CN113013286A - Antimony selenide film with high (hk1) crystal face abundance, antimony selenide film solar cell and preparation method thereof - Google Patents
Antimony selenide film with high (hk1) crystal face abundance, antimony selenide film solar cell and preparation method thereof Download PDFInfo
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- CN113013286A CN113013286A CN202110112201.0A CN202110112201A CN113013286A CN 113013286 A CN113013286 A CN 113013286A CN 202110112201 A CN202110112201 A CN 202110112201A CN 113013286 A CN113013286 A CN 113013286A
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- OQRNKLRIQBVZHK-UHFFFAOYSA-N selanylideneantimony Chemical compound [Sb]=[Se] OQRNKLRIQBVZHK-UHFFFAOYSA-N 0.000 title claims abstract description 152
- 239000013078 crystal Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000010409 thin film Substances 0.000 claims abstract description 58
- 239000010408 film Substances 0.000 claims abstract description 42
- 238000010438 heat treatment Methods 0.000 claims abstract description 38
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000000137 annealing Methods 0.000 claims description 70
- 239000000758 substrate Substances 0.000 claims description 59
- 239000011521 glass Substances 0.000 claims description 33
- 238000011065 in-situ storage Methods 0.000 claims description 23
- 230000031700 light absorption Effects 0.000 claims description 21
- 238000000151 deposition Methods 0.000 claims description 20
- 238000000859 sublimation Methods 0.000 claims description 19
- 230000008022 sublimation Effects 0.000 claims description 19
- 239000011669 selenium Substances 0.000 claims description 18
- 229910044991 metal oxide Inorganic materials 0.000 claims description 16
- 150000004706 metal oxides Chemical class 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- 238000007747 plating Methods 0.000 claims description 10
- 229910052711 selenium Inorganic materials 0.000 claims description 10
- 239000010931 gold Substances 0.000 claims description 9
- 239000000919 ceramic Substances 0.000 claims description 8
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 8
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 7
- 229910052737 gold Inorganic materials 0.000 claims description 7
- 238000004544 sputter deposition Methods 0.000 claims description 7
- 238000005092 sublimation method Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 6
- 239000013077 target material Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 230000000087 stabilizing effect Effects 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 238000001771 vacuum deposition Methods 0.000 claims description 2
- 239000000969 carrier Substances 0.000 abstract description 7
- 230000005540 biological transmission Effects 0.000 abstract description 6
- 231100000252 nontoxic Toxicity 0.000 abstract description 5
- 230000003000 nontoxic effect Effects 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 description 2
- 238000000861 blow drying Methods 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 238000007738 vacuum evaporation Methods 0.000 description 2
- 229910052774 Proactinium Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002202 sandwich sublimation Methods 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention provides an antimony selenide film with high (hk1) crystal face abundance, an antimony selenide film solar cell and a preparation method thereof, and solves the problems of low efficiency and poor stability of the conventional antimony selenide film solar cell. The invention adopts a nontoxic buffer layer to prepare FTO/SnO with a top lining structure2/Sb2Se3Au thin film solar cell or ITO/SnO2/Sb2Se3Au thin film solar cell and adopting heat treatment process to lead the antimony selenide thin film [221]]And [211]The preferred growth orientation is enhanced, the (hk1) crystal face abundance is improved, the transmission efficiency of carriers is promoted, and the device efficiency is improved. The nontoxic solar cell can be prepared in a large area, has no pollution in the whole preparation process, and is suitable for industrial production and application.
Description
Technical Field
The invention belongs to the technical field of photoelectron materials and devices, and particularly relates to an antimony selenide film with high (hk1) crystal face abundance, an antimony selenide film solar cell and a preparation method thereof.
Background
With the continuous growth of the global population and the vigorous development of the socioeconomic performance, the demand of energy is increasing, and the shortage of energy has become a critical issue of the world attention. The development and utilization of new energy resources are concerned, and among a plurality of new energy resources, the thin film solar cell has the characteristics of low raw material consumption, portability, flexibility and the like and is always a research hotspot In the energy field, wherein Copper Indium Gallium Selenide (CIGS) and cadmium telluride (CdTe) are successfully commercialized, but because the raw materials In and Ga are expensive and Cd have biological toxicity, the self development is limited, and the cheap and nontoxic solar cell material needs to be continuously explored.
