CN111682117B - Quantum dot preparation method, photosensitive material layer and photovoltaic device - Google Patents
Quantum dot preparation method, photosensitive material layer and photovoltaic device Download PDFInfo
- Publication number
- CN111682117B CN111682117B CN202010590364.5A CN202010590364A CN111682117B CN 111682117 B CN111682117 B CN 111682117B CN 202010590364 A CN202010590364 A CN 202010590364A CN 111682117 B CN111682117 B CN 111682117B
- Authority
- CN
- China
- Prior art keywords
- quantum dots
- solvent
- solution
- nucleation
- prepared
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
- H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/15—Deposition of organic active material using liquid deposition, e.g. spin coating characterised by the solvent used
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
Abstract
The invention provides a preparation method of quantum dots, a photosensitive material layer and a photovoltaic device, which comprises the following steps: dispersing a Grignard reagent and an anion precursor in a non-co-melting solvent to obtain a mixed solution; and heating the mixed solution to a temperature range of the solution during the nucleation reaction, injecting the solution of the metal halide into the mixed solution, performing the nucleation reaction, and cooling and purifying after the reaction to obtain the quantum dot. By utilizing the characteristic of rapid crystallization of heat injection, the quantum dot with better peak width and fewer defects can be effectively and rapidly prepared, and the obtained quantum dot has good stability and does not influence exciton diffusion. The photosensitive material layer of the photovoltaic device prepared by the quantum dots can effectively improve the charge conversion rate and the service life of the photovoltaic device.
Description
Technical Field
The invention relates to the technical field of quantum dot synthesis, in particular to a preparation method of quantum dots, a photosensitive material layer and a photovoltaic device.
Background
Quantum dots are the most potential nanomaterials, leading to technological trends. The development of the quantum dot synthesis technology is not kept away from one purpose no matter the synthesis method or the corresponding application, namely, the excellent performance of the quantum dot is improved to the greatest extent, such as: fluorescence intensity, half-width, stability, etc. of the quantum dots. The quantum dot has the characteristics of quantum limiting effect, size effect and the like, so that the quantum dot can be applied to various technical fields such as the display technical field, the solar cell field, the biological mark field, the sensing and detecting field and the like.
The field of quantum dot photovoltaic cells mainly utilizes the fact that quantum dots have a wide absorption band and a large exciton Bohr radius. The preparation method of the quantum dots (such as CdSe, pbS, cdTe and the like) is simple, but the stability of the prepared quantum dots is poor, and the effect of the relevant light Fu Guangfu device prepared by the quantum dots with poor stability is poor. Thus, the stability of the quantum dots becomes critical in the preparation of quantum dot batteries.
In the prior art, in order to obtain quantum dots with better stability, a method of growing a layer of inorganic shell layer with wide band gap outside the quantum dot core is mostly adopted. Although the stability of the quantum dots prepared by the method is improved, the absorption bandwidth of the quantum dots is reduced, and meanwhile, the diffusion free path of excitons is also reduced, so that the performance of the prepared photovoltaic device is affected.
In view of this, the present invention has been made.
Disclosure of Invention
According to the preparation method of the quantum dot, provided by the invention, the technical problems are solved, the Grignard reagent is utilized, the heat injection method is adopted, the solution of the metal halide is injected into the mixture obtained by mixing the Grignard reagent and the anion precursor, and the quantum dot with better peak width and fewer defects can be effectively and rapidly prepared by utilizing the characteristic of rapid crystallization of heat injection, so that the obtained quantum dot has good stability and does not influence exciton diffusion.
The photovoltaic device provided by the invention comprises the photosensitive material layer prepared by the quantum dots, so that the charge conversion rate of the photovoltaic device can be effectively improved.
In order to achieve the above object of the present invention, the following technical solutions are specifically adopted:
a preparation method of quantum dots comprises the following steps:
dispersing a Grignard reagent and an anion precursor in a non-co-melting solvent to obtain a mixed solution; and heating the mixed solution to a temperature range of the solution during the nucleation reaction, injecting the solution of the metal halide into the mixed solution, performing the nucleation reaction, and cooling and purifying after the reaction to obtain the quantum dot.
