CN103589427A - Preparation method of Cu-Zn-In-S quantum dot luminescent thin film - Google Patents
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Abstract
The invention discloses a preparation method of a Cu-Zn-In-S quantum dot luminescent thin film. The preparation method comprises the following steps: (1) adding cuprous chloride, indium chloride, zinc salt, a capping agent and a surface coating agent to a non-polar high boiling point organic solvent so as to obtain a Cu, In and Zn mixed precursor solution, stirring and heating under the atmosphere of nitrogen or inert gas so as to form a clear transparent solution; (2) adding an oleylamine solution of sulfur to the clear transparent solution obtained in the step (1), and heating for reacting so as to prepare a Cu-Zn-In-S quantum dot solution; (3) separating so as to obtain Cu-Zn-In-S quantum dots; (4) mixing the prepared Cu-Zn-In-S quantum dots with a component A of an LED (Light Emitting Diode) pouring sealant; (5) uniformly mixing a component B of the LED pouring sealant with a mixture obtained in the step (4), removing air bubbles, then coating a product on a glass substrate, and curing at a room temperature so as to obtain the Cu-Zn-In-S quantum dot luminescent thin film. The fluorescence spectra of the Cu-Zn-In-S quantum dot luminescent thin film prepared by the method can be adjusted. The Cu-Zn-In-S quantum dot luminescent thin film has the excellent fluorescence property of the Cu-Zn-In-S quantum dots and the good machining property of an organic silicon adhesive AB.
Description
Technical field
The present invention relates to novel fluorescent material technical field, be specially the preparation method of a kind of copper zinc indium sulphur (Cu-Zn-In-S) quantum dot light emitting film.
Background technology
As novel fluorescence nanocrystalline (nanocrystal also claims quantum dot), copper indium sulphur (CuInS
2) nanocrystal has the advantages such as luminous intensity is high, wavelength is adjustable, preparation technology is simple, and compare with common binary fluorescence quantum,, containing poisonous and harmful element, biocompatibility, toxicity, be not all better than binary fluorescence quantum, has broad application prospects.Prepare that light emitting region is wide, glow peak position is adjustable, quantum yield (QY) is high, the CuInS of stable performance
2quantum dot, and widen the active demand that its Application Areas has become synthetic quanta point material.For addressing the above problem, it is presoma that the people such as Xie be take neutralized verdigris, indium acetate, and selecting Dodecyl Mercaptan is the activity that part is controlled Cu presoma, syntheticly obtains the CuInS that quantum yield is less than 3%
2quantum dot, and further quantum yield is brought up to 30%(R.Xie by coated ZnS shell material, M.Rutherford, X.Peng., J.Am.Chem.Soc., 2009,131,5691-5697).Although nucleocapsid structure can significantly improve quantum yield, but its synthesis technique is comparatively loaded down with trivial details, and the people such as Zhang have improved preparation technology, on the basis that guarantees quantum yield, abandon nucleocapsid structure, by doping of Zn element, synthesized the nanocrystalline (J.Zhang of zink sulphide type Cu-Zn-In-S quad alloy, R.Xie, W.Yang, Chem.Mater., 2011,23,3357-3361), positively charged ion presoma used is similarly acetate.
Although the quantum dot fluorescence better performances that adopts aforesaid method to prepare, but they also come with some shortcomings: first, the presoma of at present synthetic Cu-Zn-In-S quantum dot mostly is the isometric chain molecule of acetate, backbone sterically hindered large, activity is lower, can reduce the rate of diffusion of Cu ion, be unfavorable for crystallization, the quantum dot obtaining only possesses a kind of crystal formation conventionally; The second, synthetic quantum dot is stored in the high toxicity solvent such as toluene, chloroform conventionally, and this has increased the difficulty that quantum dot is applied to the devices such as LED, has limited it to further develop; The 3rd, toluene, chloroform equal solvent highly volatile, the volatilization of solvent can cause the reunion of quantum dot, and its fluorescence property is significantly decayed.On the basis of existing open report, we choose active high, nucleation and growth velocity is fast, the muriate of the economic environmental protection Cu-Zn-In-S quantum dot of three kinds of different crystal forms that has been precursor synthesis, and be dispersed in stable performance, not volatile, the nontoxic LED joint sealant having no irritating odor, through thermofixation, process and prepare a kind of novel C u-Zn-In-S quantum dot light emitting film.
