CN113913794B - AgBiS 2 Film, preparation method and application thereof - Google Patents

AgBiS 2 Film, preparation method and application thereof Download PDF

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CN113913794B
CN113913794B CN202111168824.6A CN202111168824A CN113913794B CN 113913794 B CN113913794 B CN 113913794B CN 202111168824 A CN202111168824 A CN 202111168824A CN 113913794 B CN113913794 B CN 113913794B
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CN113913794A (en
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林乾乾
姚方
江力
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Wuhan University WHU
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
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    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/30—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising bulk heterojunctions, e.g. interpenetrating networks of donor and acceptor material domains
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Abstract

The invention relates to AgBiS 2 The preparation method comprises the following steps: according to the proportion of Ag: bi = 1:1-3 molar ratio is added to waterAdding soluble thiosulfate with the sulfur molar weight not lower than the sum of Ag and Bi into soluble silver salt and soluble bismuth salt, uniformly mixing, and adding acid to adjust the pH value to be =3 to obtain a precursor solution; in the precursor solution, cations of soluble thiosulfate, soluble silver salt, soluble bismuth salt and anions of acid do not participate in deposition reaction; placing the substrate in the precursor solution, standing and depositing for at least 30 minutes at 80 +/-5 ℃, and taking out the substrate; annealing the substrate in air at 80-300 ℃ to obtain the AgBiS attached 2 A substrate of a thin film. The preparation method has the advantages of simple operation, mild reaction conditions, low cost, low requirements on equipment and environment and the like, and the prepared AgBiS 2 The film has high quality, good optical and electrical properties, good photovoltaic performance and good detection performance, and has great application potential in the photoelectric field.

Description

AgBiS 2 Film, preparation method and application thereof
Technical Field
The invention relates to the technical field of manufacturing of light absorption layer materials of photoelectric devices, in particular to AgBiS 2 A film, a preparation method and application thereof.
Background
AgBiS 2 Is a nontoxic and abundant material, has proper forbidden band width (about 1.1 eV) and high ultraviolet-near infrared absorption coefficient (about 10 eV) 5 cm -1 ) It is one of the most promising materials in the field of optoelectronics. Based on AgBiS 2 The solar cell made of the material has ultrahigh stability, achieves the photoelectric conversion efficiency of over 6.4 percent, and has great application potential in the field of photovoltaics. However, efficient optoelectronic devices are all based on AgBiS 2 Quantum dot implementation. The synthesis steps of the quantum dots are complex, and series of projects such as surface ligand regulation and control have great influence on the performance of materials and devices. AgBiS of nano-scale grain size 2 It is difficult to deposit a film with sufficient thickness and large crystal grains, which limits the application of the film in photoelectric devices. Thus, simple AgBiS was developed 2 Thin film fabrication techniques are necessary.
At present, agBiS 2 The film mostly adopts the traditional solution methods of molecular precursor, sol-gel, colloid nanocrystalline and the like, and the precursor is used for preparing AgBiS 2 Thin film method due to thermal decomposition reaction, resulting in AgBiS 2 The quality of the film is reduced, and holes are easy to appear; preparation of AgBiS from colloidal nanocrystals 2 Method of producing filmThe method has complex process, needs inert gas protection, multiple centrifugal cleaning of surface ligands and other complex operations.
In the Chemical Bath Deposition (CBD) method, ions are directly adsorbed on a substrate to form a film, and other residues are left in the solution, so that the film has few impurities and is simple to operate. However, the chemical bath deposition method produces AgBiS 2 In-process Ag of film 2 S and Bi 2 S 3 The deposition rate is difficult to keep balance, resulting in AgBiS 2 The film is doped with Ag 2 S or Bi 2 S 3 Isocratic, poorly crystalline, and even amorphous deposits. As any holes and non-uniformity in the film can cause complete or partial short circuit of the device and further affect the performance of the device, the AgBiS with single phase, high quality and excellent photoelectric device performance prepared by a chemical bath deposition method does not exist at present 2 Thin film report.
Disclosure of Invention
Aiming at the problem that AgBiS with single phase, high quality and excellent photoelectric device performance cannot be prepared by a chemical bath deposition method in the prior art 2 The invention prepares AgBiS with high purity, large crystal grains and high quality by regulating the chemical composition of the precursor, the chemical environment, the film deposition time and the annealing temperature and utilizing a chemical bath deposition method under the low temperature condition 2 Film, which can meet the requirements of solar cells and photodetectors (visible light and X-ray), in AgBiS 2 The preparation of the film shows great application potential.
The technical scheme provided by the invention is as follows:
in a first aspect, the present invention provides a method for preparing AgBiS 2 A method of making a film comprising the steps of:
according to the proportion of Ag: adding soluble silver salt and soluble bismuth salt into water according to the molar ratio of Bi = 1:1-3, adding soluble thiosulfate with the sulfur molar weight not lower than the sum of Ag and Bi, uniformly mixing, and adding acid to adjust the pH value =3 to obtain a precursor solution; in the precursor solution, cations of soluble thiosulfate, soluble silver salt, soluble bismuth salt and anions of acid do not participate in deposition reaction;
placing the substrate in the precursor solution, standing and depositing for at least 30 minutes at 80 +/-5 ℃, and taking out the substrate;
annealing the substrate in air at 80-300 ℃ to obtain the AgBiS attached 2 A substrate of a thin film.
By adopting the technical scheme, the invention can rapidly prepare the high-quality AgBiS with the crystal grain of about 150nm under the low-temperature condition 2 A film.
Preferably, the molar amount of sulfur is 5 to 20 times the sum of Ag and Bi; further, the molar weight of sulfur is 8 to 15 times of the sum of Ag and Bi; further, the molar amount of sulfur is 10 times the sum of Ag and Bi.
Preferably, the Ag concentration in the precursor solution is 0.001-0.01 mol/L; further, the concentration of Ag in the precursor solution is 0.002mol/L. In a further preferred embodiment of the above process, the molar ratio of Ag to Bi in the precursor solution is 1:2, at which ratio AgBiS is obtained 2 Absence of Ag in the film 2 S and AgBi 3 S 5 And the like.
As a further preferable mode of the above technical solution, a CdS thin film is provided on the substrate, and further, the CdS thin film is prepared by a chemical bath deposition method.
As a further preferred aspect of the above technical solution, the annealing temperature is 200 + -5 deg.C, at which temperature AgBiS is present 2 Thin film solar cells have the best photovoltaic performance.
As a further preferred aspect of the above technical solution, the soluble silver salt is AgCl; the soluble bismuth salt is BiCl 3 The soluble thiosulfate is sodium thiosulfate or hydrate thereof, the acid is hydrochloric acid, and sodium ions and chloride ions do not participate in the deposition reaction, so that AgBiS is avoided 2 Other metal salts are deposited in the film, and AgBiS is further improved 2 Purity of the film.
In a second aspect, the invention provides an AgBiS prepared by the above method 2 AgBiS prepared by thin film method 2 The film has the advantages of compact growth, larger crystal particles (more than 100 nm), good appearance and no holes, and is favorable for improving the photoelectric property of the film material.
In a third aspect, the present invention provides AgBiS 2 The thin film is applied to the preparation of solar cells and visible light and X-ray photoelectric detectors.
The invention has the following advantages and beneficial effects:
(1) The invention adopts a chemical bath deposition method to deposit AgBiS on a substrate 2 The method is simple and efficient, the thickness of the film is controllable, the components of the film are controllable, the requirements on equipment and preparation environment are low, the energy consumption is low, the utilization rate of raw materials is high, the cost is low, and the method is suitable for large-scale production.
(2) The preparation method of the invention can obtain uniform and pure cubic phase AgBiS 2 Film, agBiS 2 The film is compact, the crystal particles are large (about 150 nm), the appearance is good, and no holes exist. AgBiS prepared by the invention 2 The films have significant long-term stability on storage in air and under light, without encapsulation.
(3) AgBiS prepared by chemical bath deposition method 2 The photoelectric detector prepared by the film has high responsivity covering the whole visible light and near infrared range,<fast response speed of 1 mus and up to 10 10 Jones' specific detection rate and exhibits good detection performance for X-rays.
Drawings
The invention will be further described with reference to the accompanying drawings, to which, however, the invention is not limited in any way.
FIG. 1 shows the chemical bath deposition method for preparing AgBiS 2 A schematic flow diagram of the film;
FIG. 2 shows AgBiS prepared from precursor solutions of example 1 with different molar ratios of Ag to Bi 2 XRD pattern of the film;
FIG. 3 is an AgBiS obtained at different annealing temperatures 2 Scanning electron microscopy of the film; wherein FIG. 3a represents 150 ℃; FIG. 3b represents 200 ℃; FIG. 3c represents 250 ℃; FIG. 3d represents 300 ℃;
FIG. 4 shows AgBiS obtained at different annealing temperatures 2 XPS plot of thin film;
FIG. 5 is AgBiS 2 Film thickness and depositionA time dependence curve;
FIG. 6 is AgBiS prepared in example 4 2 A schematic structural diagram and an energy level diagram of an optoelectronic device; agBiS 2 The photoelectric device comprises ITO conductive glass, an electron transport layer CdS and a light absorption layer AgBiS from bottom to top in sequence 2 Thin film, hole transport layer, spiro-OMeTAD and MoO x And a metal electrode Ag;
FIG. 7 is AgBiS prepared in example 4 2 Photovoltaic curve graph of solar cell;
FIG. 8 shows AgBiS 2 Solar cell efficiency and AgBiS 2 The relationship of the annealing temperature of the film;
FIG. 9 is AgBiS under visible light in example 4 2 Time response, responsivity and specific detectivity curve diagrams of the photoelectric detector; wherein FIG. 9a represents normalized current density versus time; FIG. 9b represents responsivity and specific detectivity curves;
FIG. 10 shows AgBiS under X-ray in example 4 2 A current-dose rate curve and a current-time curve of the detector; wherein FIG. 10a represents a current-dose rate curve; fig. 10b represents a current-time curve.
Detailed Description
In order that the invention may be more readily understood, specific embodiments thereof will be described further below.
Example 1
We first studied Ag 2 S and Bi 2 S 3 Deposition rate of film, ag was found 2 Growth rate ratio Bi of S 2 S 3 Much faster. Based on this result, we carefully adjusted the Ag and Bi molar ratio in the precursor solution.
(1) AgCl and BiCl are added according to Ag and Bi molar ratios of 1:1, 1.5, 1:2, 1.5 and 1:3 3 Dissolving in deionized water (Ag) + Concentration of 0.002 mol/L) to obtain 5 parts of metal salt aqueous solution;
(2) According to S 2 O 2 2- Na with the concentration of 0.02mol/L 2 S 2 O 2 ·5H 2 Adding O into the metal salt water solution, and fully stirring until the solid is completely dissolved;
(3) Respectively adding hydrochloric acid into the solutions obtained in the step (2), and adjusting the pH values to be =3 to obtain precursor solutions;
(4) Respectively and completely immersing the conductive substrate deposited with the CdS film by the chemical bath deposition method in each precursor solution, maintaining the temperature of the precursor solution at 80 ℃, standing and depositing for 30 minutes, and taking out the conductive substrate;
(5) Placing the conductive substrate treated in the step (4) on a heating table, and annealing in air at 200 ℃ for 30 minutes to obtain the AgBiS attached 2 A thin film conductive substrate.
As shown in fig. 2, when the molar ratio of Ag and Bi is 1:1 and 1.5, agBiS 2 The XPS spectrum of the film shows that Ag appears 2 The characteristic peak of S, which indicates Ag excess; when the molar ratio of Ag to Bi is 1:2, agBiS 2 XPS spectrum of the film shows no Ag 2 S and AgBi 3 S 5 Characteristic peak of (A), illustrating AgBiS 2 AgBiS with pure phase film 2 (ii) a When the molar ratio of Ag to Bi is 1.5 and 1:3, agBiS 2 XPS spectrum of the film shows AgBi 3 S 5 Characteristic peak of (b), indicating an excess of Bi. When the molar ratio of Ag to Bi is 1:2, the AgBiS of the film with only homogeneous cubic phase is measured 2 The crystal size can reach 150nm.
Example 2
Preparation of AgBiS as provided in this example 2 The method of the thin film was substantially the same as that of example 1 except that the molar ratio of Ag to Bi was controlled to 1:2 and the annealing temperature in step (5) was changed (150 ℃,200 ℃, 250 ℃, 300 ℃, 350 ℃, 400 ℃).
As shown in fig. 3, the higher the annealing temperature, the larger the grain size; as shown in FIG. 4, from the XRD pattern of the film, agBiS was already formed at 80 deg.C 2 Phase (1); agBiS as the annealing temperature is increased to 300 ℃ 2 The characteristic peak is obviously enhanced. However, with further increase in annealing temperature, agBiS 2 The characteristic peak is obviously reduced, and Ag appears 5 BiO 4 Phase of AgBiS 2 Deterioration of the crystalline phase and formation of complex oxides of Ag and Bi after degradationExcessive annealing temperature can cause AgBiS 2 High-temperature oxidation in air. Further studies show that the absorption spectrum of the sample annealed at 150-300 ℃ has no obvious change, and when the annealing temperature is increased to 400 ℃, ag-S bonds are converted into Ag-O bonds, and a Bi-S characteristic peak is almost absent. AgBiS annealed at 200 DEG C 2 The film has a high absorption coefficient alpha (about 10) in the whole visible range 5 cm -1 ) The absorption edge appears at-1200 nm, indicating a band gap of-1.03 eV, comparable to that of Si.
Example 3
Preparation of AgBiS as provided in this example 2 The method of the film was substantially the same as that of example 1 except that the molar ratio of Ag to Bi was 1:2 and the time (0.5 hour, 1 hour, 1.5 hours, 2 hours) of the standing deposition in step (4) was changed. As shown in FIG. 5, agBiS 2 The thickness of the film is in a linear relationship with the standing deposition time, which proves that AgBiS is prepared by the method provided by the embodiment 2 The method of the film can accurately regulate and control AgBiS 2 The thickness of the film. The AgBiS with the thickness of 90nm can be prepared within 2 hours by the method provided by the embodiment 2 Compared with the traditional quantum dot preparation method, the preparation efficiency of the film is greatly improved.
Example 4
This example provides a method for preparing AgBiS 2 The method of the photoelectric detector comprises the following steps:
(1) AgCl and BiCl 3 Dissolving in deionized water, adjusting the molar ratio of Ag to Bi to be 1 + The concentration is 0.002mol/L, and a metal salt water solution is obtained;
(2) According to S 2 O 2 2- Na with a concentration of 0.02mol/L 2 S 2 O 2 ·5H 2 Adding O into the aqueous solution of the metal salt, and fully stirring until the solid is completely dissolved;
(3) Adding hydrochloric acid into the solution obtained in the step (2), and adjusting the pH value to be =3 to obtain a precursor solution;
(4) Completely immersing the conductive substrate deposited with the CdS film by a chemical bath deposition method in a precursor solution, maintaining the temperature of the precursor solution at 80 ℃, standing and depositing for 30 minutes, and taking out the conductive substrate;
(5) Placing the conductive substrate treated in the step (4) on a heating table, and annealing in air at 150 ℃,200 ℃, 250 ℃ and 300 ℃ for 30 minutes to obtain the AgBiS attached 2 A conductive substrate of a thin film;
(6) After cooling to room temperature, in AgBiS 2 Sequentially spin-coating a hole transport layer and evaporating MoO on the surface of the film x And manufacturing a metal electrode to finally obtain AgBiS 2 A device.
AgBiS prepared in this example 2 The performance test of the solar cell is shown in fig. 6 to 8, the performance of the visible light detector is shown in fig. 9, and the performance of the X-ray detector is shown in fig. 10
When AgBiS is used, as shown in FIG. 8 2 AgBiS when the film is annealed at 200 DEG C 2 The solar cell has the highest photoelectric conversion efficiency. AgBiS prepared by annealing at 200 ℃ using a modulated 528nm LED and picosecond pulsed laser as the light source, as shown in FIG. 9a 2 The photoelectric detector shows extremely fast response with the rise time of about 960ns, the fast response can be compared with the photoelectric detectors prepared by a solution method (such as perovskite and organic photodiodes), and the photoelectric detector shows great application potential in the field of high-bandwidth photoelectric detection. FIG. 9b shows AgBiS prepared by annealing at 200 deg.C 2 Spectral responsivity and specific detectivity curve of photoelectric detector at-0.1V, agBiS prepared by annealing at 200 deg.C 2 The photodetector exhibits a broadband response of 350nm to 1200nm and reaches a maximum of 0.25 A.W.at 580nm -1 Specific detectivity of approximately 10 10 Jones。
We further tested AgBiS 2 Photodetectors, find these AgBiS 2 The photodetector showed excellent response to both 35kV and 60kV X-rays (fig. 10). As shown in FIG. 10a, we further calculated their sensitivities to be 4.73 and 4.41. Mu.C Gy cm, respectively -2 The lowest detectable dose rate under X-ray irradiation at 60keV is only 0.17 μ Gy s -1 . FIG. 10b shows AgBiS 2 The time response of the photodetector under X-ray irradiation, which means that the X-ray is responsiveFast response and good repeatability.
In addition, we further evaluated AgBiS prepared by annealing at 200 ℃ 2 Stability of the photodetector it was found that under continuous light illumination the photocurrent still retained its initial value after 1 hour, indicating significant photostability. We also stored these devices in air without encapsulation and tested their performance for stability over a month, and found that these devices also exhibited good long term stability.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (9)

1. Preparation of AgBiS 2 A method of making a film, comprising the steps of:
according to the proportion of Ag: adding soluble silver salt and soluble bismuth salt into water according to the molar ratio of Bi =1:2, adding soluble thiosulfate with the sulfur molar weight not lower than the sum of Ag and Bi, uniformly mixing, and adding acid to adjust the pH value =3 to obtain a precursor solution; in the precursor solution, cations of soluble thiosulfate, soluble silver salt, soluble bismuth salt and anions of acid do not participate in deposition reaction;
placing the substrate in the precursor solution, standing and depositing for at least 30 minutes at 80 +/-5 ℃, and taking out the substrate;
annealing the substrate in air at 80-300 ℃ to obtain the AgBiS attached 2 A substrate of a thin film.
2. Preparation of AgBiS according to claim 1 2 A method of making a film, comprising: the molar weight of the sulfur is 5 to 20 times of the sum of Ag and Bi.
3. Preparation of AgBiS according to claim 1 or 2 2 A method of making a film, comprising: the concentration of Ag in the precursor solution is 0.001-0.01 mol/L.
4. Preparation of AgBiS according to claim 3 2 A method of making a film, comprising: the concentration of Ag in the precursor solution is 0.002mol/L.
5. Preparation of AgBiS according to claim 1 2 A method of making a film, comprising: and the CdS film deposited by a chemical bath deposition method is arranged on the substrate.
6. Preparation of AgBiS according to claim 1 2 A method of making a film, comprising: the annealing temperature is 200 +/-5 ℃.
7. Preparation of AgBiS according to claim 1 2 A method of making a film, comprising: the soluble silver salt is AgCl; the soluble bismuth salt is BiCl 3 The soluble thiosulfate is sodium thiosulfate or a hydrate thereof, and the acid is hydrochloric acid.
8. AgBiS 2 A film characterized by: preparation of AgBiS according to any of claims 1 to 7 2 The film is prepared by the method.
9. The AgBiS of claim 8 2 The thin film is applied to the preparation of solar cells and visible light and X-ray photoelectric detectors.
CN202111168824.6A 2021-09-30 2021-09-30 AgBiS 2 Film, preparation method and application thereof Expired - Fee Related CN113913794B (en)

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