Wherein the grignard reagent is RMgX, wherein R is an alkanyl group; x is halogen element;
further, the halogen element X is selected from one of Cl, br, F or I, more preferably Cl or Br;
further, the alkane is CH 3 -(CH 2 ) n -wherein n has a value of any one of 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17 or 18;
further, the alkane group is (CH) 2 ) m -wherein m has a value of any one of 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17 or 18.
Further, the anion precursor comprises S-ODE, S-TOP, S-OA, se-TOP, S-OLA, S-TBP, se-TBP, te-ODE, te-OA, te-TOP, te-TBP, (TMS) 3 S sum (TMS) 3 At least one of P;
further, in the process of dispersing the Grignard reagent and the anion precursor in the non-co-molten solvent, the solution temperature is 25-200 ℃, the dispersing time is 5-120 min, and the dispersing operation is performed under the protection of inert atmosphere.
Further, the non-co-solvent comprises at least one of octadecene, paraffin oil, and diphenyl ether.
Further, the metal halide comprises ZnX 2 、PbX 2 、CdX 2 、HgX 2 Or InX 3 Wherein X is selected from one of Cl, br, F or I;
further, the metal halide solution is prepared by dispersing the metal halide in a non-co-solvent, more preferably, the dispersion is performed in a non-co-solvent process at a solution temperature of 25 to 200 ℃, the dispersion time is 5min to 2h, and the dispersion operation is performed under the protection of an inert atmosphere.
Further, the molar volume ratio of the metal halide, the grignard reagent, the anion precursor, and the non-co-solvent is (1-10 mmol): (1-10 mmol): 1mmol: (5-30 ml), more preferably (2-8 mmol): (2-8 mmol): 1mmol: (8-24 ml).
Further, the temperature of the solution at the time of the nucleation reaction is in the range of 60 to 320 ℃, more preferably 80 to 260 ℃.
Further, the nucleation reaction time is 1min to 2h, more preferably 20min to 80min;
further, the nucleation reaction is carried out under the protection of an inert atmosphere.
Further, the purification process specifically includes: adding a proper amount of precipitant into the mixed solution containing the quantum dots after the nucleation reaction, and performing centrifugal separation to obtain the quantum dots;
further, the precipitant consists of an organic ester solvent and a polar solvent; the volume ratio of the mixed solution containing the quantum dots, the organic ester solvent and the polar solvent is 1 (1-3): (0.5-1);
the organic ester solvent comprises at least one of ethyl acetate, propyl acetate, butyl ethyl acetate, butyl acetate, ethyl formate, ethyl propionate and methyl acetate;
the polar solvent includes at least one of ethanol, methanol, and isopropanol.
The photosensitive material layer is prepared from the quantum dots prepared by the preparation method of the quantum dots.
A photovoltaic device includes a cathode, a hole transport layer, a photoactive material layer, a charge transport layer, and an anode connected in sequence.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, by utilizing the characteristic of rapid crystallization of heat injection, the quantum dot with good peak width and fewer defects can be effectively and rapidly prepared, and the obtained quantum dot has good stability and does not influence exciton diffusion.
(2) The invention comprises the photosensitive material layer prepared by the quantum dots prepared by the method, and can effectively improve the charge conversion rate of the photovoltaic device.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic flow chart of a preparation method of quantum dots provided by the invention;
fig. 2 is a schematic cross-sectional structure of a photovoltaic device according to the present invention.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings and detailed description, but it will be understood by those skilled in the art that the examples described below are some, but not all, examples of the present invention, and are intended to be illustrative of the present invention only and should not be construed as limiting the scope of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
In the description of the present invention, it should be noted that the directions or positional relationships indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
The preparation method of the quantum dot provided by the invention has a flow chart shown in figure 1, and comprises the following steps:
dispersing the Grignard reagent and the anion precursor in a non-co-solvent (the Grignard reagent and the anion precursor can be mixed firstly and then dispersed in the non-co-solvent, or respectively dispersed in the non-co-solvent and then mixed) to finally obtain a mixed solution; heating the mixed solution to a temperature range of a solution required by nucleation, injecting a metal halide solution into the mixed solution, carrying out nucleation, cooling after reaction, and purifying to obtain the quantum dot.