Summary of the invention
Problem to be solved by this invention is to overcome the deficiencies in the prior art, the preparation method of the controlled high-performance Cu-Zn-In-S quantum dot light emitting film of a kind of crystal formation is provided, the Cu-Zn-In-S quantum dot light emitting film fluorescence spectrum making is adjustable, have fluorescence property and the good machining property of organosilicon AB glue of Cu-Zn-In-S quantum dot excellence concurrently, and preparation process environmental protection, preparation method is simple, is expected to be further applied to solid-state illumination LED.
The present invention solves the problems of the technologies described above technical scheme used:
A quantum dot light emitting method for manufacturing thin film, comprises the steps:
(1) cuprous chloride, indium chloride, zinc salt and block agent, surperficial coating are joined and in the reaction vessel that nonpolar high boiling organic solvent is housed, obtain Cu, In, Zn mixing precursor solution, pass into nitrogen or rare gas element and get rid of the air in reaction vessel, under stirring, Cu, In, Zn mixing precursor solution are heated to 170～200 ℃ from room temperature, until form clear solution; Cu in described Cu, In, Zn mixing precursor solution
+concentration is 0.002～0.02M, and surperficial coating concentration is 0.02～0.075M, and block agent concentration is 0.1～0.5M, Cu
+and Zn
2+, In
2+molar ratio be 1:4～21:1～11;
(2) the oleyl amine solution of sulphur is joined in the clear solution of step (1) acquisition, make S and Cu
+molar ratio be 4～42:1, adjust temperature to 150～220 ℃, maintain this temperature, make reaction carry out 30～120min, prepare Cu-Zn-In-S quantum dot solution;
(3) Cu-Zn-In-S quantum dot solution is naturally cooled to room temperature, add polar solvent, centrifugal purification obtains Cu-Zn-In-S quantum dot;
(4) the Cu-Zn-In-S quantum dot making is mixed with the A component of LED joint sealant, heat 0.5～1h at 68～90 ℃, obtain mixture;
(5) the B component of LED joint sealant is evenly mixed with the mixture obtaining in step (4), remove bubble, then the product mixing is coated on glass substrate, at room temperature solidify 19～29h, obtain Cu-Zn-In-S quantum dot light emitting film.
In described step (1), using cuprous chloride (CuCl) as copper source, with indium chloride (InCl
3) as indium source, using zinc salt as zinc source, the preferred zinc chloride (ZnCl of described zinc salt
2) or Zinic stearas (Zn(St)
2), the preferred oleic acid of described coating, described block agent preferred alkyl mercaptan, as Dodecyl Mercaptan, the described preferred octadecylene of nonpolar high boiling organic solvent or octadecane.The preferred argon gas of described rare gas element.
In described step (2), in the oleyl amine solution of sulphur, sulphur concentration is 0.1～0.4mol/L.
In described step (3), polar solvent can be methyl alcohol, ethanol, acetone etc.
In described step (4), making Cu-Zn-In-S quantum dot concentration in mixture is 0.0001～0.02mol/L
LED joint sealant of the present invention is the commercially available LED special-purpose organic silicon type joint sealant that is divided into A, B component packing.In described preparation process, the volume ratio that feeds intake of the B component of LED joint sealant and A component is 0.98:10～1.02:10.
The inventive method can make three kinds of different crystal forms Cu-Zn-In-S quantum dots (wurtzite structure, zincblende lattce structure and yellow copper structure), and according to bibliographical information, wurtzite structure is compared chalcopyrite and the more difficult acquisition of zincblende lattce structure, and the present invention is by changing Cu
+: Zn
2+molar ratio can conveniently obtain the quantum dot of three kinds of different crystal forms, and this quantum dot fluorescence quantum yield is 26%～46%, the fluorescence emission spectrum of light-emitting film covers 400-800nm.Preferably, work as Cu
+: Zn
2+for 1:4～6 o'clock, product is wurtzite structure, and quantum yield reaches maximum simultaneously.