Antimony selenide belongs to a V-VI group inorganic semiconductor material and has a chemical formula of Sb2Se3Only one orthorhombic phase is available at normal pressure, the selenium and the antimony are abundant in reserves and low in price, and the antimony selenide has proper forbidden bandwidth (-1.17 eV), good photoelectric response, larger absorption coefficient in ultraviolet and visible light regions, better chemical stability and non-volatilityIs suitable for being used as the light absorption layer material of inorganic thin-film solar cells.
At present, the preferred growth planes of the existing antimony selenide thin-film solar cells are mostly (221), (230) and (120), wherein the transmission efficiency of a photon-generated carrier is reduced due to more (hk0) crystal planes, and the efficiency of the solar cell is further lower. Meanwhile, the existing antimony selenide thin-film solar cell mainly adopts CdS as a buffer layer, the biotoxicity of Cd and Cd+Diffusion at the heterojunction interface also leads to poor device stability.
Disclosure of Invention
The invention aims to solve the problems of low efficiency and poor stability of the conventional antimony selenide thin-film solar cell, and provides an antimony selenide thin-film with high (hk1) crystal face abundance, an antimony selenide thin-film solar cell and a preparation method thereof.
In order to achieve the purpose, the technical solution provided by the invention is as follows:
the method for improving the abundance of the crystal face of the antimony selenide film (hk1) is characterized in that the antimony selenide film is subjected to in-situ annealing or selenization annealing, so that the antimony selenide film preferentially grows along the direction of [221] and/or [211 ].
Further, the in-situ annealing is specifically as follows: cooling the antimony selenide film prepared by the near-space sublimation method to room temperature along with a furnace, and carrying out in-situ annealing at 300-400 ℃ for 20-40 min;
the specific mode of the selenization annealing is as follows: and (3) placing the antimony selenide film prepared by the near-space sublimation method in a selenium atmosphere, vacuumizing to 1-5 Pa, and performing selenization annealing at 300-400 ℃ for 20-40 min.
Meanwhile, the invention also provides the antimony selenide film with high (hk1) face abundance, which is prepared by the method.
An antimony selenide thin-film solar cell with high (hk1) crystal face abundance is characterized in that a glass substrate, a transparent conductive metal oxide layer, an N-type buffer layer, an antimony selenide light absorption layer and an electrode layer are sequentially arranged from bottom to top;
wherein, the antimony selenide light absorption layer adopts the antimony selenide film with high (hk1) crystal face abundance prepared by the method;
the N-type buffer layer is SnO2A buffer layer.
Further, the transparent conductive metal oxide layer is ITO (indium tin oxide) or FTO (fluorine-doped SnO)2) The thickness is 150-200 nm;
the SnO2The thickness of the buffer layer is 50-120 nm;
the thickness of the antimony selenide light absorption layer is 600-1500 nm;
the electrode is a gold electrode with a thickness of 50-100 nm.
The invention also provides a preparation method of the antimony selenide thin-film solar cell, which is characterized by comprising the following steps:
1) plating a transparent conductive metal oxide layer on the surface of the glass substrate;
2) cleaning the glass substrate plated with the transparent conductive metal oxide layer in the step 1);
3) deposition of SnO on the upper surface of a transparent conductive metal oxide layer2Buffer layer and for SnO2Annealing the buffer layer;
4) at SnO2An antimony selenide light absorption layer grows on the upper surface of the buffer layer;
5) carrying out heat treatment on the antimony selenide light absorption layer by adopting in-situ annealing or selenizing annealing;
6) and plating an electrode on the upper surface of the antimony selenide light absorption layer to form the antimony selenide thin-film solar cell.
