CN103589427B - 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 a kind of preparation method 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 tunable, preparation technology are simple, and compared with common binary fluorescence quantum, not containing poisonous and harmful element, biocompatibility, toxicity, be 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 the active demand of widening that its Application Areas has become synthesis quanta point material.For solving the problem, the people such as Xie for presoma, select Dodecyl Mercaptan to be the activity of part controls Cu presoma with neutralized verdigris, indium acetate, synthesize that to obtain quantum yield be CuInS less than 3%
2quantum dot, and further quantum yield is brought up to 30%(R.Xie, M.Rutherford, X.Peng., J.Am.Chem.Soc., 2009,131,5691-5697 by coated ZnS shell material).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 improve preparation technology, nucleocapsid structure is abandoned on the basis ensureing quantum yield, nanocrystalline (the J.Zhang of zinc blende-type Cu-Zn-In-S quad alloy has been synthesized by doping of Zn element, R.Xie, W.Yang, Chem.Mater., 2011,23,3357-3361), positively charged ion presoma used is similarly acetate.
Although adopt the quantum dot fluorescence better performances that aforesaid method is prepared, but they also come with some shortcomings: first, the presoma of current synthesis Cu-Zn-In-S quantum dot mostly is the isometric chain molecule of acetate, backbone sterically hindered comparatively large, activity is lower, the rate of diffusion of Cu ion can be reduced, be unfavorable for crystallization, the quantum dot obtained only possesses a kind of crystal formation usually; The second, the quantum dot of synthesis is stored in the high toxicity solvent such as toluene, chloroform usually, which increases difficulty quantum dot being applied to the devices such as LED, limits it and further develops; 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, the muriate that we choose active high, nucleation and fast, the economic environmental protection of growth velocity is the Cu-Zn-In-S quantum dot of precursor synthesis three kinds of different crystal forms, and be dispersed in stable performance, not volatile, the nontoxic LED joint sealant had no irritating odor, prepare a kind of novel C u-Zn-In-S quantum dot light emitting film through thermofixation process.
Summary of the invention
Problem to be solved by this invention to overcome the deficiencies in the prior art, the preparation method of the high-performance Cu-Zn-In-S quantum dot luminescent thin film providing a kind of crystal formation controlled, obtained Cu-Zn-In-S quantum dot luminescent thin film fluorescence spectrum is adjustable, have the fluorescence property of Cu-Zn-In-S quantum dot excellence and the good machining property of organosilicon AB glue concurrently, and preparation process environmental protection, preparation method is simple, is expected to be applied to solid-state illumination LED further.
The present invention solves the problems of the technologies described above technical scheme used:
A kind of Cu-Zn-In-S quantum dot luminescent thin film preparation method, comprises the steps:
(1) cuprous chloride, indium chloride, zinc salt and block agent, surface capping agents are joined in the reaction vessel that nonpolar high boiling organic solvent is housed obtain Cu, In, Zn mixing precursor solution, pass into the air in nitrogen or rare gas element eliminating reaction vessel, under stirring, Cu, In, Zn mixing precursor solution is heated to 170 ~ 200 DEG C from room temperature, until form clear transparent solutions; Cu in described Cu, In, Zn mixing precursor solution
+concentration is 0.002 ~ 0.02M, and Surface coating agent 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 transparent solutions that step (1) obtains, make S and Cu
+molar ratio be 4 ~ 42:1, adjustment temperature to 150 ~ 220 DEG C, 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) obtained Cu-Zn-In-S quantum dot is mixed with the component A of LED joint sealant, heat 0.5 ~ 1h at 68 ~ 90 DEG C, obtain mixture;
(5) the mixture Homogeneous phase mixing will obtained in the B component of LED joint sealant and step (4), removes bubble, then is applied on a glass substrate by the product mixed, and at room temperature solidifies 19 ~ 29h, obtains Cu-Zn-In-S quantum dot luminescent thin 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), Cu-Zn-In-S quantum dot concentration in mixture is made to be 0.0001 ~ 0.02mol/L
LED joint sealant of the present invention is the commercially available LED special-purpose organic silicon type joint sealant being divided into A, B component to pack.In described preparation process, the B component of LED joint sealant and the volume ratio that feeds intake of component A are 0.98:10 ~ 1.02:10.
