CN109473552B - Solar cell based on solution method and preparation method thereof - Google Patents
Solar cell based on solution method and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a solar cell based on a solution method and a preparation method thereof, wherein the method comprises the following steps: providing a substrate comprising a cathode; forming an electron transport layer on the substrate; forming Sb on the electron transport layer2S3A film; wherein said Sb2S3The preparation process of the film comprises the following steps: sb2S5Dissolving in ammonium sulfide solution, filtering, and collecting supernatant; spin coating the supernatant on the electron transport layer, and then sequentially drying and annealing to obtain the Sb2S3A film; in the Sb2S3Forming a hole transport layer on the film; an anode is formed on the hole transport layer. The invention adopts the technology of spin coating by a solution method, and ammonium sulfide is used for dissolving Sb2S5Preparing a precursor, and preparing Sb after spin-coating annealing2S3A film. High-quality Sb is realized by accurately controlling parameters such as concentration, spin coating times, annealing temperature and time2S3The preparation of the film is beneficial to the improvement of the efficiency of the solar cell.
Description
Technical Field
The invention relates to the field of novel thin-film solar cell photoelectric functional materials, in particular to a solar cell based on a solution method and a preparation method thereof.
Background
Sb2S3The thin film has a high absorption coefficient in the visible region, approaching the optimal band gap for solar cell applications. In addition, Sb2S3The thin-film solar cell still has good photovoltaic performance under the condition of weak light irradiation, and can realize high-efficiency photoelectric conversion in cloudy weather, indoor conditions and building walls. Therefore, for Sb2S3The research of the thin-film solar cell has high value for the next generation of photovoltaic cells. To promote Sb2S3The development of thin film solar cells has carried out the optimization of device structure design and film quality. It is well known that the absorber layer plays an important role in the photovoltaic performance of the device. Therefore, many methods have been introduced in recent years to optimize Sb2S3The quality of the film. One method for preparing Sb by adopting water-soluble Chemical Bath Deposition (CBD)2S3Film using a solution mixture of antimony chloride and sodium thiosulfate as Sb3+And S2-A low temperature precursor source of ions. However, oxidation of antimony sulfide is hardly avoided using the CBD method, and thus the formed antimony oxide generates a deep trap defect on the surface, resulting in severe recombination of photo-excited charge carriers. After thioacetamide treatment is introduced in the later period, the defect of deep oxide is eliminated, and the photoelectric conversion efficiency reaches 7.5 percent, but the CBD method still faces mesoporous TiO2Long time required for Sb formation on thin film2S3To a problem of (a). Other methods, including atomic layer deposition and precise thickness deposition, are also applicable to planar Sb2S3However, these methods have complicated preparation processes and do not meet the requirements of the existing industrialization. Therefore, the preparation method based on the vacuum evaporation deposition technology which is beneficial to large-scale industrialization obtains wide attention. Wherein Sb is prepared by adopting a vacuum single-source thermal evaporation method2S3Film, process of direct evaporation of Sb2S3Precursor powder material, deposition of Sb on a substrate2S3A method for preparing a film. However, direct single source thermally evaporated Sb2S3The film experiences sulfur loss during evaporation and post-annealing,the ease of composition deviation from stoichiometry directly leads to degradation of film quality and repeatability, which severely compromises film quality and device performance.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention is directed to a solar cell based on a solution method and a method for preparing the same, which is intended to solve the existing single-source thermal evaporation of Sb2S3The films experience sulfur loss during evaporation and post-annealing, which severely compromises film quality and device performance, while the use of SbCl3Or Sb2O3The antimony sulfide prepared by the antimony source solution method needs a low-temperature environment, and the prepared film has more impurity phases, so that the quality of the film and the performance of a device are improved.