Further, step 3) adopts a magnetron sputtering method to deposit SnO on the upper surface of the transparent conductive metal oxide layer2The buffer layer comprises the following specific steps:
3.1) fixing the glass substrate cleaned in the step 2) on a sample table, placing the glass substrate into a vacuum chamber, and enabling the magnetron sputtering target to be opposite to the upper surface of the glass substrate at a distance of 10 cm;
3.2) evacuating to make the vacuum degree of the chamber reach 2X 10-4Heating the sample table to 100-400 ℃ after Pa;
3.3) use of SnO with a purity of 4N2A target material is used as a target material,at Ar/O2Sputtering under the pressure of 1-5 Pa in the atmosphere of 1: 1 for 2-5 min, and depositing SnO on the upper surface of the transparent conductive metal oxide2A buffer layer;
3.4) deposition of SnO in step 3.3)2And placing the glass substrate of the buffer layer in an annealing furnace, and annealing at 400-500 ℃ for 20-40 min in an air atmosphere.
Further, step 4) adopts a close space sublimation method to perform SnO2The antimony selenide light absorption layer grows on the upper surface of the buffer layer, and the method comprises the following specific steps:
4.1) installing a graphite mask on an upper heating table of a sublimation furnace chamber, installing an AlN ceramic plate on a lower heating table, and placing an antimony selenide growth source on the AlN ceramic plate;
4.2) depositing SnO in the step 3)2The glass substrate of the buffer layer is arranged on the graphite mask and is arranged opposite to the antimony selenide growth source, the distance between the glass substrate and the antimony selenide growth source is 5-10 mm, and the chamber is closed;
4.3) vacuumizing the chamber of the sublimation furnace to 5Pa, introducing 100Pa high-purity Ar gas, vacuumizing to 5Pa, repeating the operation until residual air in the chamber of the sublimation furnace is removed, and stabilizing the air pressure in the chamber of the sublimation furnace to 5 Pa;
4.4) growing source of antimony selenide and depositing SnO2Heating the glass substrate of the buffer layer to 200 ℃, and preserving the heat for 200-300S; after the heat preservation is finished, the temperature of the antimony selenide growth source is increased to 430-550 ℃, the temperature of the glass substrate is increased to 200-300 ℃, the growth time is 10-120 min, and the growing time is SnO2And an antimony selenide film is grown on the upper surface of the buffer layer.
Further, in the step 5), the in-situ annealing is to cool the antimony selenide film obtained in the step 4.4) to room temperature along with the furnace, and then both an upper heating table and a lower heating table of the sublimation furnace are heated to 300-400 ℃ for in-situ annealing, wherein the annealing time is 20-40 min;
and the selenizing annealing is to cool the antimony selenide film obtained in the step 4.4) to room temperature along with the furnace, take out an antimony selenide growth source, place the selenium source, close the chamber, vacuumize to 1-5 Pa, then heat the upper heating table and the lower heating table of the sublimation furnace to 300-400 ℃ for selenizing annealing, wherein the annealing time is 20-40 min.
Further, in the step 6), an electrode is plated on the upper surface of the antimony selenide light absorption layer by a vacuum evaporation method to form the antimony selenide thin-film solar cell.
The invention has the advantages that:
1. the invention adopts annealing modification to improve the abundance of the crystal face of the antimony selenide film (hk1) and has specific preferred orientation, especially in [221]]And [211]These two directions; edge [221]]And [211]Epitaxially grown (Se)4Sb6) The nano-band is inclined and vertical to the substrate, photogenerated carriers can be more transported in the band, the transport efficiency of the carriers is promoted, and therefore the jump between the bands is reduced, and the van der Waals force needs to be overcome when the jump between the bands is carried out, so that the Sb is enabled to be in situ annealed or selenized annealed specially to ensure that the Sb is in situ annealed2Se3The diffraction peaks of the (221) and (211) crystal planes of the film are stronger, and the prepared solar cell has higher short-circuit current density.
2. The invention adopts a nontoxic buffer layer to avoid Cd+The problem of poor stability of the device caused by diffusion at a heterojunction interface is solved, and FTO/SnO of a top lining structure is prepared2/Sb2Se3Au thin film solar cell or ITO/SnO2/Sb2Se3Au thin film solar cell and SnO2The buffer layer and the antimony selenide film are respectively subjected to heat treatment to promote SnO2Crystallinity of buffer layer, and making antimony selenide thin film [221]And [211]The preferred growth orientation is enhanced, the (hk1) crystal face abundance is improved, the transmission efficiency of current carriers is promoted, and the device efficiency is improved; the nontoxic solar cell can be prepared in a large area, is pollution-free in the whole preparation process, and is suitable for industrial production and application.