The inventive method can obtain 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 compares chalcopyrite and the more difficult acquisition of zincblende lattce structure, and the present invention is by changing Cu
+: Zn
2+molar ratio can facilitate the quantum dot of acquisition three kinds of different crystal forms, and this quantum dot fluorescence quantum yield is 26% ~ 46%, and the fluorescence emission spectrum of light-emitting film covers 400-800nm.Preferably, Cu is worked as
+: Zn
2+during for 1:4 ~ 6, product is wurtzite structure, and quantum yield reaches maximum simultaneously.
The Cu-Zn-In-S quantum dot luminescent thin 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 the need to preparing nucleocapsid structure, and pre-treatment need not be carried out to presoma, but the cuprous chloride of cheapness, indium chloride, zinc salt are simply mixed, itself and alkyl sulfhydryl are reacted.Synthesis device is simple, easy to operate, and synthesis temperature is gentleer, is a kind of technique of low temperature low cost, easily realizes scale operation;
2. the present invention take high activity chloride as positively charged ion presoma, can be obtained the Cu-Zn-In-S fluorescence quantum (wurtzite structure, zincblende lattce structure and yellow copper structure) of three kinds of crystal formations by the ratio changing copper source/zinc source;
3. the Cu-Zn-In-S quantum dot in the present invention is fixed on the nontoxic organic silicon type joint sealant substrate that has no irritating odor but not in the volatile hypertoxicity solution such as toluene, chloroform, the Cu-Zn-In-S quantum dot luminescent thin film obtained has Cu-Zn-In-S quantum dot fluorescence superior performance and the good advantage of organosilicon substrate machining property concurrently, different shape can be made according to product requirement, thus can be applied to photodiode, solid-state illumination white light LEDs etc. further.
Accompanying drawing explanation
Fig. 1: (a) is the XRD spectra of Cu-Zn-In-S quantum dot made in embodiment 1, (b) is the XRD spectra of Cu-Zn-In-S quantum dot made in embodiment 2, and (c) is the XRD spectra of Cu-Zn-In-S quantum dot made in embodiment 3.
Fig. 2: the fluorescence emission spectrum schematic diagram of Cu-Zn-In-S quantum dot luminescent thin film made in embodiment 1.
Fig. 3: the fluorescence emission spectrum schematic diagram of Cu-Zn-In-S quantum dot luminescent thin film made in embodiment 2.
Fig. 4: the fluorescence emission spectrum schematic diagram of Cu-Zn-In-S quantum dot luminescent thin film made in embodiment 3.
Embodiment
Implement to be described in further detail the present invention below in conjunction with accompanying drawing.The present embodiment is implemented under premised on technical solution of the present invention, gives detailed embodiment and process, is 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 DEG C makes CuCl, ZnCl
2and InCl
3dissolve completely, form clear transparent solutions, in solution, now inject 4mL sulphur powder-oleyl amine solution (sulphur powder concentration is 0.2mol/L), adjustment temperature to 160 DEG C, maintains this temperature, makes reaction carry out 90min, prepare Cu-Zn-In-S quantum dot solution.
3rd step, removes thermal source and naturally cools to room temperature, gets 0.5mlCu-Zn-In-S quantum dot stoste, adds 4ml dehydrated alcohol, carries out centrifugal purification process to Cu-Zn-In-S quantum dot stoste.
4th step, in being produced with 9ml Nanjing Zhong Bei Electronics Co., Ltd. by the Cu-Zn-In-S quantum dot after purification, uncommon board ZB3118 organic silicon type joint sealant component A mixes, and puts into water-bath 90 DEG C heating 1h;
5th step, mixes 0.9ml organic silicon type joint sealant B component with the dissolution homogeneity obtained in the 4th step, removes bubble, and by the coating of Cu-Zn-In-S quantum dot-AB glue mixture on a glass substrate (25.4 × 76.2mm), ambient temperature curing 24h.
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 fluorescence emission wavelengths 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 DEG C makes CuCl, ZnCl
2and InCl
3dissolve completely, form clear transparent solutions, in solution, now inject 4mL sulphur powder-oleyl amine solution (sulphur powder concentration is 0.2mol/L), adjustment temperature to 170 DEG C, maintains this temperature, makes reaction carry out 90min, prepare Cu-Zn-In-S quantum dot solution.