The Cu-Zn-In-S quantum dot light emitting film that preparation method of the present invention obtains can be applied to photodiode, solid-state illumination white light LEDs etc.
Compared with prior art, the present invention has following beneficial effect:
1. when the present invention synthesizes quantum dot, without preparing nucleocapsid structure, and need not carry out pre-treatment to presoma, but cheap cuprous chloride, indium chloride, zinc salt are simply mixed, it is reacted with alkyl sulfhydryl.Synthesis device is simple, easy to operate, and synthesis temperature is gentleer, is a kind of low temperature technique cheaply, easily realizes scale operation;
2. the present invention be take high activity chloride as positively charged ion presoma, can obtain the Cu-Zn-In-S fluorescence quantum (wurtzite structure, zincblende lattce structure and yellow copper structure) of three kinds of crystal formations by changing the ratio in /Xin source, copper source;
3. the Cu-Zn-In-S quantum dot in the present invention is fixed on the nontoxic organosilicon type joint sealant substrate having no irritating odor but not in the volatile hypertoxicity solution such as toluene, chloroform, the Cu-Zn-In-S quantum dot light emitting film obtaining has Cu-Zn-In-S quantum dot fluorescence superior performance and the good advantage of organosilicon substrate machining property concurrently, can make different shape according to product requirement, thereby can be further applied to photodiode, solid-state illumination white light LEDs etc.
Accompanying drawing explanation
Fig. 1: (a) being the XRD spectra of Cu-Zn-In-S quantum dot made in embodiment 1, is (b) XRD spectra of Cu-Zn-In-S quantum dot made in embodiment 2 is (c) XRD spectra of Cu-Zn-In-S quantum dot made in embodiment 3.
The fluorescence emission spectrum schematic diagram of made Cu-Zn-In-S quantum dot light emitting film in Fig. 2: embodiment 1.
The fluorescence emission spectrum schematic diagram of made Cu-Zn-In-S quantum dot light emitting film in Fig. 3: embodiment 2.
The fluorescence emission spectrum schematic diagram of made Cu-Zn-In-S quantum dot light emitting film in Fig. 4: embodiment 3.
Embodiment
Below in conjunction with accompanying drawing, implement the present invention to be described in further detail.The present embodiment is implemented take technical solution of the present invention under prerequisite, has provided detailed embodiment and process, be to further illustrate of the present invention, but the present invention should be not limited to the content that following instance is specifically expressed.
Embodiment 1
The first step, takes 3.96mg(0.04mmol) CuCl, 27.26mg(0.2mmol) ZnCl
2, 44.24mg(0.2mmol) InCl
3be placed in a three-necked bottle, and add 0.2mmol oleic acid, 2mmol Dodecyl Mercaptan, 8ml octadecylene.
Second step, under the condition of magnetic agitation and argon shield, heating mixing solutions to 180 ℃ makes CuCl, ZnCl
2and InCl
3dissolve completely, form clear solution, now in solution, inject 4mL sulphur powder-oleyl amine solution (sulphur powder concentration is 0.2mol/L), adjust temperature to 160 ℃, maintain this temperature, make reaction carry out 90min, prepare Cu-Zn-In-S quantum dot solution.
The 3rd step, removes thermal source and naturally cools to room temperature, gets 0.5mlCu-Zn-In-S quantum dot stoste, adds 4ml dehydrated alcohol, and Cu-Zn-In-S quantum dot stoste is carried out to centrifugal purification processing.
The 4th step, during the Cu-Zn-In-S quantum dot after purifying is produced with 9ml Nanjing Zhong Bei Electronics Co., Ltd., uncommon board ZB3118 organosilicon type joint sealant A component is mixed, and puts into 90 ℃ of heating 1h of water-bath;
The 5th step, evenly mixes 0.9ml organosilicon type joint sealant B component with the solution obtaining in the 4th step, removes bubble, and Cu-Zn-In-S quantum dot-AB glue mixture is coated in to (25.4 * 76.2mm) on glass substrate, solidifies 24h under normal temperature.