3. In the process of preparing the antimony selenide film, the melting point of selenium is lower, so that selenium is easy to lose when the antimony selenide is decomposed, and a selenium vacancy defect is formed.
Drawings
FIG. 1 is an antimony selenide thin film solar cell structure;
FIG. 2 is an X-ray diffraction pattern of an antimony selenide film under different treatment modes: (a) unannealed, (b) in-situ annealed, (c) selenization annealed;
fig. 3 is an SEM image of antimony selenide thin films under different processing modes: (a) in-situ annealing, (b) selenization annealing, (c) no annealing;
FIG. 4 is a J-V spectrum of an antimony selenide thin film solar cell: (a) unannealed, (b) in-situ annealed, (c) selenization annealed.
FIG. 5 is a J-V spectrum of an antimony selenide thin-film solar cell during selenization annealing at different temperatures.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
as shown in fig. 1, the antimony selenide thin-film solar cell sequentially comprises a glass substrate, a transparent conductive metal oxide layer, an N-type buffer layer, an antimony selenide light absorption layer and an electrode layer from bottom to top;
wherein the antimony selenide light absorption layer adopts an antimony selenide film with high (hk1) crystal face abundance, and the thickness is 600-1500 nm; the N-type buffer layer is SnO2A buffer layer with a thickness of 50-120 nm; the transparent conductive metal oxide layer is ITO or FTO, and the thickness is 150-200 nm; the electrode is a gold electrode with a thickness of 50-100 nm.
Example 1
The specific preparation method of the antimony selenide thin-film solar cell comprises the following steps:
1) plating an ITO layer with the thickness of 150nm on the surface of a glass substrate by adopting the existing deposition method or directly purchasing the glass substrate plated with the ITO layer as a substrate;
2) cleaning the glass substrate plated with the ITO layer in the step 1);
and sequentially using acetone, absolute ethyl alcohol and deionized water to respectively ultrasonically clean the substrate in an ultrasonic cleaning machine for 20min, flushing the substrate with the deionized water to remove residues of the original solvent before replacing the solvent each time, blow-drying the substrate which is ultrasonically cleaned by using high-pressure nitrogen, and placing the substrate into a container in which dust-free paper is laid.
3) Depositing SnO on the upper surface of the transparent conductive metal oxide layer by adopting a magnetron sputtering method2A buffer layer;
3.1) fixing the substrate cleaned in the step 2) on a sample table, placing the substrate into a vacuum chamber, and enabling the magnetron sputtering target to be opposite to the upper surface of the substrate at a distance of 10 cm;
3.2) evacuating to make the vacuum degree of the chamber reach 2X 10-4After Pa, heating the sample table to 100 ℃;
3.3) use of SnO with a purity of 4N2Sputtering the target material in the atmosphere of Ar/O2 of 1: 1 at the working pressure of 1Pa for 3min, cooling the chamber to room temperature after the sputtering is finished, taking out the sample to obtain the SnO coated with the coating with the thickness of 75nm2A substrate of a buffer layer;
3.4) deposition of SnO in step 3.3)2And (3) placing the substrate of the buffer layer in an annealing furnace, annealing at 450 ℃ for 30min in an air atmosphere, cooling to room temperature along with the furnace, and taking out.
4) In SnO by adopting near space sublimation method2An antimony selenide light absorption layer grows on the upper surface of the buffer layer;
4.1) preparation of antimony selenide growth source
3g of antimony selenide Sb were weighed on an electronic balance2Se3Pouring the powder into a specific die, and pressing for 120s under the pressure of 12.5MPa by using a tablet press to obtain an antimony selenide tablet with the diameter of 20 mm;
4.2) opening the cavity, installing a graphite mask on a heating table in the sublimation furnace cavity, installing an AlN ceramic plate on a lower heating table, and placing the antimony selenide growth source prepared in the step 4.1) on the AlN ceramic plate, wherein at the moment, the through hole of the graphite mask is positioned right above the antimony selenide growth source;
4.3) depositing SnO in the step 3)2The substrate of the buffer layer is arranged at the through hole of the graphite mask plate and is arranged opposite to the antimony selenide growth source, the distance between the antimony selenide growth source and the substrate is adjusted to be 10mm, and the chamber is closed;
4.4) vacuumizing the chamber of the sublimation furnace to 5Pa, introducing 100Pa high-purity Ar gas, vacuumizing to 5Pa, removing residual air in the chamber of the sublimation furnace by performing the operation for 3-5 times, and finally stabilizing the gas pressure in the chamber of the sublimation furnace at 5 Pa;
4.5) growing source of antimony selenide and depositing SnO2Heating the substrate to 200 ℃, and preserving heat for 300S; after the heat preservation is finished, the temperature of the antimony selenide growth source is increased to 500 ℃, the temperature of the glass substrate is increased to 250 ℃, the growth time is 900s, and the growing time is SnO2And an antimony selenide film is grown on the upper surface of the buffer layer.
