CN111312522B - Quantum dot sensitized solar cell CuS/Ti3C2Composite counter electrode and preparation method thereof - Google Patents
Quantum dot sensitized solar cell CuS/Ti3C2Composite counter electrode and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a quantum dot sensitized solar cell CuS/Ti3C2A composite counter electrode and a preparation method thereof. CuS/Ti of the invention3C2The composite material consists of CuS nano-particles and Ti3C2Prepared by a chemical method of in-situ reaction, and the composite material is deposited on FTO conductive glass by a dripping coating method to prepare CuS/Ti3C2And compounding a counter electrode. The counter electrode has simple preparation process and low cost, and the CuS nano-particles can be uniformly anchored on the Ti3C2The surface and the interlayer improve the electrocatalytic activity of the counter electrode, and have low charge transmission resistance and large exchange current density. At 100mW cm‑2Based on CuS/Ti under the conditions of3C2The quantum dot sensitized solar cell assembled by the composite counter electrode has good photoelectric property, the open-circuit voltage is 0.540V, and the short-circuit current density is 21.13mA cm‑2The photoelectric conversion efficiency was 5.13%.
Description
Technical Field
The invention belongs to the technical field of solar cells, and relates to a quantum dot sensitized solar cell CuS/Ti3C2A composite counter electrode and a preparation method thereof.
Background
Quantum Dot Sensitized Solar Cells (QDSSCs) are the third generation solar cells that appeared in the 90 s of the last century, i.e., the base materials for sensitizing broadband with narrow-bandgap inorganic semiconductor Quantum Dots (QDs), and have the advantages of low cost, easy manufacturing, and excellent performance of Quantum Dots (QDs). The quantum dots have great advantages compared with dye organic molecules, on one hand, the quantum dots have quantum confinement effect, and the band gap width of the quantum dots can be adjusted by controlling the size and shape of the particles so as to adjust the range of an absorption spectrum; on the other hand, the semiconductor quantum dot has an exciton multiplication effect, and one high-energy photon excites the semiconductor quantum dot to generate a plurality of electron-hole pairs. If the two advantages of the semiconductor quantum dots are successfully applied to the solar cell, the theoretical photoelectric conversion efficiency of the QDSSCs can reach 44%, which is much higher than the theoretical conversion efficiency of the crystalline silicon solar cell, namely 32.9%. Therefore, QDSSCs have great potential for development, both in terms of cost and application.
Transition metal sulfides such as Cu2S, CoS, CuS, PbS and ternary cobalt spinels have been used in counter electrodes. CuS is a commonly used composite Counter Electrode material that is low in cost and easy to synthesize, CoS/CuS, NiS/CuS and C/CuS have been successfully used in QDSSC, and the power conversion efficiencies (η) obtained based on composite CE are 4.1%, 4.19% and 3.86% (Z.Yang, C.Y.Chen, C.W.Liu, et al, Quantum Dot-Sensitized Solar cell dressing CuS/CoS Electrodes Provide 4.1% Efficiency, Advanced Energy Materials,1(2011) cell 264; H.J.Kim, S.M.Suh, S.S.Raester, Invitro. CuS/NiS Electrode composite coating layer reaction, research cell, Investigation, application of chemical reaction, chemical, 118 (2014)16526-16535.).
The counter electrode mainly comprises noble metal, conductive polymer, carbon material and metal sulfide. MXene is a new family transition metal carbide/nitride two-dimensional crystal material with graphene structure and chemical formula of Mn+1Xn, where M is an early transition metal, X is C and/or N, and N is 1,2, 3. Ti3C2Is a typical representative of MXene in the family, can be used as a reinforcement of a novel composite material and also can be used as a high-temperature lubricating material due to excellent mechanical, electronic and magnetic properties, and is widely applied to various fields, such as catalytic hydrogen production, supercapacitors, lithium ion batteries, environmental disinfection and the like.