3rd step, removes thermal source and naturally cools to room temperature, gets 0.5mlCu-Zn-In-S quantum dot stoste, adds 4ml dehydrated alcohol, carries out centrifugal purification process to Cu-Zn-In-S quantum dot stoste.
4th step, in being produced with 9ml Nanjing Zhong Bei Electronics Co., Ltd. by the Cu-Zn-In-S quantum dot after purification, uncommon board ZB3118 organic silicon type joint sealant component A mixes, and puts into water-bath 90 DEG C heating 1h;
5th step, mixes 0.9ml organic silicon type joint sealant B component with the dissolution homogeneity obtained in the 4th step, removes bubble, and by the coating of Cu-Zn-In-S quantum dot-AB glue mixture on a glass substrate (25.4 × 76.2mm), ambient temperature curing 24h.
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 fluorescence emission wavelengths 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 DEG C makes CuCl, ZnCl
2and InCl
3dissolve completely, form clear transparent solutions, in solution, now inject 4mL sulphur powder-oleyl amine solution (sulphur powder concentration is 0.2mol/L), adjustment temperature to 220 DEG C, maintains this temperature, makes reaction carry out 90min, prepare Cu-Zn-In-S quantum dot solution.
3rd step, removes thermal source and naturally cools to room temperature, gets 0.5mlCu-Zn-In-S quantum dot stoste, adds dehydrated alcohol, carries out centrifugal purification process to Cu-Zn-In-S quantum dot stoste.
4th step, in being produced with 9ml Nanjing Zhong Bei Electronics Co., Ltd. by the Cu-Zn-In-S quantum dot after purification, uncommon board ZB3118 organic silicon type joint sealant component A mixes, and puts into water-bath 90 DEG C heating 1h;
5th step, mixes 0.9ml organic silicon type joint sealant B component with the dissolution homogeneity obtained in the 4th step, removes bubble, and by the coating of Cu-Zn-In-S quantum dot-AB glue mixture on a glass substrate (25.4 × 76.2mm), ambient temperature curing 24h.
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 fluorescence emission wavelengths 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 DEG C makes CuCl, ZnCl
2and InCl
3dissolve completely, form clear transparent solutions, in solution, now inject 4mL sulphur powder-oleyl amine solution (sulphur powder concentration is 0.2mol/L), adjustment temperature to 160 DEG C, maintains this temperature, makes reaction carry out 90min, prepare Cu-Zn-In-S quantum dot solution.
3rd step, removes thermal source and naturally cools to room temperature, gets 0.5mlCu-Zn-In-S quantum dot stoste, adds 4ml dehydrated alcohol, carries out centrifugal purification process to Cu-Zn-In-S quantum dot stoste.
4th step, in being produced with 9ml Nanjing Zhong Bei Electronics Co., Ltd. by the Cu-Zn-In-S quantum dot after purification, uncommon board ZB3118 organic silicon type joint sealant component A mixes, and puts into water-bath 90 DEG C heating 1h;
5th step, mixes 0.9ml organic silicon type joint sealant B component with the dissolution homogeneity obtained in the 4th step, removes bubble, and by the coating of Cu-Zn-In-S quantum dot-AB glue mixture on a glass substrate (25.4 × 76.2mm), ambient temperature curing 24h.
The Cu-Zn-In-S quantum dot obtained is wurtzite structure, and Cu-Zn-In-S quantum dot fluorescence quantum yield is 40%, and the fluorescence emission wavelengths 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 DEG C makes CuCl, ZnCl
2and InCl
3dissolve completely, form clear transparent solutions, in solution, now inject 4mL sulphur powder-oleyl amine solution (sulphur powder concentration is 0.2mol/L), adjustment temperature to 160 DEG C, maintains this temperature, makes reaction carry out 90min, prepare Cu-Zn-In-S quantum dot solution.
3rd step, removes thermal source and naturally cools to room temperature, gets 0.5mlCu-Zn-In-S quantum dot stoste, adds 4ml dehydrated alcohol, carries out centrifugal purification process to Cu-Zn-In-S quantum dot stoste.
4th step, in being produced with 9ml Nanjing Zhong Bei Electronics Co., Ltd. by the Cu-Zn-In-S quantum dot after purification, uncommon board ZB3118 organic silicon type joint sealant component A mixes, and puts into water-bath 90 DEG C heating 1h;
5th step, mixes 0.9ml organic silicon type joint sealant B component with the dissolution homogeneity obtained in the 4th step, removes bubble, and by the coating of Cu-Zn-In-S quantum dot-AB glue mixture on a glass substrate (25.4 × 76.2mm), ambient temperature curing 24h.