5) Adopting a vacuum evaporation plating machine, and evaporating a gold electrode on the surface of the antimony selenide by using a special mask, wherein the thickness of the gold electrode is 80 nm; and obtaining the antimony selenide thin-film solar cell.
The embodiment does not anneal the grown antimony selenide thin film, and the X-ray diffraction pattern of the antimony selenide thin film is shown as (a) in figure 2, the SEM image is shown as (c) in figure 3, and the J-V pattern of the antimony selenide thin film solar cell is shown as (a) in figure 4;
example 2
The differences from example 1 are limited only to: and 4) after the growth of the antimony selenide film is finished in the step 4), cooling the antimony selenide film to room temperature along with the furnace, opening the chamber, taking out the antimony selenide growth source, putting the selenium source, closing the chamber, vacuumizing to 5Pa, then heating the upper heating table and the lower heating table to 350 ℃ for selenylation annealing, wherein the annealing time is 30min, and thus the antimony selenide film is subjected to selenylation annealing.
In the example, the growing antimony selenide thin film is subjected to selenization annealing, and the X-ray diffraction pattern of the antimony selenide thin film is shown as (c) in fig. 2, the SEM image is shown as (b) in fig. 3, and the J-V pattern of the antimony selenide thin film solar cell is shown as (c) in fig. 4.
Example 3
The differences from example 1 are limited only to: after the growth of the antimony selenide film in the step 4), reducing the temperature in the chamber of the sublimation furnace to room temperature, then heating to 350 ℃ for in-situ annealing, wherein the annealing time is 30min, namely, the in-situ annealing is carried out on the antimony selenide film.
In the embodiment, the grown antimony selenide thin film is subjected to in-situ annealing, and the X-ray diffraction pattern of the antimony selenide thin film is shown as (b) in figure 2, the SEM image is shown as (a) in figure 3, and the J-V pattern of the antimony selenide thin film solar cell is shown as (b) in figure 4.
Examples 1 to 3 show that, as shown in the comparison graph of the surface morphology of the SEM of the antimony selenide thin film in fig. 3, it can be seen that there is no sharp crystal grain shape before annealing and a small number of pores exist between the crystal grains, and these pores can block the transmission of carriers, thereby reducing the performance of the device, and the surface pores of the antimony selenide thin film after in-situ annealing or selenization annealing are obviously reduced, the thin film is more compact, the crystal grains are more rounded, the more rounded crystal grains, the antimony selenide thin film with higher density, and the N-type buffer layer (in this embodiment, the N-type buffer layer is SnO2The buffer layer, certainly, other types of N-type buffer layers, for example, a CdS buffer layer) constitutes a high-quality P-N junction, so that the collection and separation efficiency of photogenerated carriers is improved, and the open-circuit voltage is improved. The invention prepares Sb under different annealing modes2Se3The J-V test of the thin-film solar cell under the standard am1.5g simulated solar illumination obtains various performance parameters of the solar cell, and as a result, as shown in fig. 4, it can be seen that the open-circuit voltage after annealing treatment is improved, which indicates that the annealing plays a forward promoting role in the open-circuit voltage of the device.