The technical scheme of the invention is as follows:
a preparation method of a solar cell based on a solution method comprises the following steps:
providing a substrate comprising a cathode;
forming an electron transport layer on the substrate;
forming Sb on the electron transport layer2S3A film; wherein said Sb2S3The preparation process of the film comprises the following steps: sb2S5Dissolving in ammonium sulfide solution, filtering, and collecting supernatant; spin coating the supernatant on the electron transport layer, and then sequentially drying and annealing to obtain the Sb2S3A film;
in the Sb2S3Forming a hole transport layer on the film;
an anode is formed on the hole transport layer.
The preparation method of the solar cell based on the solution method is characterized in that the concentration of the ammonium sulfide solution is 1-50 wt%.
The preparation method of the solar cell based on the solution method is characterized in that Sb is adopted2S5The mass ratio of the Sb to the ammonium sulfide solution is 0.1-12S5Dissolving in ammonium sulfide solution.
The preparation method of the solar cell based on the solution method is characterized in that the rotation speed of the spin coating is 500-6000 rpm.
The preparation method of the solar cell based on the solution method is characterized in that the spin coating time is 10-120 s.
The preparation method of the solar cell based on the solution method is characterized in that the annealing treatment temperature is 240-400 ℃.
The preparation method of the solar cell based on the solution method is characterized in that the annealing treatment time is 2-30 minutes.
A solar cell based on a solution method sequentially comprises a substrate containing a cathode, an electron transport layer and Sb from bottom to top2S3The solar cell comprises a film, a hole transport layer and an anode, wherein the solar cell is prepared by the preparation method of the solar cell based on the solution method.
The solar cell based on the solution method, wherein the Sb is2S3The film has a thickness of 50 to 1000 nm.
Has the advantages that: the invention adopts the technology of spin coating by a solution method, and ammonium sulfide is used for dissolving Sb2S5Preparing precursor, spin-coating annealing and preparing crystallized Sb2S3A film. Compared with the prior art, the method has the following advantages: 1. mature process, simple operation and repeatable preparation, and improves Sb2S3The film quality and the yield are improved, and the utilization rate of raw materials is improved; 2. spin coating at normal temperature to avoid low-temperature treatment in the existing solution method; 3. using Sb2S5Preparation of Sb by using ammonium sulfide solution as precursor2S3The number of spin-coating times is less than that of the previous times; 4. using Sb2S5Preparation of Sb by using ammonium sulfide solution as precursor2S3The film has rich sulfur source, and the prepared film has less impurities; 5. by accurately controlling the spin coating speed, the spin coating time and the annealing condition, the required film thickness and the adjustable film microstructure performance can be easily obtained according to requirements; 6. using Sb2S5The ammonium sulfide solution is used as a precursor, and a complex and expensive vacuum device is not needed for preparing the film.
Drawings
FIG. 1 shows Sb prepared in example 12S3X-ray diffraction pattern of the film.
FIG. 2 is a Sb-based alloy prepared in example 12S3J-V plot of thin film solar cells.
Detailed Description
The present invention provides a solar cell based on a solution method and a method for manufacturing the same, and the present invention is further described in detail below in order to make the objects, technical solutions, and effects of the present invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a preparation method of a solar cell based on a solution method, which comprises the following steps:
providing a substrate comprising a cathode;
forming an electron transport layer on the substrate;
forming Sb on the electron transport layer2S3A film; wherein said Sb2S3The preparation process of the film comprises the following steps: sb2S5Dissolving in ammonium sulfide solution, filtering, and collecting supernatant; spin coating the supernatant on the electron transport layer, and then sequentially drying and annealing to obtain the Sb2S3A film;
in the Sb2S3Forming a hole transport layer on the film;
an anode is formed on the hole transport layer.