Disclosure of Invention
The invention aims to provide a Ti based on accordion structure3C2Quantum dot sensitized solar cell CuS/Ti3C2A composite counter electrode and a preparation method thereof. In the composite counter electrode, Ti3C2A large number of catalytic active sites are provided, CuS has high catalytic activity, and the CuS have synergistic effect, so that the catalytic activity of the counter electrode is greatly improved.
The technical scheme for realizing the purpose of the invention is as follows:
quantum dot sensitized solar cell CuS/Ti3C2The preparation method of the composite counter electrode comprises the following specific steps:
Ti3AlC2placing the titanium substrate in 40% HF acid for etching, stirring and reacting for 24-48 h, centrifugally washing and drying after the reaction is finished to obtain Ti with an accordion structure3C2；
mixing Ti3C2Adding CuSO into the powder4Adding Na slowly into the solution, stirring and mixing uniformly2S solution is stirred for reaction, and after the reaction is finished, Ti is obtained by centrifugal washing and drying3C2CuS/Ti with the mass ratio of 1: 1-2 to CuS3C2A composite material;
step 3, CuS/Ti3C2Preparing a composite counter electrode:
mixing CuS/Ti3C2Adding the composite material into an ethanol aqueous solution, performing ultrasonic dispersion, uniformly and dropwisely coating the suspension on the surface of clean FTO conductive glass to obtain CuS/Ti3C2And compounding a counter electrode.
Preferably, in step 1, said Ti3AlC2The mass ratio of the hydrogen fluoride to the HF acid is 1: 4-5.
Preferably, in the step 1, the drying temperature is 50-80 ℃, the drying time is more than 12 hours, and the drying is vacuum drying.
Preferably, in step 2, the time for stirring and mixing uniformly is more than 30 min.
Preferably, in step 2, the stirring reaction time is 30min or more.
Preferably, in the step 3, the volume ratio of ethanol to water in the ethanol aqueous solution is 3-5: 5-7.
Preferably, in the step 3, the ultrasonic dispersion time is 10-15 min.
The invention also provides a catalyst based on CuS/Ti3C2The quantum dot sensitized solar cell with the composite counter electrode comprises CuS/Ti3C2Composite counter electrode, S2 n -/S2-Polysulfide electrolyte and TiO2the/CdS/CdSe/ZnS co-sensitized photo-anode.
Compared with the prior art, the invention has the following advantages:
(1) the process is simple, and the manufacturing cost is low;
(2) CuS/Ti of the invention3C2Electrochemical series resistance (R) of composite counter electrodes) Charge transfer resistance (R)ct) Exchange current density (J)0) The improvement is remarkable;
(3) after the composite counter electrode and the photo-anode are assembled into a battery, the short-circuit current (J)sc) And open circuit voltage (V)oc) And the photoelectric conversion efficiency is obviously improved at 100mW cm-2Under the conditions of (1), the open-circuit voltage is 0.540V, and the short-circuit current density is 21.13mA cm-2The photoelectric conversion efficiency was 5.13%.
Drawings
FIG. 1 shows Ti in example 13C2Scanning electron microscopy images of (a);
FIG. 2 is a schematic representation of the example 2 CuS/Ti3C2Electron microscopy of the composite;
FIG. 3 is an XRD pattern for example 1 and example 2;
FIG. 4 is a graph showing the values of CuS/Ti in example 23C2A composite counter electrode battery performance test result graph;
FIG. 5 shows CuS/Ti in example 33C2CompoundingAnd (4) a counter electrode photoelectric conversion result graph.
Detailed Description
The present invention will be described in further detail with reference to the following examples and accompanying drawings.