FIG. 2 is an XRD spectrum of an antimony selenide film, after annealing, the peak position of the film as a whole is kept unchanged, and all main diffraction peaks are consistent with the standard PDF card of antimony selenide (JCPDS No. 00-015-]And [211]The enhancement of the peak enables the abundance of the (hk1) crystal plane to be improved, the better crystallinity and the abundance of the (hk1) crystal plane enable the short-circuit current density of the solar cell to be further increased, and the short-circuit current density of the film after in-situ annealing is increased (see fig. 4); after selenization annealing, the crystallinity of the antimony selenide film is better, the abundance of the crystal face of the antimony selenide film (hk1) is improved, and the strongest peak is [221]]And [211]Peak with reduced (hk0) face abundance comprising [ 120%]、[230]、[240]The peak is obviously weakened, and the number of the mixed peaks is less; more (hk1) crystal planes make the carriers easier to be in (Se)4Sb6) The covalent bond transmission between the nano-belts is realized, so the transmission efficiency of the current carrier is further improvedHigh, a higher short-circuit current density is obtained (see fig. 4), and thus the device efficiency is further improved. Thus, it can also be seen that the selenization annealing is more effective than the in-situ annealing under the same conditions.
Example 4
The specific preparation method of the antimony selenide thin-film solar cell with high (hk1) crystal face abundance is as follows:
1) plating an FTO layer with the thickness of 200nm on the surface of a glass substrate, or directly purchasing the glass substrate plated with the FTO layer as a substrate;
2) cleaning the glass substrate plated with the FTO layer in the step 1);
and sequentially using acetone, absolute ethyl alcohol and deionized water to respectively ultrasonically clean the substrate in an ultrasonic cleaning machine for 20min, flushing the substrate with the deionized water to remove residues of the original solvent before replacing the solvent each time, blow-drying the substrate which is ultrasonically cleaned by using high-pressure nitrogen, and placing the substrate into a container in which dust-free paper is laid.
3) Depositing SnO on the upper surface of the transparent conductive metal oxide layer by adopting a magnetron sputtering method2A buffer layer;
3.1) fixing the substrate cleaned in the step 2) on a sample table, placing the substrate into a vacuum chamber, and enabling the magnetron sputtering target to be opposite to the upper surface of the substrate at a distance of 10 cm;
3.2) evacuating to make the vacuum degree of the chamber reach 2X 10-4After Pa, heating the sample table to 100 ℃;
3.3) use of SnO with a purity of 4N2Target material, working pressure 1-5 Pa, in Ar/O2Sputtering in the atmosphere of 1: 1 for 3min, taking out the sample when the temperature of the chamber is reduced to room temperature after the sputtering is finished, and obtaining SnO with the thickness of 75nm2A buffer layer;
3.4) deposition of SnO in step 3.3)2And (3) placing the substrate of the buffer layer in an annealing furnace, annealing at 400 ℃ for 40min in an air atmosphere, cooling to room temperature along with the furnace, and taking out.
4) In SnO by adopting near space sublimation method2An antimony selenide light absorption layer grows on the upper surface of the buffer layer;
4.1) preparation of antimony selenide growth source
Weighing 3g of antimony selenide powder on an electronic balance, pouring the antimony selenide powder into a specific mould, and pressing the antimony selenide powder for 120s under the pressure of 12.5MPa by using a tablet press to obtain an antimony selenide tablet with the diameter of 20 mm;
4.2) opening the cavity, arranging an AlN ceramic plate on a heating table below the sublimation furnace cavity, arranging a graphite mask on an upper heating table, and placing the antimony selenide growth source prepared in the step 4.1) on the AlN ceramic plate, wherein at the moment, the through hole of the graphite mask is positioned right above the antimony selenide growth source;
4.3) depositing SnO in the step 3)2The substrate is arranged at the through hole of the graphite mask plate and is arranged opposite to the antimony selenide growth source, the distance between the antimony selenide growth source and the substrate is adjusted to be 5-10 mm, and the chamber is closed;
4.4) vacuumizing the chamber of the growth furnace to 5Pa, introducing 100Pa high-purity Ar gas, vacuumizing to 5Pa, removing residual air in the chamber of the sublimation furnace by the operation for 3-5 times, and finally stabilizing the pressure of the chamber of the growth furnace at 5 Pa;
4.5) growing source of antimony selenide and depositing SnO2Heating the substrate to 200 ℃, and keeping the temperature for 200-300S; after the heat preservation is finished, the temperature of the antimony selenide growth source is increased to 470 ℃, the temperature of the glass substrate is increased to 250 ℃, the growth time is 60min, and the growing time is SnO2And an antimony selenide film is grown on the upper surface of the buffer layer.