Compared with the prior art, the main improvements of the embodiment are as follows: adopts a solution spin coating technology, takes an ammonium sulfide solution as a solvent and takes Sb as2S5As precursor material, realize Sb2S3And (3) preparing a film. This example employed direct dissolution of Sb2S5Formation of Sb2S5Complex with ammonium sulfide (Sb)2S5+3(NH4)S→2(NH4)3SbS4) Can be decomposed to form Sb after spin coating and heating2S3 (2(NH4)3SbS4 → Sb2S5 + 3(NH4)S, Sb2S5 →Sb2S3 + 2S ×). The preparation method of the embodiment has the following advantages:
1. adopts the solution spin coating deposition technology, has mature process, simple operation and repeatable preparation, improves Sb2S3The film quality and the yield are improved, and the utilization rate of raw materials is improved;
2. spin coating at normal temperature to avoid the need of low-temperature treatment in the prior solution method to keep the stability of the precursor solution;
3. using Sb2S5Preparation of Sb by using ammonium sulfide solution as precursor2S3The film avoids the slow water bath reaction process in the existing solution method, reduces the reaction time, and ensures that the spin coating times are less than the previous times;
4. using Sb2S5Preparation of Sb by using ammonium sulfide solution as precursor2S3The film has rich sulfur source, and the prepared film has less impurities;
5. by accurately controlling the spin coating speed, the spin coating time and the annealing condition, the required film thickness and the adjustable film microstructure performance can be easily obtained according to requirements;
6. using Sb2S5The ammonium sulfide solution is used as a precursor, and a complex and expensive vacuum device is not needed for preparing the film.
In a preferred embodiment, the concentration of the ammonium sulfide solution is 1 to 50 wt.%.
In a preferred embodiment, according to Sb2S5The mass ratio of the Sb to the ammonium sulfide solution is 0.1-12S5Dissolving in ammonium sulfide solution.
In a preferred embodiment, the spin coating speed is 500-.
In a preferred embodiment, the method comprisesThe temperature of the annealing treatment is 240-400 ℃, and the time of the annealing treatment is 2-30 minutes. The precursor spin-coated film becomes Sb after drying process2S5With ammonium sulfide. When the film is heated in the range of 240 ℃ to 400 ℃, the ammonium sulfide is quickly volatilized, and the Sb remained2S5Will quickly become Sb2S3. Heat treatment for 2-30 min to form Sb with good crystallization2S3Film, over which time some sulfur loss will result.
This example uses a solution spin coating technique to dissolve Sb using ammonium sulfide2S5Preparing precursor, spin-coating annealing and preparing crystallized Sb2S3A film. High-quality Sb is realized by accurately controlling parameters such as concentration, spin coating times, annealing temperature and time2S3The preparation of the film is directly beneficial to Sb2S3The efficiency of the thin film solar cell is improved. The present embodiment can repeat the spin coating and annealing for several times to obtain the desired Sb2S3And (5) the thickness of the film layer.
The invention also provides a solar cell based on the solution method, which sequentially comprises a substrate containing a cathode, an electron transport layer and Sb from bottom to top2S3The solar cell comprises a film, a hole transport layer and an anode, wherein the solar cell is prepared by the preparation method of the solar cell based on the solution method.
In a preferred embodiment, the Sb is2S3The thickness of the film is 50-1000 nm. Visible light can be well absorbed in the thickness range, and photon-generated carrier separation is formed.
The present invention will be described in detail below with reference to examples.