Example 1
Ti of accordion structure3C2Preparation of
500mg of Ti3AlC2Placing in a 100ml autoclave liner, measuring 60ml of 40% HF acid solution with a plastic measuring cylinder, slowly adding into the autoclave liner along the liner wall, slowly stirring uniformly at the beginning, carefully sealing the liner until all the HF acid solution is added into the liner, and then stirring vigorously. After the reaction is carried out for 12h, 24h, 36h and 48h respectively, the mixed solution is centrifugally washed at the rotating speed of 10000r/min for 5min each time until the Ph is 7 easily. The centrifuged sample was dried under vacuum at 60 ℃ for 12 hours. FIG. 1 is Ti of accordion structure3C2Scanning electron microscopy of (a). As can be seen from the figure, when the reaction times are different, Ti3C2The sample shows different shapes, when the reaction time is 12 hours, the reaction is insufficient, the sample lamellar structure is not obvious, when the reaction time is increased, the lamellar structure is gradually clear, and when the reaction time is 48 hours, the sample shows the optimal lamellar structure.
Example 2
Ti of accordion structure3C2Preparation of
500mg of Ti3AlC2Placing in a 100ml autoclave liner, measuring 60ml of 40% HF acid solution with a plastic measuring cylinder, slowly adding into the autoclave liner along the liner wall, slowly stirring uniformly at the beginning, carefully sealing the liner until all the HF acid solution is added into the liner, and then stirring vigorously. After 48 hours of reaction, the mixed solution is centrifugally washed at the rotating speed of 10000r/min for 5min each time until the Ph is 7 easily. The centrifuged sample was dried under vacuum at 60 ℃ for 12 hours.
CuS/Ti3C2Synthesis of composite materials
Mixing Ti3C2Adding into CuSO of 5g/L4The solution was stirred at room temperature for 30min, and then 4.8g/L Na was added to the mixed solution using a dropper2The S solution was then stirred at room temperature for 30 min. Centrifugally washing at 5000r/min for 3 times, washing with deionized water for the first two times and ethanol for the last time, and drying in a vacuum oven at 60 deg.C for 12 hr to obtain Ti3C2The mass ratio of CuS to CuS is 4:1, 1:2, denoted T4C1, T1C1, and T1C 2. FIG. 2 is CuS/Ti3C2Electron microscopy of the composite. As can be seen from the figure, when Ti is used3C2When the mass ratio of the CuS nanoparticles to the CuS is 1:2, the CuS nanoparticles can be sufficiently embedded into Ti3C2Between layers and on the surface, when the mass ratio is 4:1, CuS nano particles can not completely cover Ti3C2When the mass ratio is 1:1, the CuS nano-particles can only be covered on Ti3C2And cannot be embedded between layers.
CuS/Ti3C2Preparing a composite counter electrode:
taking 22mgCuS/Ti3C2The composite material was added to 10ml of a mixed solution of ethanol and water (ethanol: water ═ 3:7), and then subjected to ultrasonic dispersion with a cell disruptor at a power of 10% for 10 min. 20 mul of the solution was dropped on FTO conductive glass by a pipette at a time, and then dried on a hot plate at 60 ℃ and repeated 5 times.
Example 3
Quantum dot sensitized solar cell (CuS/Ti)3C2The composite counter electrode is a counter electrode, TiO2the/CdS/CdSe/ZnS electrode is a photo-anode.
CuS/Ti3C2The composite counter electrode was the same as in example 2.
The preparation method of the quantum dot sensitized solar cell photo-anode comprises the following steps:
(1)TiO2preparation of films
Firstly, cleaning the FTO transparent conductive glass.
Second step, TiO2Preparation of slurry. TiO used in the invention2The slurry is prepared by the following specific steps: putting 55g of terpineol into a beaker of 100mL, then taking 0.5g of ethyl cellulose, putting the beaker of 100mL mixed with the raw materials of the terpineol and the ethyl cellulose on a heating stirrer, heating to 130 ℃, and simultaneously stirring vigorously until the ethyl cellulose is completely dissolved in the terpineol, after the mixture is cooled to room temperature, adding 1.2g of nano titanium dioxide P25 powder into the beaker of 100mL, and stirring vigorously until the nano titanium dioxide P25 powder is dissolved in the mixed solution.