The application utilizes a Grignard reagent (RMgX, wherein R is alkyl, X is halogen, X is one of Cl, br, F or I, preferably Cl or Br) and metal halide (including but not limited to CdX) 2 、ZnX 2 、PbX 2 、InX 3 Or HgX 2 Wherein X is selected from one of Cl, br, F or I) may react to generate an organometallic precursor, and the generated organometallic precursor may react with a corresponding anion precursor (including but not limited to at least one of S-ODE, S-TOP, se-TOP, S-OA, se-TBP, S-TBP, (TMS) 3P, te-OA, te-TOP, te-TBP, S-OLA, (TMS) 3S and Te-ODE) to generate quantum dots.
The reaction is as follows:
CdX 1 +RMgX 2 →CdR+MgX 1 X 2 (wherein X is 1 、X 2 Is halogen element, R is alkyl), and MgX is simultaneously generated 1 X 2 The halogen element in the fluorescent material can passivate the quantum dot, so that the stability of the quantum dot after the passivation of the halogen element is improved, and meanwhile, the diffusion of excitons is facilitated.
Wherein, the Grignard reagent (RMgX, wherein R is alkyl, X is halogen element) is a covalent compound, magnesium atom is directly connected with carbon to form a polar covalent bond, carbon is electronegative terminal, and metal Mg is presented to have higher activity; therefore, the Grignard reagent has stronger activity compared with the metal magnesium halide, and the halogen element in the Grignard reagent is easier to fall off compared with the same halogen element in the metal magnesium halide.
Wherein the alkyl is CH 3 -(CH 2 ) n -wherein n has a value of any one of 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17 or 18; alternatively, the alkyl group is (CH 2 ) m -m has a value of any one of 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17 or 18.
Further, in the process of dispersing the grignard reagent and the anion precursor in the non-co-solvent, the solution temperature is 25 ℃ to 200 ℃ and the dispersing time is 5min to 120min, and the dispersing operation is carried out in the inert gas atmosphere.
In particular embodiments of the present invention, the non-co-solvent includes, but is not limited to, at least one of octadecene, paraffinic oil, and diphenyl ether.
In a specific embodiment of the present invention, a metal halide solution is prepared by dispersing the metal halide in a non-co-solvent at a solution temperature of 25 ℃ to 200 ℃ (e.g., 25, 60, 80, 120, 180, 200 ℃) for a period of 5min to 120min, and the dispersing operation is performed under the protection of an inert atmosphere.
In a specific embodiment of the present invention, the molar volume ratio of the metal halide, the grignard reagent, the anion precursor and the non-co-solvent is (1-10) mmol: (1-10) mmol:1mmol: (5-30) ml; (e.g., (1:1:1) mmol:5ml, (10:1:10) mmol:30ml, (5:1:5) mmol:15ml, (10:1:1) mmol:20 ml) or (2-8) mmol: (2-8) mmol:1mmol: (8-24) ml.
In the embodiment of the present invention, the solution temperature is too high to form many by-products and too low to react, and thus the temperature of the solution at the time of the nucleation reaction is in the range of 60 to 320 c (e.g., 60, 100, 150, 200, 250, 300, 320 c), preferably 80 to 260 c.
In the specific embodiment of the invention, the quantum dots with corresponding wavelengths cannot be obtained after the reaction time is too short, the reaction time is too long, so that the prepared quantum dot cores are re-divided, the nucleation reaction time is controlled to be 1 min-120 min (for example, 1, 10, 30, 50, 60, 80, 90, 100 and 120 min), and the preferred nucleation time is 20 min-80 min; the nucleation is carried out under the protection of inert atmosphere.
In a specific embodiment of the present invention, the obtained quantum dots are subjected to further purification operation, and high-speed centrifugation is adopted to obtain the prepared quantum dots, specifically: adding a proper amount of precipitant into the mixed solution containing the quantum dots after the nucleation reaction, and performing centrifugal separation to obtain the quantum dots;
wherein the precipitant consists of an organic ester solvent and a polar solvent; the volume ratio of the mixed solution containing the quantum dots, the organic ester solvent and the polar solvent is 1 (1-3): (0.5-1).