Example 1
Sb2S5Dissolving in ammonium sulfide solution, filtering to obtain precursor, and preparing solar cell by using flat solar cell structure as follows: FTO/c-TiO2/ Sb2S3First an FTO substrate (SnO doped with fluorine)2Glass) is cleaned, and compact titanium dioxide (c-TiO) is added2) Is spin-coated toPlacing the FTO substrate (3000 rpm/30 s) into a high-temperature sintering furnace to be sintered for 4 hours at 450 ℃, and cooling to room temperature for later use; 0.5 g of Sb2S5Fully dissolving in 1 ml of 47wt% ammonium sulfide solution, and filtering supernatant for later use; placing a substrate on a spin coater, setting the rotation speed to be 3000rpm for 30 seconds, dropwise adding 40 microliter of filtrate, spreading the whole substrate, spin-coating, drying, and transferring to a nitrogen glove box; setting the temperature of a heating plate in a nitrogen glove box to be 300 ℃, placing the dried substrate on the heating plate for annealing for 10 minutes, and then taking down the substrate to cool to room temperature; repeating the spin-coating annealing step for 4 times to obtain Sb2S3Thin film (said Sb2S3The X-ray diffraction pattern of the film is shown in figure 1); then in Sb2S3A spiroo-OMeTAD (2, 2 ', 7, 7' -tetra- (dimethoxydiphenylamine) -spirofluorene) hole transport layer (3000 rpm/30 s) is spin-coated on the layer, and finally an Ag electrode is evaporated to form the device structure of FTO/c-TiO2/ Sb2S3a/spiro-OMeTAD/Ag solar cell. The solar cell prepared in this example had the following properties:
1. sb measured in room temperature environment under AM1.5 simulated sunlight condition2S5The solar cell prepared by the method using the ammonium sulfide solution as the precursor solution has obvious photovoltaic effect;
2. as shown in the J-V graph of the solar cell of fig. 2: the prepared solar cell has the open-circuit voltage of 0.56V and the short-circuit current density of 12.35mA/cm2The fill factor was 41.1%, and the photoelectric conversion efficiency was 2.84%.
Example 2
Using Sb2S5The ammonium sulfide solution is used as a precursor for preparing the solar cell, and the mesoporous solar cell has the following structure: FTO/c-TiO2/meso-TiO2/ Sb2S3First, the FTO substrate is cleaned and dense titanium dioxide (c-TiO) is added2) Spin coating on an FTO substrate (3000 r/30 s), and sintering in a high-temperature sintering furnace at 450 ℃ for 1 hour; after cooling, spin-coating a mesoporous titanium dioxide layer (meso-TiO) at 4000rpm2) Sintering at 500 ℃ for 1 hour, and cooling for later use; 0.4 g of Sb2S5Fully dissolving in 1 ml of 40wt% ammonium sulfide solution, and filtering supernatant for later use; placing the substrate on a spin coater, setting the rotation speed to be 2500rpm for 40 seconds, dropwise adding 40 microliter of filtrate, spreading the whole substrate, spin-coating, drying, and transferring to a nitrogen glove box; setting the temperature of a heating plate in a nitrogen glove box to be 320 ℃, placing the dried substrate on the heating plate for annealing for 5 minutes, and then taking down the substrate to cool to room temperature; repeating the spin-coating annealing step for 4 times to obtain Sb2S3A film; then in Sb2S3Spin-coating a spiro-OMeTAD hole transport layer (3000 r/30 s), and finally evaporating an Ag electrode to form a device structure of FTO/c-TiO2/ meso-TiO2/ Sb2S3a/spiro-OMeTAD/Ag solar cell. The solar cell prepared in this example had the following properties:
1. sb measured in room temperature environment under AM1.5 simulated sunlight condition2S5The solar cell prepared by the method using the ammonium sulfide solution as the precursor solution has obvious photovoltaic effect;
2. the prepared solar cell has the open-circuit voltage of 0.56V and the short-circuit current density of 11.96mA/cm2The fill factor was 43.0% and the photoelectric conversion efficiency was 2.87%.