The Cu-Zn-In-S quantum dot obtained is wurtzite structure, and Cu-Zn-In-S quantum dot fluorescence quantum yield is 42%, and the fluorescence emission wavelengths of its light-emitting film is 643nm.
Claims (8)
1. a Cu-Zn-In-S quantum dot luminescent thin film preparation method, comprises the steps:
(1) cuprous chloride, indium chloride, zinc salt and block agent, surface capping agents are joined in the reaction vessel that nonpolar high boiling organic solvent is housed obtain Cu, In, Zn mixing precursor solution, pass into the air in nitrogen or rare gas element eliminating reaction vessel, under stirring, Cu, In, Zn mixing precursor solution is heated to 170 ~ 200 DEG C from room temperature, until form clear transparent solutions; Cu in described Cu, In, Zn mixing precursor solution
+concentration is 0.002 ~ 0.02M, and Surface coating agent concentration is 0.02 ~ 0.075M, and block agent concentration is 0.1 ~ 0.5M, Cu
+and Zn
2+, In
3+molar ratio be 1:4 ~ 21:1 ~ 11;
(2) the oleyl amine solution of sulphur is joined in the clear transparent solutions that step (1) obtains, make S and Cu
+molar ratio be 4 ~ 42:1, adjustment temperature to 150 ~ 220 DEG C, 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) obtained Cu-Zn-In-S quantum dot is mixed with the component A of LED joint sealant, heat 0.5 ~ 1h at 68 ~ 90 DEG C, obtain mixture;
(5) the mixture Homogeneous phase mixing will obtained in the B component of LED joint sealant and step (4), remove bubble, again the product mixed is applied on a glass substrate, at room temperature solidify 19 ~ 29h, obtain Cu-Zn-In-S quantum dot luminescent thin film.
2. Cu-Zn-In-S quantum dot luminescent thin film preparation method 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 luminescent thin film preparation method as claimed in claim 1 or 2, is characterized in that: in described step (1), molar ratio Cu
+: Zn
2+for 1:4 ~ 6.
4. Cu-Zn-In-S quantum dot luminescent thin film preparation method 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 luminescent thin film preparation method 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 luminescent thin film preparation method 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 being divided into A, B component to pack.
7. Cu-Zn-In-S quantum dot luminescent thin film preparation method as claimed in claim 1 or 2, is characterized in that: in described step (4), makes Cu-Zn-In-S quantum dot concentration in mixture be 0.0001 ~ 0.02mol/L.
8. Cu-Zn-In-S quantum dot luminescent thin film preparation method as claimed in claim 7, it is characterized in that: in described step (5), the B component of LED joint sealant and the volume ratio that feeds intake of component A are 0.98 ~ 1.02:10.
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| CN105255479B (en) * | 2015-09-28 | 2017-06-20 | 上海皇广光电科技有限公司 | A kind of Colloidal Quantum Dots fluorescent material preparation method of composite film |
| EP3162874A1 (en) | 2015-11-02 | 2017-05-03 | ETH Zurich | Luminescent semiconductor nanocrystals and methods for making same |
| CN106318374B (en) * | 2016-08-17 | 2019-03-05 | 安徽大学 | A kind of preparation method of multi layered quantum dots core-silica shell composite structure and its application in the led |
| CN106833610B (en) * | 2017-01-20 | 2020-04-10 | 深圳天吉新创科技有限公司 | Core-shell structure quantum dot and preparation method thereof |
| 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 |
| CN110511747A (en) * | 2019-09-19 | 2019-11-29 | 青岛大学 | A kind of gradient Zn-Cu-In-S core-shell quanta dots material and preparation method thereof |
| CN111233902A (en) * | 2020-03-06 | 2020-06-05 | 浙江农林大学暨阳学院 | Rare earth europium complex for near ultraviolet white light LED, red light LED device, white light fluorescent powder and white light LED device |
| CN112898966A (en) * | 2021-01-22 | 2021-06-04 | 电子科技大学长三角研究院(湖州) | Copper-zinc-indium-sulfur quantum dot, photo-anode, photoelectrochemical cell and preparation method |
| 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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