As shown in Fig. 1 (a), the Cu-Zn-In-S quantum dot of acquisition is wurtzite structure.
As shown in Figure 2, the Cu-Zn-In-S quantum dot fluorescence quantum yield of acquisition is 46%, and the fluorescent emission wavelength of its light-emitting film is 663nm.
Embodiment 2
The first step, takes 2.48mg(0.025mmol) CuCl, 51.11mg(0.375mmol) ZnCl
2, 44.24mg(0.2mmol) InCl
3be placed in a three-necked bottle, and add 0.2mmol oleic acid, 2mmol Dodecyl Mercaptan, 8ml octadecylene.
Second step, under the condition of magnetic agitation and argon shield, heating mixing solutions to 190 ℃ makes CuCl, ZnCl
2and InCl
3dissolve completely, form clear solution, now in solution, inject 4mL sulphur powder-oleyl amine solution (sulphur powder concentration is 0.2mol/L), adjust temperature to 170 ℃, maintain this temperature, make reaction carry out 90min, prepare Cu-Zn-In-S quantum dot solution.
The 3rd step, removes thermal source and naturally cools to room temperature, gets 0.5mlCu-Zn-In-S quantum dot stoste, adds 4ml dehydrated alcohol, and Cu-Zn-In-S quantum dot stoste is carried out to centrifugal purification processing.
The 4th step, during the Cu-Zn-In-S quantum dot after purifying is produced with 9ml Nanjing Zhong Bei Electronics Co., Ltd., uncommon board ZB3118 organosilicon type joint sealant A component is mixed, and puts into 90 ℃ of heating 1h of water-bath;
The 5th step, evenly mixes 0.9ml organosilicon type joint sealant B component with the solution obtaining in the 4th step, removes bubble, and Cu-Zn-In-S quantum dot-AB glue mixture is coated in to (25.4 * 76.2mm) on glass substrate, solidifies 24h under normal temperature.
As shown in Fig. 1 (b), the Cu-Zn-In-S quantum dot of acquisition is yellow copper structure.
As shown in Figure 3, the Cu-Zn-In-S quantum dot fluorescence quantum yield of acquisition is 39%, and the fluorescent emission wavelength of its light-emitting film is 590nm.
Embodiment 3
The first step, takes 1.89mg(0.019mmol) CuCl, 240.89mg(0.381mmol) Zn(St)
2, 44.24mg(0.2mmol) InCl
3be placed in a three-necked bottle, and add 0.2mmol oleic acid, 2mmol Dodecyl Mercaptan, 8ml octadecylene.
Second step, under the condition of magnetic agitation and argon shield, heating mixing solutions to 200 ℃ makes CuCl, ZnCl
2and InCl
3dissolve completely, form clear solution, now in solution, inject 4mL sulphur powder-oleyl amine solution (sulphur powder concentration is 0.2mol/L), adjust temperature to 220 ℃, maintain this temperature, make reaction carry out 90min, prepare Cu-Zn-In-S quantum dot solution.
The 3rd step, removes thermal source and naturally cools to room temperature, gets 0.5mlCu-Zn-In-S quantum dot stoste, adds dehydrated alcohol, and Cu-Zn-In-S quantum dot stoste is carried out to centrifugal purification processing.
The 4th step, during the Cu-Zn-In-S quantum dot after purifying is produced with 9ml Nanjing Zhong Bei Electronics Co., Ltd., uncommon board ZB3118 organosilicon type joint sealant A component is mixed, and puts into 90 ℃ of heating 1h of water-bath;
The 5th step, evenly mixes 0.9ml organosilicon type joint sealant B component with the solution obtaining in the 4th step, removes bubble, and Cu-Zn-In-S quantum dot-AB glue mixture is coated in to (25.4 * 76.2mm) on glass substrate, solidifies 24h under normal temperature.