Example 3
Sb2S5Dissolving in ammonium sulfide solution, filtering to obtain precursor, and preparing solar cell by using flat solar cell structure as follows: FTO/c-TiO2/ Sb2S3First, the FTO substrate is cleaned and dense titanium dioxide (c-TiO) is added2) Spin-coating on an FTO substrate (3000 rpm/30 s), sintering in a high-temperature sintering furnace at 450 ℃ for 4 hours, and cooling to room temperature for later use; 0.5 g of Sb2S5Fully dissolving in 1 ml of 20wt% ammonium sulfide solution, and filtering supernatant for later use; placing a substrate on a spin coater, setting the rotation speed to be 3000rpm for 30 seconds, dropwise adding 40 microliter of filtrate, spreading the whole substrate, spin-coating, drying, and transferring to a nitrogen glove box; setting the temperature of a heating plate in a nitrogen glove box to be 300 ℃, placing the dried substrate on the heating plate for annealing for 10 minutes, and then taking down the substrate to cool to room temperature; repeating the above spin coatingAnnealing for 7 times to obtain Sb2S3A film; then in Sb2S3Spin-coating a spiro-OMeTAD hole transport layer (3000 rpm/30 s) on the layer, and finally evaporating an Ag electrode to form the device structure of FTO/c-TiO2/ Sb2S3a/spiro-OMeTAD/Ag solar cell. The solar cell prepared in this example had the following properties:
1. sb measured in room temperature environment under AM1.5 simulated sunlight condition2S5The solar cell prepared by the method using the ammonium sulfide solution as the precursor solution has obvious photovoltaic effect;
2. the prepared solar cell has the open-circuit voltage of 0.57V and the short-circuit current density of 13.35mA/cm2The fill factor was 38.5%, and the photoelectric conversion efficiency was 2.93%.
In conclusion, the Sb-based material provided by the invention2S3The invention discloses a thin-film solar cell and a preparation method thereof, which adopts a solution method spin coating technology and uses ammonium sulfide to dissolve Sb2S5Preparing precursor, spin-coating annealing and preparing crystallized Sb2S3A film. Compared with the prior art, the method has the following advantages: 1. mature process, simple operation and repeatable preparation, and improves Sb2S3The film quality and the yield are improved, and the utilization rate of raw materials is improved; 2. spin coating at normal temperature to avoid low-temperature treatment in the existing solution method; 3. using Sb2S5Preparation of Sb by using ammonium sulfide solution as precursor2S3The number of spin-coating times is less than that of the previous times; 4. using Sb2S5Preparation of Sb by using ammonium sulfide solution as precursor2S3The film has rich sulfur source, and the prepared film has less impurities; 5. by accurately controlling the spin coating speed, the spin coating time and the annealing condition, the required film thickness and the adjustable film microstructure performance can be easily obtained according to requirements; 6. using Sb2S5The ammonium sulfide solution is used as a precursor, and a complex and expensive vacuum device is not needed for preparing the film.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (3)
1. A method for preparing a solar cell based on a solution method is characterized by comprising the following steps:
providing a substrate comprising a cathode;
forming an electron transport layer on the substrate;
forming Sb on the electron transport layer2S3A film; wherein said Sb2S3The preparation process of the film comprises the following steps: according to Sb2S5The mass ratio of the Sb to the ammonium sulfide solution is 0.1-12S5Dissolving in ammonium sulfide solution to form Sb2S5Filtering the complex with ammonium sulfide, and taking the supernatant for later use; spin coating the supernatant on the electron transport layer, and then sequentially drying and annealing to obtain the Sb2S3A film;
in the Sb2S3Forming a hole transport layer on the film;
forming an anode on the hole transport layer;
the concentration of the ammonium sulfide solution is 20-50 wt%;
the rotation speed of the spin coating is 500-6000rpm, and the spin coating time is 10-120 s;
the temperature of the annealing treatment is 240-400 ℃, and the time of the annealing treatment is 2-30 minutes.
2. A solar cell based on a solution method sequentially comprises a substrate containing a cathode, an electron transport layer and Sb from bottom to top2S3The thin film, the hole transport layer and the anode, wherein the solar cell is prepared by the method for preparing a solar cell based on the solution method according to claim 1.
3. The solution process-based solar cell according to claim 2, wherein the Sb2S3The thickness of the film is 50-1000 nm.
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Application publication date: 20190315 Assignee: Hengquan industry (Shenzhen) Co.,Ltd. Assignor: SHENZHEN University Contract record no.: X2022980023962 Denomination of invention: Solar cell based on solution method and its preparation method Granted publication date: 20201124 License type: Common License Record date: 20221201 |