Wherein the organic ester solvent includes, but is not limited to, at least one of ethyl acetate, methyl acetate, propyl acetate, butyl acetate, ethyl formate, ethyl propionate, and butyl ethyl propionate; the polar solvent includes, but is not limited to, at least one of ethanol, methanol, and isopropanol.
The photosensitive material layer is prepared from the quantum dots prepared by the preparation method of the quantum dots.
A schematic cross-sectional structure of the photovoltaic device is shown in fig. 1, wherein the cathode, the hole transport layer, the photosensitive material layer, the charge transport layer and the anode are prepared from the quantum dots prepared by the preparation method of the quantum dots, and the charge conversion rate of the photovoltaic device can be effectively improved.
Example 1
The embodiment uses CdC l2 、Se-TOP、CH 3 -(CH 2 ) 17 MgCl is used as a raw material, and the preparation method specifically comprises the following steps:
(1) Preparation of Se-TOP solution:
dissolving 1mmol of Se powder in 2ml of TOP solution, stirring at 60 ℃ in nitrogen atmosphere for 20 minutes, and cooling to room temperature for standby;
(2) Mixing Se-TOP solution and CH 3 -(CH 2 ) 17 MgCl, the reaction formula is as follows:
CdCl 2 +RMgCl→CdR+MgCl 2
taking 2 millimoles of CH 3 -(CH 2 ) 17 MgCl and Se-TOP solution prepared in the step (1) are dispersed in a three-neck flask containing 20ml of eighteen-part solution, and then stirred uniformly and protected by nitrogen for standby.
(3) CdSe quantum dots are prepared, and the reaction formula is as follows:
Se-TOP+CdR→CdSe
raising the mixing temperature in the step (2) to 200 ℃, and then taking 3 millimoles of CdCl 2 Dissolving in 2ml of octadecene, and then quickly injecting into the mixed solution obtained in the step 2) to react for 10min; after the reaction is finished, cooling to room temperature, adding a precipitator, and carrying out high-speed centrifugal separation to obtain CdSe quanta.
(4) Preparing an octane solution with the concentration of 20 mg/ml from the quantum dots prepared in the step (3), and preparing the quantum dots into a photosensitive material layer.
(5) A quantum dot photovoltaic device:
and (3) sequentially stacking a cathode, a hole transport layer, a photosensitive material layer, a charge transport layer and an anode on the transparent conductive substrate, wherein the photosensitive material layer is prepared by the step (4).
The photovoltaic devices are prepared under the same conditions and are divided into a first batch and a second batch, wherein the photosensitive material layer in the first batch of devices is the quantum dot prepared by the embodiment; the photosensitive material layer in the second batch of devices is quantum dots prepared by adopting a conventional heat injection method; the device efficiency and device lifetime of both batches of devices were then tested in the same test mode and the results are shown in table one.
Results of device efficiency and device lifetime tests for photovoltaic devices
| Device class | Device efficiency (EQE) | Device life (h) |
| First batch of | 4.5％ | 9.5 |
| Second batch | 2％ | 5 |
Example 2
The embodiment uses InCl 3 、CH 3 -(CH 2 ) 17 MgC、(TMS) 3 P is used as a raw material, and the preparation method specifically comprises the following steps:
(1) Preparation (TMS) 3 P solution:
take 0.5 millimoles (TMS) 3 The P solution was dissolved in 2ml of TOP solution and mixed well under nitrogen atmosphere for further use.
(2) Mixed CH 3 -(CH 2 ) 17 MgCl & ltTMS 3 P solution:
taking 2 millimoles of CH 3 -(CH 2 ) 17 MgCl and the above prepared (TMS) 3 The P solutions were dispersed together in a three-necked flask containing 20ml of an eighteen solution, and then stirred well and protected with nitrogen for use.
(3) Preparing InP quantum dots:
raising the mixing temperature in the step (2) to 200 ℃, and then taking 3 millimoles of CdCl 2 Dissolving in 2 milliliters of octadecene, quickly injecting into the mixed solution obtained in the step (2), and reacting for 10 minutes; and cooling to room temperature after the reaction is finished, adding a precipitator, and performing high-speed centrifugal separation to obtain the InP quantum dots.
