elementary composition by II-VI group, prepared quantum dot size is evenly distributed, the peak width at half height of spectrum is narrower, after organic-inorganic passivation is carried out to its surface, show very high quantum yield and stability and be subject to extensively research and pay close attention to.But, employ heavy metal cadmium (Cd) in CdSe quantum dots, certain toxicity and pollution are all existed to human body and physical environment, it is applied again, receive certain limitation, therefore synthesis exploitation has very major and immediate significance without cadmium low cadmium quantum dot light emitting material.In addition, because CdSe quantum dots has less Stokes shift, make in the process of application, the overlap that absorption spectrum and emmission spectrum exist a part causes self absorption effect, is subject to certain restrictions in display lighting field.
The copper indium sulphur that II-III-VI race is elementary composition and alloy quantum dot thereof are the Nano semiconductor crystalline materials being subject to extensive concern at present; the main non-coordinating solvent mainly adopted at organic synthesis copper indium sulphur quantum dot is at present octadecylene; this compound cost is higher; irritant to the skin of people; and contaminate environment; chemical property is relatively unstable, inflammable and explosive, so building-up process needs to carry out under vacuum environment atmosphere protection.
Summary of the invention
Technical problem to be solved by this invention is the synthetic method of a kind of high quality colloid without cadmium quantum dot.
The technical solution used in the present invention is:
High quality colloid, without a synthetic method for cadmium quantum dot, comprises the following steps:
Copper source, indium source, sulphur source are dissolved in whiteruss, are heated to 100-150 DEG C, obtain body fluid before copper indium, vacuumize, repeatedly nitrogen injection, under atmospheric environment or under inert atmosphere protection, continue to be heated to 180-260 DEG C, insulation 1-30min, obtains core quantum dot solution;
Be dissolved in whiteruss by zinc source, be heated to 100-200 DEG C, obtain body fluid before zinc, at such a temperature, body fluid before described zinc is injected described core quantum dot solution, is warming up to 180-260 DEG C, insulation, obtains quantum dot solution with core-shell structure;
By described quantum dot solution with core-shell structure purifying, obtain nuclear shell structure quantum point finished product.
Preferably, prepare in the process of described core quantum dot solution, be also added with doping metals source, doping metals source is zinc source or gallium source.
Preferably, described copper source is cuprous iodide or organic copper.
Preferably, described indium source is any one in Zinic stearas, zinc oleate, zinc acetate.
Preferably, described sulphur source is any one in Dodecyl Mercaptan, H2S, sodium sulphite, sulphur powder.
Preferably, the amount of substance in described copper source, indium source is than being 1:(1-10).
Preferably, the concrete steps of described purge process are: in described quantum dot solution with core-shell structure, add organic solvent extract, then add ethanol, centrifugally obtain quantum dot powder.
Further preferably, described purge process is multiple purge process.
The invention has the beneficial effects as follows: the present invention adopts cheapness, nontoxic, the whiteruss of stable chemical nature is as non-coordinating solvent, and preparation is without cadmium quantum dot.Due to the chemical property that whiteruss is stable, have isolated effect very well for the moisture in air and oxygen, this preparation process also can be carried out under air ambient, has greatly saved the cost of vacuum environment.
Accompanying drawing explanation
Fig. 1 is the CuInS that embodiment 1 prepares
2/ ZnS quantum dot fluorescence spectrum figure;
Fig. 2 is the CuInS that embodiment 2 prepares
2/ ZnS quantum dot fluorescence spectrum figure;
Fig. 3 is the ZnCuInS that embodiment 4 prepares
2/ ZnS quantum dot fluorescence spectrum figure;
Fig. 4 is the CuGa that embodiment 5 prepares
0.8in
0.2s
2/ ZnS quantum dot fluorescence spectrum figure.
Embodiment
Be clearly and completely described below with reference to embodiment and the accompanying drawing technique effect to design of the present invention, concrete structure and generation, to understand object of the present invention, characteristic sum effect fully.Obviously; described embodiment is a part of embodiment of the present invention, instead of whole embodiment, based on embodiments of the invention; other embodiments that those skilled in the art obtains under the prerequisite not paying creative work, all belong to the scope of protection of the invention.In addition, all connection/annexations related in patent, not singly refer to that component directly connects, and refer to and according to concrete performance, can connect auxiliary by adding or reducing, and form more excellent draw bail.Each technical characteristic in the invention, can combination of interactions under the prerequisite of not conflicting conflict.
embodiment 1:
1, CuInS
2the preparation of core quantum dot
Get the indium acetate (In (Ac) of the cuprous iodide (CuI) of 0.25mmol, 1mmol
2), the Dodecyl Mercaptan (DDT) of 5mL and the whiteruss of 10mL be placed in the there-necked flask of 50mL, heated and stirred to 100 DEG C, vacuumize and nitrogen injection 30 minutes repeatedly; under the protection of inert atmosphere; solution is heated to 230 DEG C, keeps 3 minutes, can CuInS be obtained
2core quantum dot.