5) Carrying out heat treatment on the antimony selenide light absorption layer by adopting selenizing annealing;
after growth is finished, the chamber is self-heated and cooled to room temperature, the chamber is opened, an antimony selenide growth source is taken out, a selenium source is put in, the chamber is closed, vacuum pumping is carried out to 1-5 Pa, then the upper heating table and the lower heating table are both heated to 300 ℃ for selenide annealing, the annealing time is 30min,
6) adopting a vacuum evaporation plating machine, and carrying out gold evaporation plating on the surface of the antimony selenide by using a special mask, wherein the thickness of the electrode is 80 nm; and obtaining the antimony selenide thin-film solar cell.
The main process differences between examples 5 to 14 and example 4 are detailed in table 1, with the remainder being adjusted within the appropriate ranges:
table 1 example 5 to example 14 main process conditions
ITO or FTO with a thickness of 150 to 200nm is coated on the surface of the glass substrate selected in embodiments 5 to 14, and SnO with a thickness of 50 to 120nm is deposited on the upper surface of the glass substrate by sputtering for different times2Buffer layer, under the regulation and control of different temperatures and deposition time, in SnO2Depositing an antimony selenide film with the thickness of 600-1500 nm on the buffer layer, and then performing the heat treatment process (to be noted, the heat treatment process aims at SnO2The heat treatment process of the buffer layer, the annealing temperature of the embodiments 6, 12 and 13 is 500 ℃, and the annealing time is 20 min; annealing temperature of 400-500 ℃ and annealing time of 20-40 min in other embodiments) and finally evaporating a gold electrode with thickness of 50-100 nm to form the antimony selenide thin-film solar cell. The invention detects the performance of the antimony selenide thin-film solar cell prepared by each embodiment, and improves the short-circuit current. Meanwhile, the J-V test of the antimony selenide thin-film solar cells obtained in examples 6, 12 and 13 under the standard am1.5g simulated solar illumination is performed, as shown in fig. 5, it can be seen that under the same conditions, when the annealing temperature is 350 ℃, the short-circuit current density of the antimony selenide thin-film solar cells is higher, and the device efficiency is higher.
Claims (10)
1. A method for improving the abundance of the crystal face of an antimony selenide thin film (hk1), which is characterized by comprising the following steps: and carrying out in-situ annealing or selenization annealing on the antimony selenide thin film to ensure that the antimony selenide thin film preferentially grows along the [221] and/or [211] direction.
2. The method for improving the abundance of the crystal planes of the antimony selenide thin film (hk1) according to claim 1, wherein:
the in-situ annealing is specifically as follows: cooling the antimony selenide film prepared by the near-space sublimation method to room temperature along with a furnace, and carrying out in-situ annealing at 300-400 ℃ for 20-40 min;
the specific mode of the selenization annealing is as follows: and (3) placing the antimony selenide film prepared by the near-space sublimation method in a selenium atmosphere, vacuumizing to 1-5 Pa, and performing selenization annealing at 300-400 ℃ for 20-40 min.
3. An antimony selenide thin film having a high (hk1) lattice plane abundance prepared by the method of claim 1 or 2.
4. An antimony selenide thin-film solar cell with high (hk1) crystal plane abundance, which is characterized in that: the structure of the light-absorbing electrode sequentially comprises a glass substrate, a transparent conductive metal oxide layer, an N-type buffer layer, an antimony selenide light-absorbing layer and an electrode layer from bottom to top;
wherein, the antimony selenide light absorption layer adopts the antimony selenide film with high (hk1) crystal face abundance prepared by the method of claim 1 or 2;
the N-type buffer layer is SnO2A buffer layer.
5. The antimony selenide thin-film solar cell according to claim 4, wherein:
the transparent conductive metal oxide layer is ITO or FTO, and the thickness is 150-200 nm;
the SnO2The thickness of the buffer layer is 50-120 nm;
the thickness of the antimony selenide light absorption layer is 600-1500 nm;
the electrode is a gold electrode with a thickness of 50-100 nm.