As shown in Fig. 1 (c), the Cu-Zn-In-S quantum dot of acquisition is zincblende lattce structure.
As shown in Figure 4, the Cu-Zn-In-S quantum dot fluorescence quantum yield of acquisition is 26%, and the fluorescent emission wavelength of its light-emitting film is 526nm.
Embodiment 4
The first step, takes 7.92mg(0.08mmol) CuCl, 43.62mg(0.32mmol) ZnCl
2, 44.24mg(0.2mmol) InCl
3be placed in a three-necked bottle, and add 0.2mmol oleic acid, 2mmol Dodecyl Mercaptan, 8ml octadecylene.
Second step, under the condition of magnetic agitation and argon shield, heating mixing solutions to 180 ℃ makes CuCl, ZnCl
2and InCl
3dissolve completely, form clear solution, now in solution, inject 4mL sulphur powder-oleyl amine solution (sulphur powder concentration is 0.2mol/L), adjust temperature to 160 ℃, maintain this temperature, make reaction carry out 90min, prepare Cu-Zn-In-S quantum dot solution.
The 3rd step, removes thermal source and naturally cools to room temperature, gets 0.5mlCu-Zn-In-S quantum dot stoste, adds 4ml dehydrated alcohol, and Cu-Zn-In-S quantum dot stoste is carried out to centrifugal purification processing.
The 4th step, during the Cu-Zn-In-S quantum dot after purifying is produced with 9ml Nanjing Zhong Bei Electronics Co., Ltd., uncommon board ZB3118 organosilicon type joint sealant A component is mixed, and puts into 90 ℃ of heating 1h of water-bath;
The 5th step, evenly mixes 0.9ml organosilicon type joint sealant B component with the solution obtaining in the 4th step, removes bubble, and Cu-Zn-In-S quantum dot-AB glue mixture is coated in to (25.4 * 76.2mm) on glass substrate, solidifies 24h under normal temperature.
The Cu-Zn-In-S quantum dot obtaining is wurtzite structure, and Cu-Zn-In-S quantum dot fluorescence quantum yield is 40%, and the fluorescent emission wavelength of its light-emitting film is 674nm.
Embodiment 5
The first step, takes 5.64mg(0.057mmol) CuCl, 46.75mg(0.343mmol) ZnCl
2, 44.24mg(0.2mmol) InCl
3be placed in a three-necked bottle, and add 0.2mmol oleic acid, 2mmol Dodecyl Mercaptan, 8ml octadecylene.
Second step, under the condition of magnetic agitation and argon shield, heating mixing solutions to 180 ℃ makes CuCl, ZnCl
2and InCl
3dissolve completely, form clear solution, now in solution, inject 4mL sulphur powder-oleyl amine solution (sulphur powder concentration is 0.2mol/L), adjust temperature to 160 ℃, maintain this temperature, make reaction carry out 90min, prepare Cu-Zn-In-S quantum dot solution.
The 3rd step, removes thermal source and naturally cools to room temperature, gets 0.5mlCu-Zn-In-S quantum dot stoste, adds 4ml dehydrated alcohol, and Cu-Zn-In-S quantum dot stoste is carried out to centrifugal purification processing.
The 4th step, during the Cu-Zn-In-S quantum dot after purifying is produced with 9ml Nanjing Zhong Bei Electronics Co., Ltd., uncommon board ZB3118 organosilicon type joint sealant A component is mixed, and puts into 90 ℃ of heating 1h of water-bath;
The 5th step, evenly mixes 0.9ml organosilicon type joint sealant B component with the solution obtaining in the 4th step, removes bubble, and Cu-Zn-In-S quantum dot-AB glue mixture is coated in to (25.4 * 76.2mm) on glass substrate, solidifies 24h under normal temperature.
The Cu-Zn-In-S quantum dot obtaining is wurtzite structure, and Cu-Zn-In-S quantum dot fluorescence quantum yield is 42%, and the fluorescent emission wavelength of its light-emitting film is 643nm.