Third step, TiO2And (5) manufacturing a film. The invention adopts Spin coating method to prepare photoanode TiO2Film, TiO2The specific manufacturing steps of the film are as follows: taking out the cleaned FTO conductive glass stored in the ethanol solution previously, measuring the conductive surface of the FTO conductive glass, facing the conductive surface upwards, drying, placing the dried FTO conductive glass on a sheet support of a spin coater by using tweezers, sucking the sheet, dropping 1-2 drops of slurry to the conductive surface of the FTO glass by using a suction tube, starting spin coating, and drying after the spin coating is finished. The above process was cycled 9 times.
Step four, TiO2And (4) carrying out heat treatment on the film. After drying, coating TiO on the coating2Placing the FTO conductive glass of the film in a box furnace, calcining for 30min at 500 ℃, heating at the rate of 5 ℃/min, and cooling to room temperature to obtain the TiO2A film.
(2) Deposition of CdS quantum dots
CdS quantum dots were deposited by sequential ionic layer adsorption and reaction method (SILAR): first, 0.1MCd (CH3COO) is prepared2·2H2O methanol solution and 0.1M Na2S·9H2O methanol and water (1:1) solution, then, will carry TiO2Soaking FTO conductive glass of the film in a Cd (CH3COO) 2.2H 2O methanol solution for 1min, taking out, washing with deionized water, soaking in deionized water for 30s, air drying, and soaking in Na2S·9H2Dissolving in O methanol and water (1:1) solution for 1min, washing with deionized water, soaking in deionized water for 30s, and air drying. The process was cycled 12 times. The prepared electrode is named as TiO2a/CdS electrode.
(3) Deposition of CdSe quantum dots
CdSe quantum dots were deposited on TiO2/CdS covered FTO conductive substrates by Chemical Bath Deposition (CBD). Firstly, NaSeSO is prepared3And (3) solution. The preparation steps are as follows: formulated to contain 0.3MNa2SO3And 0.1M Se in 400mL of water, placing the mixture in a round-bottom flask, and refluxing at 70 ℃ for 7h to obtain NaSeSO3And (3) solution. Then, the TiO thus obtained is subjected to a thermal treatment2CdS electrode immersion Cd (CH3COO)2·2H2Taking out the electrode after 1min of O-methanol solution, washing with deionized water, soaking in deionized water for 30s, air drying, and soaking in NaSeSO3And (3) carrying out water bath for 30min at 50 ℃ in a beaker of the solution, taking out the electrode after the water bath is finished, washing the electrode with deionized water, soaking the electrode in the deionized water for 30s, and airing the electrode. This process needs to be repeated 3 times. The obtained electrode is represented by TiO2a/CdS/CdSe electrode.
(4) Deposition of ZnS passivation layer
The deposition method of ZnS passivation layer is the same as that of CdS quantum dot (CBD). Only the solution needs to be changed to 0.1M Zn (CH3COO)2·2H2O methanol solution and 0.1M Na2S·9H2O methanol and water (1: 1). The process was cycled 2 times. The final prepared electrode is denoted as TiO2a/CdS/CdSe/ZnS photo-anode.
(5) Preparation of polysulfide electrolyte
S.sub.123. sup. 122 was prepared according to the literature (Hee-Je Kim, Seong-Min Suh, S.Srinivasa Rao, Dinah Punnoose, Chebrolu Venkata Tulasivarma, Chandu.V.M.Gopi, Nagabhushanam Kundagara, Seenu Ravi, Ikkurthi Kanaka Durga, Journal of Electroanalytical Chemistry,777(2016) 123. sup. 132)2 n -/S2-Polysulfide electrolyte, which is slightly different from the literature, the electrolyte of the invention comprises 2M Na dissolved in a mixed solution (volume ratio of 3:7) of deionized water and methanol2S·9H2O, 2M S and 0.2M KCl, stirred in a water bath at 50 ℃ for 1 h.