(4) Preparing an octane solution with the concentration of 20 mg/ml from the quantum dots prepared in the step (3), and preparing the quantum dots into a photosensitive material layer.
(5) A photovoltaic device:
and (3) sequentially stacking a cathode, a hole transport layer, a photosensitive material layer, a charge transport layer and an anode on the transparent conductive substrate, wherein the photosensitive material layer is prepared in the step (4).
The photovoltaic devices are prepared under the same conditions and are divided into a third batch and a fourth batch, wherein the photosensitive material layer in the third batch of devices is the quantum dot prepared by the embodiment; the photosensitive material layer in the fourth batch of devices is quantum dots prepared by adopting a conventional heat injection method; the same test mode was then used to test the device efficiency and device lifetime of both batches of devices. The results are shown in Table II.
Device efficiency and device lifetime test results for a photovoltaic device
| Device class | Device efficiency (EQE) | Device life (h) |
| Third batch | 3.9％ | 17.5 |
| Fourth batch | 2％ | 10 |
As can be seen from examples 1 and 2, the quantum dots prepared by using the grignard reagent in the present application can effectively and rapidly prepare the quantum dots with good peak width and few defects by using the characteristic of rapid crystallization by hot injection, and the obtained quantum dots have good stability and do not affect exciton diffusion. The photosensitive material layer of the photovoltaic device prepared by the quantum dots can effectively improve the charge conversion rate and the service life of the photovoltaic device.
While the invention has been illustrated and described with reference to specific embodiments, it is to be understood that the above embodiments are merely illustrative of the technical aspects of the invention and not restrictive thereof; those of ordinary skill in the art will appreciate that: modifications may be made to the technical solutions described in the foregoing embodiments, or equivalents may be substituted for some or all of the technical features thereof, without departing from the spirit and scope of the present invention; such modifications and substitutions do not depart from the spirit of the corresponding technical solutions; it is therefore intended to cover in the appended claims all such alternatives and modifications as fall within the scope of the invention.
Claims (15)
1. The preparation method of the quantum dot is characterized by comprising the following steps of:
dispersing a Grignard reagent and an anion precursor in a non-co-melting solvent to obtain a mixed solution; heating the mixed solution to a temperature range of the solution during nucleation, injecting the solution of the metal halide into the mixed solution for nucleation, cooling and purifying after the reaction to obtain quantum dots;
the Grignard reagent is RMgX, wherein R is an alkane group; x is halogen element;
the halogen element X is selected from one of Cl, br, F or I;
the alkyl is CH 3 -(CH 2 ) n -wherein n is an integer from 1 to 18; or alternatively; the alkyl is (CH) 2 ) m -wherein m is an integer from 1 to 18;
the anion precursor comprises S-ODE, S-TOP, S-OA, se-TOP, S-OLA, S-TBP, se-TBP, te-ODE, te-OA, te-TOP, te-TBP, (TMS) 3 S sum (TMS) 3 At least one of P;
the non-co-melting solvent comprises at least one of octadecene, paraffin oil and diphenyl ether;
the metal halideThe chemical compound comprises CdX 2 、ZnX 2 、PbX 2 、InX 3 Or HgX 2 Wherein X is selected from one of Cl, br, F or I;
the temperature range of the solution during the nucleation reaction is 60-320 ℃;
the nucleation reaction is carried out under the protection of inert atmosphere.
2. The method for preparing quantum dots according to claim 1, wherein the halogen element X is Cl or Br.
3. The method of preparing quantum dots according to claim 1, wherein the solution temperature is 25 to 200 ℃ and the dispersing time is 5 to 120min in the process of dispersing the grignard reagent and the anion precursor in the non-co-solvent, and the dispersing operation is performed under the protection of inert atmosphere.
4. The method of claim 1, wherein the solution of metal halide is prepared by dispersing the metal halide in a non-co-solvent.