6. The method for preparing the antimony selenide thin-film solar cell as claimed in claim 4 or 5, which is characterized by comprising the following steps:
1) plating a transparent conductive metal oxide layer on the surface of the glass substrate;
2) cleaning the glass substrate plated with the transparent conductive metal oxide layer in the step 1);
3) on the transparent conductive metal oxide layerSurface deposited SnO2Buffer layer and for SnO2Annealing the buffer layer;
4) at SnO2An antimony selenide light absorption layer grows on the upper surface of the buffer layer;
5) carrying out heat treatment on the antimony selenide light absorption layer by adopting in-situ annealing or selenizing annealing;
6) and plating an electrode on the upper surface of the antimony selenide light absorption layer to form the antimony selenide thin-film solar cell.
7. The preparation method of the antimony selenide thin-film solar cell according to claim 6, wherein the step 3) adopts a magnetron sputtering method to deposit SnO on the upper surface of the transparent conductive metal oxide layer2The buffer layer comprises the following specific steps:
3.1) fixing the glass substrate cleaned in the step 2) on a sample table, placing the glass substrate into a vacuum chamber, and enabling the magnetron sputtering target to be opposite to the upper surface of the glass substrate at a distance of 10 cm;
3.2) evacuating to make the vacuum degree of the chamber reach 2X 10-4Heating the sample table to 100-400 ℃ after Pa;
3.3) use of SnO with a purity of 4N2Target material in Ar/O2Sputtering under the pressure of 1-5 Pa in the atmosphere of 1: 1 for 2-5 min, and depositing SnO on the upper surface of the transparent conductive metal oxide2A buffer layer;
3.4) deposition of SnO in step 3.3)2And placing the glass substrate of the buffer layer in an annealing furnace, and annealing at 400-500 ℃ for 20-40 min in an air atmosphere.
8. The method for preparing the antimony selenide thin-film solar cell according to claim 7, wherein the step 4) adopts a near space sublimation method to perform SnO2The antimony selenide light absorption layer grows on the upper surface of the buffer layer, and the method comprises the following specific steps:
4.1) installing a graphite mask on an upper heating table of a sublimation furnace chamber, installing an AlN ceramic plate on a lower heating table, and placing an antimony selenide growth source on the AlN ceramic plate;
4.2) depositing SnO in the step 3)2Of buffer layersThe glass substrate is arranged on the graphite mask and is arranged opposite to the antimony selenide growth source, the distance between the glass substrate and the antimony selenide growth source is 5-10 mm, and the chamber is closed;
4.3) vacuumizing the chamber of the sublimation furnace to 5Pa, introducing 100Pa high-purity Ar gas, vacuumizing to 5Pa, repeating the operation until residual air in the chamber of the sublimation furnace is removed, and stabilizing the air pressure in the chamber of the sublimation furnace to 5 Pa;
4.4) growing source of antimony selenide and depositing SnO2Heating the glass substrate of the buffer layer to 200 ℃, and preserving the heat for 200-300S; after the heat preservation is finished, the temperature of the antimony selenide growth source is increased to 430-550 ℃, the temperature of the glass substrate is increased to 200-300 ℃, the growth time is 10-120 min, and the growing time is SnO2And an antimony selenide film is grown on the upper surface of the buffer layer.
9. The method for preparing an antimony selenide thin-film solar cell according to claim 8, wherein:
in the step 5), the in-situ annealing is to cool the antimony selenide film obtained in the step 4.4) to room temperature along with the furnace, and then both an upper heating table and a lower heating table of the sublimation furnace are heated to 300-400 ℃ for in-situ annealing, wherein the annealing time is 20-40 min;
and the selenizing annealing is to cool the antimony selenide film obtained in the step 4.4) to room temperature along with the furnace, take out an antimony selenide growth source, place the selenium source, close the chamber, vacuumize to 1-5 Pa, then heat the upper heating table and the lower heating table of the sublimation furnace to 300-400 ℃ for selenizing annealing, wherein the annealing time is 20-40 min.
10. The method for preparing an antimony selenide thin-film solar cell according to claim 9, wherein:
and 6), plating an electrode on the upper surface of the antimony selenide light absorption layer by adopting a vacuum evaporation method to form the antimony selenide thin-film solar cell.
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