Fig. 4 and 5 are a graph of electrochemical performance of the counter electrode and a graph of photoelectric performance of the assembled solar cell, respectively. It can be seen from FIG. 4 that the Rct value of the counter electrode has a significant change with the increase of the amount of CuS, when Ti is used3C2When the mass ratio of the electrode to CuS is 1:2, the Rct value of the counter electrode reaches the minimum value of 2.96 omega cm-2At this time, the catalytic activity of the whole counter electrode reaches the maximum, and at this time, the short-circuit current J of the counter electrode0The value also reaches the maximum value of 10.26mA cm-2Description of Ti3C2The recombination with CuS plays a positive role for the whole counter electrode. As can be seen from FIG. 5, when Ti is used3C2When the mass ratio of the current to the CuS is 1:2, the short-circuit current and the open-circuit voltage of the whole cell tend to be obviously increased compared with those of the other two cells, the maximum short-circuit current and the maximum open-circuit voltage are respectively 21.13 mA-cm < -2 > and 0.55V, and the photoelectric conversion efficiency of the cell is 5.13%.
Claims (10)
1. Quantum dot sensitized solar cell CuS/Ti3C2The preparation method of the composite counter electrode is characterized by comprising the following specific steps of:
step 1, Ti of accordion structure3C2The preparation of (1): ti3AlC2Placing the titanium substrate in 40% HF acid for etching, stirring and reacting for 24-48 h, centrifugally washing and drying after the reaction is finished to obtain Ti with an accordion structure3C2；
Step 2, CuS/Ti3C2Synthesis of the composite material: mixing Ti3C2Adding CuSO into the powder4Adding Na slowly into the solution, stirring and mixing uniformly2S solution is stirred for reaction, and after the reaction is finished, Ti is obtained by centrifugal washing and drying3C2CuS/Ti with the mass ratio of 1: 1-2 to CuS3C2A composite material;
step 3, CuS/Ti3C2Preparing a composite counter electrode: mixing CuS/Ti3C2Adding the composite material into an ethanol aqueous solution, performing ultrasonic dispersion, uniformly and dropwisely coating the suspension on the surface of clean FTO conductive glass to obtain CuS/Ti3C2And compounding a counter electrode.
2. The method of claim 1, wherein the step of1, said Ti3AlC2The mass ratio of the hydrogen fluoride to the HF acid is 1: 4-5.
3. The preparation method according to claim 1, wherein in the step 1, the drying temperature is 50-80 ℃, the drying time is more than 12h, and the drying is vacuum drying.
4. The process according to claim 1, wherein the stirring and mixing in step 2 are carried out for 30min or more.
5. The process according to claim 1, wherein the stirring reaction time in the step 2 is 30min or more.
6. The preparation method according to claim 1, wherein in the step 3, the volume ratio of ethanol to water in the ethanol aqueous solution is 3-5: 5-7.
7. The preparation method according to claim 1, wherein in the step 3, the ultrasonic dispersion time is 10-15 min.
8. CuS/Ti obtained by the production method according to any one of claims 1 to 73C2And compounding a counter electrode.
9. CuS/Ti according to claim 83C2A quantum dot sensitized solar cell with a composite counter electrode.
10. The quantum dot sensitized solar cell according to claim 9, comprising CuS/Ti3C2A counter electrode is compounded, and the electrode is combined,
polysulfide electrolyte and TiO2the/CdS/CdSe/ZnS co-sensitized photo-anode.
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| CN111916290A (en) * | 2020-06-30 | 2020-11-10 | 河海大学 | Transition metal sulfide/Ti3C2TxMethod for preparing composite material |
| CN113171784A (en) * | 2021-04-25 | 2021-07-27 | 福州大学 | Preparation method of MXene modified cadmium selenide quantum dot heterogeneous composite material for photolysis of water to produce hydrogen |
| CN115247058A (en) * | 2021-04-28 | 2022-10-28 | Tcl科技集团股份有限公司 | Composite material and preparation method thereof, and quantum dot light-emitting diode and preparation method thereof |
| CN115074739B (en) * | 2022-07-19 | 2023-10-13 | 中国科学院海洋研究所 | CdS@TiO for metal photogenerated cathode protection 2 Preparation method and application of NTAs composite material |
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