5. The method of preparing quantum dots according to claim 4, wherein the solution temperature is 25 to 200 ℃ during the dispersion in the non-co-solvent, the dispersion time is 5min to 2h, and the dispersion operation is performed under the protection of inert atmosphere.
6. The method of claim 1, wherein the molar volume ratio of the metal halide, the grignard reagent, the anion precursor, and the non-co-solvent is (1-10 mmol): (1-10 mmol): 1mmol: (5-30 ml).
7. The method of claim 1, wherein the molar volume ratio of the metal halide, the grignard reagent, the anion precursor, and the non-co-solvent is (2-8 mmol): (2-8 mmol): 1mmol: (8-24 ml).
8. The method for preparing quantum dots according to claim 1, wherein the temperature of the solution at the time of the nucleation reaction is in the range of 80 to 260 ℃;
and/or;
the nucleation reaction time is 1 min-2 h.
9. The method of claim 1, wherein the nucleation is performed for a period of 20 to 80 minutes.
10. The method for preparing quantum dots according to claim 1, wherein the purification process specifically comprises: and adding a proper amount of precipitant into the mixed solution containing the quantum dots after the nucleation reaction, and carrying out centrifugal separation to obtain the quantum dots.
11. The method of claim 10, wherein the precipitant is composed of an organic ester solvent and a polar solvent.
12. The method for preparing quantum dots according to claim 11, wherein the volume ratio of the mixed liquid containing quantum dots, the organic ester solvent and the polar solvent is 1 (1-3): (0.5-1).
13. The method of preparing a quantum dot according to claim 11, wherein the organic ester solvent comprises at least one of ethyl acetate, methyl acetate, propyl acetate, butyl acetate, ethyl formate, ethyl propionate, and butyl ethyl propionate;
the polar solvent includes at least one of ethanol, methanol, and isopropanol.
14. A photoactive material layer prepared from quantum dots prepared by the method for preparing quantum dots according to any one of claims 1-13.
15. A photovoltaic device comprising a cathode, a hole transport layer, the photoactive material layer of claim 14, a charge transport layer, and an anode, connected in sequence.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010590364.5A CN111682117B (en) | 2020-06-24 | 2020-06-24 | Quantum dot preparation method, photosensitive material layer and photovoltaic device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010590364.5A CN111682117B (en) | 2020-06-24 | 2020-06-24 | Quantum dot preparation method, photosensitive material layer and photovoltaic device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111682117A CN111682117A (en) | 2020-09-18 |
| CN111682117B true CN111682117B (en) | 2023-06-09 |
Family
ID=72437005
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010590364.5A Active CN111682117B (en) | 2020-06-24 | 2020-06-24 | Quantum dot preparation method, photosensitive material layer and photovoltaic device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111682117B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113105887B (en) * | 2021-04-29 | 2024-04-19 | 湖州鑫成新材料科技有限公司 | Quantum dot and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110176541A (en) * | 2019-06-09 | 2019-08-27 | 苏州大学 | A kind of vulcanized lead Colloidal Quantum Dots solar battery and preparation method based on convection current assembling sedimentation |
| CN110760306A (en) * | 2018-07-27 | 2020-02-07 | Tcl集团股份有限公司 | Quantum dot purification method |
| CN110885674A (en) * | 2018-09-07 | 2020-03-17 | Tcl集团股份有限公司 | Composite material and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8178221B2 (en) * | 2000-07-10 | 2012-05-15 | Amit Goyal | {100}<100> or 45°-rotated {100}<100>, semiconductor-based, large-area, flexible, electronic devices |
| US10490762B2 (en) * | 2015-02-04 | 2019-11-26 | University Of North Carolina At Charlotte | Quantum dot light emitting devices |
| CN106083573B (en) * | 2016-07-01 | 2021-03-23 | 京东方科技集团股份有限公司 | Organic ligand, preparation method thereof, quantum dot layer and light-emitting diode |
-
2020