Claims (8)
1. a Cu-Zn-In-S quantum dot light emitting method for manufacturing thin film, comprises the steps:
(1) cuprous chloride, indium chloride, zinc salt and block agent, surperficial coating are joined and in the reaction vessel that nonpolar high boiling organic solvent is housed, obtain Cu, In, Zn mixing precursor solution, pass into nitrogen or rare gas element and get rid of the air in reaction vessel, under stirring, Cu, In, Zn mixing precursor solution are heated to 170～200 ℃ from room temperature, until form clear solution; Cu in described Cu, In, Zn mixing precursor solution
+concentration is 0.002～0.02M, and surperficial coating concentration is 0.02～0.075M, and block agent concentration is 0.1～0.5M, Cu
+and Zn
2+, In
2+molar ratio be 1:4～21:1～11;
(2) the oleyl amine solution of sulphur is joined in the clear solution of step (1) acquisition, make S and Cu
+molar ratio be 4～42:1, adjust temperature to 150～220 ℃, maintain this temperature, make reaction carry out 30～120min, prepare Cu-Zn-In-S quantum dot solution;
(3) Cu-Zn-In-S quantum dot solution is naturally cooled to room temperature, add polar solvent, centrifugal purification obtains Cu-Zn-In-S quantum dot;
(4) the Cu-Zn-In-S quantum dot making is mixed with the A component of LED joint sealant, heat 0.5～1h at 68～90 ℃, obtain mixture;
(5) the B component of LED joint sealant is evenly mixed with the mixture obtaining in step (4), remove bubble, then the product mixing is coated on glass substrate, at room temperature solidify 19～29h, obtain Cu-Zn-In-S quantum dot light emitting film.
2. Cu-Zn-In-S quantum dot light emitting method for manufacturing thin film as claimed in claim 1, it is characterized in that: in described step (1), described zinc salt is zinc chloride or Zinic stearas, described coating is oleic acid, described block agent is alkyl sulfhydryl, and described nonpolar high boiling organic solvent is octadecylene or octadecane.
3. Cu-Zn-In-S quantum dot light emitting method for manufacturing thin film as claimed in claim 1 or 2, is characterized in that: in described step (1), and molar ratio Cu
+: Zn
2+for 1:4～6.
4. Cu-Zn-In-S quantum dot light emitting method for manufacturing thin film as claimed in claim 1 or 2, is characterized in that: in described step (2), in the oleyl amine solution of sulphur, sulphur concentration is 0.1～0.4mol/L.
5. Cu-Zn-In-S quantum dot light emitting method for manufacturing thin film as claimed in claim 1 or 2, is characterized in that: in described step (3), polar solvent is methyl alcohol, ethanol or acetone.
6. Cu-Zn-In-S quantum dot light emitting method for manufacturing thin film as claimed in claim 1 or 2, is characterized in that: described LED joint sealant is the LED special-purpose organic silicon type joint sealant that is divided into A, B component packing.
7. Cu-Zn-In-S quantum dot light emitting method for manufacturing thin film as claimed in claim 1 or 2, is characterized in that: in described step (4), making Cu-Zn-In-S quantum dot concentration in mixture is 0.0001～0.02mol/L.
8. Cu-Zn-In-S quantum dot light emitting method for manufacturing thin film as claimed in claim 7, is characterized in that: in described step (5), the volume ratio that feeds intake of the B component of LED joint sealant and A component is 0.98～1.02:10.
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| CN110212077A (en) * | 2019-06-13 | 2019-09-06 | 深圳扑浪创新科技有限公司 | A kind of method and its application improving quantum dot stability in the substrate |
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| CN115410829A (en) * | 2022-09-07 | 2022-11-29 | 电子科技大学长三角研究院(湖州) | Quantum dot sensitized oxide electrode and preparation method and application thereof |
| CN115410829B (en) * | 2022-09-07 | 2023-06-23 | 电子科技大学长三角研究院(湖州) | Quantum dot sensitized oxide electrode and preparation method and application thereof |
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