2, CuInS
2the preparation of/ZnS core-shell structured quantum dot
In another there-necked flask system, add the Zinic stearas (Zn (SA) of 16mmol
2), the DDT of 8mL adds the whiteruss of 16mL, heated and stirred to 150 DEG C, obtains transparent liquid.At such a temperature, under the protection of inert atmosphere, this transparent liquid is injected CuInS rapidly
2core quantum dot solution in, promote the temperature to 250 DEG C of mixing solutions, be incubated 2 hours.Obtain CuInS
2/ ZnS core-shell structured quantum dot.
3, purifying CuInS
2/ ZnS core-shell structured quantum dot
To obtain quantum dot solution with core-shell structure to add normal hexane/methyl alcohol and extract, the quantum dot extraction liquid then getting 5mL adds 10mL centrifuge tube, then continues the ethanol adding 5mL in centrifuge tube, obtains muddy milky white liquid.Speed more than 8000 revs/min carries out centrifugal treating 10 minutes, obtains quantum dot precipitation powder.Rejoin normal hexane, and alcohol, repetitive operation is centrifugal, is dispersed in normal hexane by secondary centrifuging quantum dot, the final CuInS namely obtained
2/ ZnS is without cadmium nuclear shell structure quantum point.
The present embodiment, under inert atmosphere protection, successfully prepares CuInS in whiteruss
2/ ZnS quantum dot, prepares gained CuInS
2the fluorescence spectrum figure of/ZnS quantum dot is as Fig. 1, and the emission wavelength of quantum dot is 564nm, and absolute quantum yield is up to 83%, and peak width at half height is 98nm.For high-quality without cadmium quantum dot, can be applicable to White-light LED illumination and technique of display.Inorganic passivation is completed to copper indium sulphur quantum dot surface, make it have higher quantum yield, larger Stokes shift, and emission wavelength is continuously adjustabe in visible-range, and on the basis of quantum dot size effect, there is elemental ratio adjustable, i.e. Cu/In rate regulation emission wavelength, alloying constituents is adjustable, namely Ga is mixed, on the basis of the elements such as Zn, there is blue shift in various degree and red shift in the emission peak of copper indium sulphur quantum dot, transmitting boundary is increased to 500 to 900nm, the dependence of the element for heavy metal has not only been broken away from from raw material, thus lower conversion luminescence device can be applied to, as in the device of display and lighting, it is a kind of more satisfactory light-converting material.
embodiment 2:
1, CuInS
2the preparation of core quantum dot
Get CuI, 0.5mmolIn (Ac) of 0.125mmol
2, 2.5mL the whiteruss of DDT and 10mL be placed in the there-necked flask of 50mL, heated and stirred to 100 DEG C, vacuumize and nitrogen injection 30 minutes repeatedly, then under atmospheric environment, solution be heated to 230 DEG C, keep 3 minutes, can CuInS be obtained
2core quantum dot.
2, CuInS
2the preparation of/ZnS core-shell structured quantum dot
In another there-necked flask system, add the Zinic stearas (Zn (SA) of 8mmol
2), the DDT of 4mL adds the whiteruss of 8mL, heated and stirred to 150 DEG C, obtains transparent liquid.At such a temperature, under atmospheric environment, this transparent liquid is injected CuInS rapidly
2core quantum dot solution in, promote the temperature to 250 DEG C of mixing solutions, be incubated 1.5 hours.Obtain CuInS
2/ ZnS core-shell structured quantum dot.
3, purifying CuInS
2/ ZnS core-shell structured quantum dot
To obtain quantum dot solution with core-shell structure to add normal hexane/methyl alcohol and extract, the quantum dot extraction liquid then getting 5mL adds 10mL centrifuge tube, then continues the ethanol adding 5mL in centrifuge tube, obtains muddy milky white liquid.Speed more than 8000 revs/min carries out centrifugal treating 10 minutes, obtains quantum dot precipitation powder.Rejoin normal hexane, and alcohol, repetitive operation is centrifugal, is dispersed in normal hexane by secondary centrifuging quantum dot.Namely the final CuInS obtained
2/ ZnS is without cadmium nuclear shell structure quantum point.
The present embodiment, under atmospheric environment, successfully prepares CuInS in whiteruss
2/ ZnS quantum dot, prepares gained CuInS
2the fluorescence spectrum figure of/ZnS quantum dot is as Fig. 2, and the emission wavelength of quantum dot is at 630nm, and fluorescence quantum yield is 60%, and peak width at half height is 121nm.For high quality is without cadmium quantum dot, can be applicable to White-light LED illumination and technique of display.The present invention adopts cheapness; nontoxic; the whiteruss of stable chemical nature is as non-coordinating solvent; preparation, without cadmium quantum dot, due to the chemical property that whiteruss is stable, has isolated effect very well for the moisture in air and oxygen; this preparation process also can be carried out under air ambient; greatly saved the cost of vacuum environment, the method for the invention also can be carried out under inert atmosphere protection, the quantum dot of the quantum dot produced owing to synthesizing under air ambient.
embodiment 3:
1, CuInS
2the preparation of core quantum dot
Get the indium acetate (In (Ac) of the cuprous iodide (CuI) of 0.25mmol, 1mmol
2), the Dodecyl Mercaptan (DDT) of 5mL and the whiteruss of 10mL be placed in the there-necked flask of 50mL, heated and stirred to 150 DEG C, vacuumize and nitrogen injection 30 minutes repeatedly; under the protection of inert atmosphere; solution is heated to 260 DEG C, keeps 3 minutes, can CuInS be obtained
2core quantum dot.
2, CuInS
2the preparation of/ZnS core-shell structured quantum dot
In another there-necked flask system, add the Zinic stearas (Zn (SA) of 16mmol
2), the DDT of 8mL adds the whiteruss of 16mL, heated and stirred to 100 DEG C, obtains transparent liquid.At such a temperature, under the protection of inert atmosphere, this transparent liquid is injected CuInS rapidly
2core quantum dot solution in, promote the temperature to 180 DEG C of mixing solutions, be incubated 2.5 hours.Obtain CuInS
2/ ZnS core-shell structured quantum dot.
3, purifying CuInS
2/ ZnS core-shell structured quantum dot
To obtain quantum dot solution with core-shell structure to add normal hexane/methyl alcohol and extract, the quantum dot extraction liquid then getting 5mL adds 10mL centrifuge tube, then continues the ethanol adding 5mL in centrifuge tube, obtains muddy milky white liquid.Speed more than 8000 revs/min carries out centrifugal treating 10 minutes, obtains quantum dot precipitation powder.Rejoin normal hexane, and alcohol, repetitive operation is centrifugal, is dispersed in normal hexane by secondary centrifuging quantum dot, the final CuInS namely obtained
2/ ZnS without cadmium nuclear shell structure quantum point, gained quantum dot be high quality without cadmium quantum dot, can be applicable to White-light LED illumination and technique of display.
embodiment 4:
1, ZnCuInS
2the preparation of core quantum dot
Get the Zinic stearas (Zn (SA) of CuI, 0.125mmol of 0.125mmol
2), 0.125mmolIn (Ac)
2, 2.5mL the whiteruss of DDT and 10mL be placed in the there-necked flask of 50mL, heated and stirred to 100 DEG C, vacuumize and nitrogen injection 30 minutes repeatedly, under the protection of inert atmosphere, solution be heated to 230 DEG C, keep 3 minutes, can ZnCuInS be obtained
2core quantum dot.
2, ZnCuInS
2the preparation of/ZnS core-shell structured quantum dot
In another there-necked flask system, add the Zinic stearas (Zn (SA) of 8mmol
2), the DDT of 4mL adds the whiteruss of 8mL, heated and stirred to 150 DEG C, obtains transparent liquid.At such a temperature, under the protection of inert atmosphere, this transparent liquid is injected ZnCuInS rapidly
2in core quantum dot solution, promote the temperature to 250 DEG C of mixing solutions, be incubated 1.5 hours.Obtain ZnCuInS
2/ ZnS core-shell structured quantum dot.
3, purifying ZnCuInS
2/ ZnS core-shell structured quantum dot
To obtain quantum dot solution with core-shell structure to add normal hexane/methyl alcohol and extract, the quantum dot extraction liquid then getting 5mL adds 10mL centrifuge tube, then continues the ethanol adding 5mL in centrifuge tube, obtains muddy milky white liquid.Speed more than 8000 revs/min carries out centrifugal treating 10 minutes, obtains quantum dot precipitation powder.Rejoin normal hexane, and alcohol, repetitive operation is centrifugal, is dispersed in normal hexane by secondary centrifuging quantum dot.Namely the final ZnCuInS obtained
2/ ZnS is without cadmium nuclear shell structure quantum point.
The present embodiment, under inert atmosphere protection, successfully prepares ZnCuInS in whiteruss
2/ ZnS quantum dot, prepares gained ZnCuInS
2the fluorescence spectrum figure of/ZnS quantum dot is as Fig. 3, and the emission wavelength of quantum dot is at 573nm, and fluorescence quantum yield is 68%, and peak width at half height is 110nm.For high quality is without cadmium quantum dot, can be applicable to White-light LED illumination and technique of display.
embodiment 5:
1, CuGa
0.8in
0.2s
2the preparation of core quantum dot
Get the methyl ethyl diketone gallium (Ga (Acac) of CuI, 0.4mmol of 0.125mmol
2), 0.1mmolIn (Ac)
2, 2.5mL the whiteruss of DDT and 10mL be placed in the there-necked flask of 50mL, heated and stirred to 100 DEG C, vacuumize and nitrogen injection 30 minutes repeatedly, under the protection of inert atmosphere, solution be heated to 230 DEG C, keep 3 minutes, can CuGa be obtained
0.8in
0.2s
2core quantum dot.
2, CuGa
0.8in
0.2s
2the preparation of/ZnS core-shell structured quantum dot
In another there-necked flask system, the interpolation Zinic stearas of 8mmol, the DDT of 4mL add the whiteruss of 8mL, and heated and stirred to 150 DEG C, obtains transparent liquid.At such a temperature, under the protection of inert atmosphere, this transparent liquid is injected CuGa rapidly
0.8in
0.2s
2in core quantum dot solution, promote the temperature to 250 DEG C of mixing solutions, be incubated 1.5 hours.Obtain CuGa
0.8in
0.2s
2/ ZnS core-shell structured quantum dot.
3, purifying CuGa
0.8in
0.2s
2/ ZnS core-shell structured quantum dot
To obtain quantum dot solution with core-shell structure to add normal hexane/methyl alcohol and extract, the quantum dot extraction liquid then getting 5mL adds 10mL centrifuge tube, then continues the ethanol adding 5mL in centrifuge tube, obtains muddy milky white liquid.Speed more than 8000 revs/min carries out centrifugal treating 10 minutes, obtains quantum dot precipitation powder.Rejoin normal hexane, and alcohol, repetitive operation is centrifugal, is dispersed in normal hexane by secondary centrifuging quantum dot.Namely the final CuGa obtained
0.8in
0.2s
2/ ZnS is without cadmium nuclear shell structure quantum point.
The present embodiment, under inert atmosphere protection, successfully prepares CuGa in whiteruss
0.8in
0.2s
2/ ZnS quantum dot, prepares gained CuGa
0.8in
0.2s
2the fluorescence spectrum figure of/ZnS quantum dot is as Fig. 4, and the emission wavelength of quantum dot is at 530nm, and fluorescence quantum yield is 71%, and peak width at half height is 131nm.For high quality is without cadmium quantum dot, can be applicable to White-light LED illumination and technique of display.
embodiment 6:
1, CuGa
0.8in
0.2s
2the preparation of core quantum dot
Get the methyl ethyl diketone gallium (Ga (Acac) of CuI, 0.4mmol of 0.125mmol
2), 1.25mmolIn (Ac)
2, 2.5mL the whiteruss of DDT and 10mL be placed in the there-necked flask of 50mL, heated and stirred to 150 DEG C, vacuumize and nitrogen injection 30 minutes repeatedly, under the protection of inert atmosphere, solution be heated to 180 DEG C, keep 6 minutes, can CuGa be obtained
0.8in
0.2s
2core quantum dot.
2, CuGa
0.8in
0.2s
2the preparation of/ZnS core-shell structured quantum dot
In another there-necked flask system, the interpolation Zinic stearas of 8mmol, the DDT of 4mL add the whiteruss of 8mL, and heated and stirred to 200 DEG C, obtains transparent liquid.At such a temperature, under the protection of inert atmosphere, this transparent liquid is injected CuGa rapidly
0.8in
0.2s
2in core quantum dot solution, promote the temperature to 260 DEG C of mixing solutions, be incubated 1.5 hours.Obtain CuGa
0.8in
0.2s
2/ ZnS core-shell structured quantum dot.
3, purifying CuGa
0.8in
0.2s
2/ ZnS core-shell structured quantum dot
To obtain quantum dot solution with core-shell structure to add normal hexane/methyl alcohol and extract, the quantum dot extraction liquid then getting 5mL adds 10mL centrifuge tube, then continues the ethanol adding 5mL in centrifuge tube, obtains muddy milky white liquid.Speed more than 8000 revs/min carries out centrifugal treating 10 minutes, obtains quantum dot precipitation powder.Rejoin normal hexane, and alcohol, repetitive operation is centrifugal, is dispersed in normal hexane by secondary centrifuging quantum dot.Namely the final CuGa obtained
0.8in
0.2s
2/ ZnS without cadmium nuclear shell structure quantum point, gained quantum dot be high quality without cadmium quantum dot, can be applicable to White-light LED illumination and technique of display.
Claims (8)
1. high quality colloid is without a synthetic method for cadmium quantum dot, it is characterized in that, comprises the following steps:
Copper source, indium source, sulphur source are dissolved in whiteruss, are heated to 100-150 DEG C, obtain body fluid before copper indium, vacuumize, repeatedly nitrogen injection, under atmospheric environment or under inert atmosphere protection, continue to be heated to 180-260 DEG C, insulation 1-30min, obtains core quantum dot solution;
Be dissolved in whiteruss by zinc source, be heated to 100-200 DEG C, obtain body fluid before zinc, at such a temperature, body fluid before described zinc is injected described core quantum dot solution, is warming up to 180-260 DEG C, insulation, obtains quantum dot solution with core-shell structure;
By described quantum dot solution with core-shell structure purifying, obtain nuclear shell structure quantum point finished product.
2. high quality colloid according to claim 1 is without the synthetic method of cadmium quantum dot, it is characterized in that, prepares in the process of described core quantum dot solution, is also added with doping metals source, and doping metals source is zinc source or gallium source.
3. high quality colloid according to claim 1 is without the synthetic method of cadmium quantum dot, it is characterized in that, described copper source is cuprous iodide or organic copper.
4. high quality colloid according to claim 1 is without the synthetic method of cadmium quantum dot, it is characterized in that, described indium source is any one in Zinic stearas, zinc oleate, zinc acetate.
5. high quality colloid according to claim 1 is without the synthetic method of cadmium quantum dot, it is characterized in that, described sulphur source is Dodecyl Mercaptan, H
2any one in S, sodium sulphite, sulphur powder.
6. high quality colloid according to claim 1 is without the synthetic method of cadmium quantum dot, it is characterized in that, the amount of substance in described copper source, indium source is than being 1:(1-10).
7. high quality colloid according to claim 1 is without the synthetic method of cadmium quantum dot, it is characterized in that, the concrete steps of described purge process are: in described quantum dot solution with core-shell structure, add organic solvent extract, then add ethanol, centrifugally obtain quantum dot powder.
8. high quality colloid according to claim 7 is without the synthetic method of cadmium quantum dot, it is characterized in that, described purge process is multiple purge process.
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| PCT/CN2016/102486 WO2017067451A1 (en) | 2015-10-20 | 2016-10-19 | Method for synthesizing high-quality colloidal cadmium-free quantum dots |
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| CN109233808A (en) * | 2018-09-27 | 2019-01-18 | 苏州星烁纳米科技有限公司 | The preparation method of quantum dot with ZnS shell cladding |
| CN110945105A (en) * | 2017-07-27 | 2020-03-31 | Ns材料株式会社 | Quantum dot, wavelength conversion member using quantum dot, illumination member, backlight device, display device, and method for manufacturing quantum dot |
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| CN109233808B (en) * | 2018-09-27 | 2021-07-02 | 苏州星烁纳米科技有限公司 | Preparation method of quantum dot coated with ZnS shell layer |
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| CN111977685B (en) * | 2020-06-09 | 2022-09-02 | 河南大学 | Preparation method of sodium ion battery negative electrode material |
| CN115340863A (en) * | 2022-06-29 | 2022-11-15 | 河北大学 | Near-infrared core-shell structure quantum dot CuInS 2 Method for synthesizing/ZnS |
| CN115340863B (en) * | 2022-06-29 | 2023-11-14 | 河北大学 | Near infrared core-shell structure quantum dot CuInS 2 Method for synthesizing ZnS |
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| WO2017067451A1 (en) | 2017-04-27 |
| CN105219380B (en) | 2018-01-23 |
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