- 2020-06-24 CN CN202010590364.5A patent/CN111682117B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110760306A (en) * | 2018-07-27 | 2020-02-07 | Tcl集团股份有限公司 | Quantum dot purification method |
| CN110885674A (en) * | 2018-09-07 | 2020-03-17 | Tcl集团股份有限公司 | Composite material and preparation method thereof |
| CN110176541A (en) * | 2019-06-09 | 2019-08-27 | 苏州大学 | A kind of vulcanized lead Colloidal Quantum Dots solar battery and preparation method based on convection current assembling sedimentation |
Non-Patent Citations (2)
| Title |
|---|
| Sung Won Kim 等."Hybrid Nanocomposite of CdSe Quantum Dots and a P3HT-b-PDMAEMA Block Copolymer for Photovoltaic Applications".《ADVANCED MATERIALS AND NANOTECHNOLOGY》.2011,第第700卷卷(第第120-124页期),第120-124页. * |
| 郑涛 等." 热注入法合成PbX(X=S,Se)量子点的结构和性能研究".《人工晶体学报》.2016,第45卷(第5期),第1288-1292页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111682117A (en) | 2020-09-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Li et al. | Sustainable and self‐enhanced electrochemiluminescent ternary suprastructures derived from CsPbBr3 perovskite quantum dots | |
| Li et al. | A stable germanone as the first isolated heavy ketone with a terminal oxygen atom | |
| CN109133014B (en) | CoN3Preparation method of @ N-C composite electrocatalyst | |
| CN109950564B (en) | MXene-loaded PtRhFe ternary alloy catalyst and preparation method thereof | |
| Marinos et al. | High Efficiency in Catalytic Hydrosilylation of Ketones with Zinc‐Based Precatalysts Featuring Hard and Soft Tridentate O, S, O‐Ligands | |
| CN111682117B (en) | Quantum dot preparation method, photosensitive material layer and photovoltaic device | |
| CN103594561B (en) | Method for manufacturing Cu2ZnSn(S, Se)4 solar battery absorbing layer through oxide thin film in vulcanizing and selenizing mode | |
| Fehr et al. | Integrated halide perovskite photoelectrochemical cells with solar-driven water-splitting efficiency of 20.8% | |
| Peuntinger et al. | Carbene based photochemical molecular assemblies for solar driven hydrogen generation | |
| CN109569720A (en) | It is a kind of using carboxylated carbon-based material as the preparation method of the monatomic catalyst of the metal of carrier | |
| Steffen et al. | Regiospecific Formation and Unusual Optical Properties of 2, 5‐Bis (arylethynyl) rhodacyclopentadienes: A New Class of Luminescent Organometallics | |
| Mengele et al. | Generation of a stable supramolecular hydrogen evolving photocatalyst by alteration of the catalytic center | |
| CN113845142B (en) | Cesium lead iodine perovskite nanocrystalline as well as preparation method and application thereof | |
| CN111430733A (en) | Non-noble metal oxygen reduction catalyst for fuel cell and preparation method thereof | |
| CN111454279A (en) | Organic electroluminescent compound and preparation method and application thereof | |
| CN110137517A (en) | A kind of metal material and preparation method for fuel battery cathode with proton exchange film catalyst | |
| Roy et al. | Synthesis and Electrocatalytic Activity of [FeFe]‐Hydrogenase Model Complexes with Non‐Innocent Chelating Nitrogen‐Donor Ligands | |
| CN116253694A (en) | Ligand, metal organic framework material, application of ligand and metal organic framework material and perovskite solar cell | |
| Wu et al. | Ligand-partially-protected metal-chalcogenide supertetrahedral clusters | |
| CN111682118B (en) | Quantum dot preparation method, photosensitive layer and solar cell device | |
| Das et al. | A NiII–Bis (diphosphine)–Hydride Complex Containing Proton Relays–Structural Characterization and Electrocatalytic Studies | |
| Chen et al. | On the redox property of Ag16Au13 clusters: One-way conversion from anionic [Au13Ag16L24] 3− to charge neutral [Au13Ag16L24] | |
| CN112707778B (en) | Method for preparing 1, 2, 7, 8-tetrahydrodicyclopentano [ cd, lm ] perylene compound and product thereof | |
| CN107964021A (en) | A kind of acid imide photoelectricity small molecule material of boracic nitrogen key and preparation method and application | |
| CN114621761A (en) | Full-bromine-based perovskite purple light quantum dot and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |