CN110707164A - CsPW (CsPW-shaped conductor wire)11Fe/Si heterojunction composite photoelectric material and preparation method thereof - Google Patents
CsPW (CsPW-shaped conductor wire)11Fe/Si heterojunction composite photoelectric material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a CsPW11Fe/Si heterojunction composite photoelectric material, preparation method thereof and CsPW11Fe nano particles are orderly grown in holes etched on the surface of the Si substrate and are arranged in a mastoid shape; CsPW11The size of the Fe nano-particles is 95-105 nm, and the size of holes etched on the surface of the Si substrate is 1-3 mu m. By CsPW11The electron transfer between Fe and Si enhances the separation efficiency of photon-generated carriers, thereby improving the photoelectric conversion efficiency. Compared with other methods, the invention has advanced technology, energy saving, low consumption and stable property. CsPW under visible light irradiation11Incident of Fe/Si compositeThe monochromatic photon-electron conversion efficiency reaches 54.1 percent, which is obviously higher than that of pure silicon (10 percent).
Description
Technical Field
The invention belongs to the technical field of photoelectricity, particularly relates to a nano photoelectric heterojunction composite material and a preparation method thereof, and particularly relates to Keggin type iron substituted impurityPolyacid salt Cs4PW11O39Fe(III)(H2O) and silicon heterojunction photoelectric material, and preparation method and application thereof.
Background
The energy crisis is a major problem faced by the human society at present, and the development of clean energy capable of being continuously utilized is one of effective ways to solve the problems. Solar energy is a novel energy which is simple and easy to obtain and can be recycled. Research and development of a novel photoelectric material is a method for effectively utilizing solar energy, and the focus is on how to improve the photoelectric conversion efficiency of the photoelectric material. Common photovoltaic materials are based on single crystal silicon and polycrystalline silicon. However, silicon as a photoelectric material has low optical energy utilization efficiency and photoelectric conversion efficiency due to its high optical reflectivity and easy recombination of photogenerated carriers. Therefore, researchers have developed a series of methods for modifying silicon materials, in which efficient separation of photogenerated electrons and holes can be promoted by combining another semiconductor to construct a p-n heterojunction, thereby improving photoelectric conversion efficiency. Keggin type heteropoly acid is a novel photoelectric material, has unique geometric configuration and delocalized electronic configuration, and electrons can realize transition between HOMO and LUMO in the light absorption process. And the substitution of transition metal ions can introduce an intermediate energy level between HOMO and LUMO of Keggin type heteropoly acid, thereby effectively expanding the light absorption range of the Keggin type heteropoly acid. Wherein Keggin type iron substitutes heteropoly acid salt Cs4PW11O39Fe(III)(H2O) (abbreviated CsPW11Fe) synthetic method is simple and easy to implement, has high stability and can be widely applied. CsPW11Various combination modes of Fe and silicon are provided, and in order to enhance the light absorption, under the inspiration of green plant leaves and moth compound eye structures with high light absorption efficiency in nature, CsPW with a mastoid-shaped structure on the surface is prepared11Fe/Si composite material to improve photoelectric conversion efficiency.
Disclosure of Invention
The invention aims to improve the light energy utilization rate and the photoproduction electron hole separation efficiency by constructing p-n heterojunction modification on a silicon photoelectric material, thereby improving the CsPW (CsPW) of photoelectric conversion efficiency11Fe/Si heterojunction composite photoelectric material.
In order to achieve the purpose, the technical scheme of the invention is as follows: providing a CsPW11The Fe/Si heterojunction composite photoelectric material comprises: CsPW11Fe nano particles are orderly grown in holes etched on the surface of the Si substrate and are arranged in a mastoid shape; the CsPW11The size of the Fe nano-particles is 95-105 nm, and the size of holes etched on the surface of the Si substrate is 1-3 mu m. By CsPW11The electron transfer between Fe and Si enhances the separation efficiency of photon-generated carriers, thereby improving the photoelectric conversion efficiency.
Preferably, the CsPW11The size of the Fe nano-particles is 100nm, and the size of holes etched on the surface of the Si substrate is 2 microns.
Preferably, the highly ordered pores of the Si substrate surface are achieved by chemically assisted etching.
Preferably, CsPW11The Fe and the Si are tightly combined, and a p-n heterojunction is formed.
Another objective of the invention is to provide a CsPW11The preparation method of the Fe/Si heterojunction composite photoelectric material comprises the steps of firstly, carrying out chemical auxiliary etching, using gold nanoparticles prepared by reducing chloroauric acid at high temperature with sodium citrate as an etched noble metal particle template, depositing and assembling the gold nanoparticles on the surface of a processed monocrystalline silicon wafer, and then adopting HF and H2O2The mixed solution is used as an etching solution system to etch holes on the surface of the silicon wafer. Finally, growing CsPW in the etched holes through high-temperature hydrothermal reaction11Fe nanocrystal to obtain CsPW with a structure similar to mastoid on the surface11Fe/Si composite photoelectric material. The method specifically comprises the following steps:
1.CsPW11preparation of Fe
(1)Na7PW11O39The preparation of (1):
separately taking Na2HPO4·12H2O and Na2WO4·2H2Dissolving O in deionized water in a beaker, and then adding concentrated HNO3Adjusting pH, stirring in oil bathHeating to 85 ℃, keeping the temperature, continuously stirring and heating until the volume of the solution is reduced by half, naturally cooling, adding 80-100 mL of acetone, uniformly stirring, standing for a period of time, removing the upper layer of acetone by using a suction pipe, and repeating the operation until the upper layer of solution is taken to perform a brown ring experiment to show that NO NO exists3 -Evaporating the rest subnatant in oven at 50 deg.C for drying, and grinding to obtain pure white powder, i.e. Na7PW11O39；
(2)Na4PW11O39Fe(III)(H2O) preparation:
taking Na7PW11O39Dissolving in deionized water, and slowly adding dropwise Fe (NO) under stirring and heating in a magnetic stirring oil bath3)3·9H2Stopping heating until precipitate appears in O solution, cooling, filtering, evaporating the filtrate on an oil bath pan at 90 ℃ until the volume is 15-25 mL, cooling, adding acetone, filtering to remove the precipitate, evaporating the acetone, repeating the operation until no precipitate appears, evaporating the acetone at 80 ℃, drying the residual liquid in an oven at 50 ℃, and grinding to obtain light yellow solid powder, namely Na4PW11O39Fe(III)(H2O)；
(3)CsPW11Preparation of Fe:
weighing a certain proportion of Na4PW11O39Fe(III)(H2O) and CsCl are put into two beakers, an appropriate amount of ultrapure water is added for dissolving, and Na is slowly dropped into the dissolved CsCl solution under stirring4PW11O39Fe(III)(H2O) until no yellow precipitate is generated, stopping dripping; filtering and collecting Cs4PW11Fe filter residue is washed by deionized water, dried at room temperature and ground to obtain light yellow powder, namely CsPW11Fe；
2. Preparation of gold sol and pretreatment and etching of silicon wafer
(1) Preparing gold sol:
a flat-bottomed flask equipped with a reflux condenser and a temperature probe was charged with HAuC14Heating the solution under magnetic stirring, adding sodium citrate solution, and dissolvingThe liquid addition process is rapid; the solution gradually changes from colorless transparency to light red in the reaction process, when the solution finally changes into wine red clear transparent solution, the temperature is immediately closed, the heating is stopped, and the solution is continuously stirred at high speed until the reaction is finished, so that the gold sol is obtained;
(2) pretreatment of a silicon wafer:
cutting the silicon wafer, and preparing a monocrystalline silicon wafer after ultrasonic cleaning;
(3) assembly of gold nanoparticles on silicon wafers
(a) Soaking the treated monocrystalline silicon wafer in a prepared PDDA solution for 2h to dissolve PDDA in the aqueous solution, decomposing chloride ions, and modifying the remaining polymer to the surface of the silicon wafer by positively charging;
(b) cleaning the silicon slice modified by PDDA with distilled water;
(c) placing the modified silicon wafer into the prepared gold sol to form a single-layer gold nanoparticle layer which is relatively uniformly dispersed and non-adhered on the surface of the monocrystalline silicon;
(d) after the assembly of the gold nanoparticles is finished, the gold nanoparticles are cleaned by ultrapure water and placed in a constant-temperature drying oven for drying for later use;
(4) chemically assisted etching of silicon surface holes
3.CsPW11Preparation of Fe/Si heterojunction composite photoelectric material
CsPW (pseudo wire quasi-zero) is performed11Adding Fe salt into a reaction kettle, and growing CsPW in the etched holes on the surface of the monocrystalline silicon wafer by adopting a high-temperature hydrothermal reaction11Fe to obtain CsPW11Fe/Si heterojunction composite photoelectric material.
Preferably, the pretreatment of the silicon wafer comprises the following specific steps:
(a) cutting a silicon wafer into squares, sequentially carrying out ultrasonic cleaning in toluene, acetone and ultrapure water, and cleaning with ultrapure water;
(b) h concentration 98%2SO4And 30% H2O2According to the volume ratio of 4:1, treating at 80 ℃ for 10min, and cleaning with ultrapure water;
(c) HF at a concentration of 49% and 40% NH4The volume ratio of the F configuration is 1:7Etching for 90s and performing ultrasonic treatment for 60s in the solution, and cleaning with ultrapure water;
(d) at volume ratio of NH3·H2O:H2O2:H2Treating in solution with O ratio of 1:1:6 at 80 deg.C for 15min, and cleaning with ultrapure water;
(e) in the volume ratio of HCl to H2O2:H2Treating in solution with O ratio of 1:1:6 at 85 deg.C for 10min, cleaning with ultrapure water, and blowing with high-purity nitrogen gas.
Preferably, the chemically-assisted etching of the holes on the silicon surface comprises the following specific steps:
(a) the concentration of 30% H2O2Mixing with 45% HF according to the volume ratio of 2:1, and adding 30mL of the etching solution into a 50mL reaction kettle;
(b) placing the monocrystalline silicon wafer assembled with the gold nanoparticles into an etching solution, wherein the etching time is 10min, and the reaction temperature is 50 ℃;
(c) after the reaction is finished, the sample is carefully taken out, repeatedly washed by distilled water and placed in an oven for drying for later use.
Preferably, the CsPW11The preparation method of the Fe/Si heterojunction composite photoelectric material comprises the following specific steps:
accurately weighing 0.10g CsPW11Adding Fe salt into a 25mL reaction kettle, and simultaneously adding 10mL distilled water for ultrasonic dispersion to be uniform; the etched surface of the monocrystalline silicon piece is upward, and the monocrystalline silicon piece is slowly placed into a reaction kettle; placing the reaction kettle in an oven, performing hydrothermal reaction at 180 ℃ for 10h, naturally cooling to room temperature after the reaction is finished, taking out a sample in the kettle by using a forceps, slowly flushing out sediments on the surface of a silicon wafer by using distilled water, and drying at 50 ℃ for 6h to obtain the CsPW11Fe/Si heterojunction composite photoelectric material.
Compared with other methods, the invention has advanced technology, energy saving, low consumption and stable property. CsPW under visible light irradiation11The incident monochromatic photon-electron conversion efficiency of the Fe/Si composite material reaches 54.1 percent, which is obviously higher than that of pure silicon (10 percent). In addition, the photoelectric current density of the photoelectric material after being compounded is obviously enhanced compared with that of pure silicon, which shows that the photoelectric material has better photoresponse and photo-generated electron holeThe separation efficiency of (1).
Drawings
FIG. 1 shows a CsPW designed according to the present invention11A structural schematic diagram of the Fe/Si heterojunction composite material;
FIG. 2 is a scanning electron microscope image of the surface of a silicon wafer after chemically assisted etching;
FIG. 3 shows CsPW growth in nano-holes on the surface of a silicon wafer11Scanning electron microscopy after Fe;
FIG. 4 shows a pure silicon wafer and a pure CsPW11XRD patterns of the heterojunction material after Fe and recombination;
FIG. 5 shows CsPW11A mott-schottky diagram of a Fe/Si heterojunction photovoltaic material;
FIG. 6 shows a pure silicon wafer and CsPW11An incident monochromatic photon-electron conversion efficiency graph of the Fe/Si heterojunction photoelectric material;
FIG. 7 shows a pure silicon wafer and CsPW11And (3) a photoelectric current diagram of the Fe/Si heterojunction photoelectric material.
Detailed Description
The following description is further provided in conjunction with the embodiments and accompanying drawings for the purpose of describing the technical content and structural features of the present invention in detail.
1.CsPW11Preparation of Fe
(1)Na7PW11O39The preparation of (1):
10.8g of Na was weighed out separately2HPO4·12H2O and 111.3g of Na2WO4·2H2O in a beaker, dissolved with 225mL of deionized water, followed by concentrated HNO3Adjusting the pH value to 4.8, stirring and heating to 85 ℃ in an oil bath, keeping the temperature, continuously stirring and heating until the volume of the solution is reduced by half, naturally cooling, adding 80-100 mL of acetone, standing for a period of time after uniform stirring, removing the upper layer of acetone by using a suction pipe, and repeating the operation until the upper layer of solution is taken to be subjected to a brown ring experiment to show that NO NO exists3 -Evaporating the rest subnatant in oven at 50 deg.C for drying, and grinding to obtain pure white powder, i.e. Na7PW11O39；
(2)Na4PW11O39Fe(III)(H2O) ofPreparation:
12.14g of Na were weighed7PW11O39Dissolved in 60mL deionized water, and slowly added dropwise with 1.78g Fe (NO) on a magnetic stirring oil bath under stirring and heating3)3·9H2Heating the solution of O until precipitation appears, cooling, filtering, evaporating the filtrate to about 20mL in 90 deg.C oil bath, cooling, adding 60mL acetone, filtering to remove precipitate, evaporating off acetone, repeating the above steps until no precipitate is formed, evaporating off acetone at 80 deg.C, drying the rest solution in 50 deg.C oven, and grinding to obtain light yellow solid powder, i.e. Na4PW11O39Fe(III)(H2O)；
(3)CsPW11Preparation of Fe:
weighing a certain proportion of Na4PW11O39Fe(III)(H2O) and CsCl are put into two beakers, an appropriate amount of ultrapure water is added for dissolving, and Na is slowly dropped into the dissolved CsCl solution under stirring4PW11O39Fe(III)(H2O) until no yellow precipitate is generated, stopping dripping; filtering and collecting Cs4PW11Fe filter residue is washed by deionized water, dried at room temperature and ground to obtain light yellow powder, namely CsPW11Fe；
2. Preparation of gold sol and pretreatment and etching of silicon wafer
(1) Preparing gold sol:
a250 mL flat bottom flask equipped with a reflux condenser and temperature probe was charged with 100mL of 2.5X 10-4mol/L HAuC14The solution was heated to 99 ℃ with magnetic stirring at 800rpm, and then a certain amount (as Na) was added thereto2C6H5O/HAuC14Molar ratio) 0.189mol/L (5% by mass of Na)2C6H5O), the solution is added quickly. Keeping the reaction at 99 ℃ for 30min, gradually changing the solution from colorless and transparent to light red in the reaction process, immediately closing the temperature when the solution finally becomes wine red clear and transparent solution, stopping heating, keeping continuously stirring at high speed until the reaction is finished, and then naturally cooling to obtain the goldAnd (3) sol.
(2) Pretreatment of silicon wafers
The silicon wafer was cut into square pieces of about 0.5cm by 0.5cm and then processed as follows:
(a) sequentially carrying out ultrasonic cleaning in toluene, acetone and ultrapure water for 2min, and cleaning with ultrapure water;
(b) h concentration 98%2SO4And 30% H2O2Treating at 80 ℃ for 10min according to the volume ratio of 4:1, and cleaning with ultrapure water;
(c) HF at a concentration of 49% and 40% NH4F, corroding for 90s in a solution with the volume ratio of 1:7, carrying out ultrasonic treatment for 60s, and cleaning with ultrapure water;
(d) at volume ratio of NH3·H2O:H2O2:H2Treating in solution with O ratio of 1:1:6 at 80 deg.C for 15min, and cleaning with ultrapure water;
(e) in the volume ratio of HCl to H2O2:H2Treating in solution with O ratio of 1:1:6 at 85 deg.C for 10min, cleaning with ultrapure water, and blowing with high-purity nitrogen gas.
(3) Assembly of gold nanoparticles on silicon wafers
(a) Soaking the treated monocrystalline silicon wafer in a prepared 0.01mol/L PDDA solution for 2 hours to dissolve PDDA in the aqueous solution, decomposing chloride ions, and modifying the remaining polymer to the surface of the silicon wafer by positively charging;
(b) cleaning the silicon slice modified by PDDA with distilled water;
(c) placing the modified silicon wafer into the prepared gold sol, wherein Au nano particles prepared by reducing chloroauric acid by using sodium citrate have negative electricity, the surface of the modified silicon wafer has negative electricity, and the silicon wafer is immersed into the gold sol to form a single-layer gold nanoparticle layer which is relatively uniformly dispersed and non-adhesive on the surface of monocrystalline silicon;
(d) after the assembly of the gold nanoparticles is finished, the gold nanoparticles are cleaned by ultrapure water and placed in a constant-temperature drying oven for drying for later use.
(4) Chemically assisted etching of silicon surface holes
(a) The concentration of 30% H2O2Mixed with 45% HF in a volume ratio of 2:1Mixing, adding 30mL of the solution into a 50mL reaction kettle;
(b) placing the monocrystalline silicon wafer assembled with the gold nanoparticles into an etching solution, wherein the etching time is 10min, and the reaction temperature is 50 ℃;
(c) after the reaction is finished, the sample is carefully taken out, repeatedly washed by distilled water and placed in an oven for drying for later use.
3.CsPW11Preparation of Fe/Si composite material
Growing CsPW in the etched holes on the surface of the monocrystalline silicon wafer by adopting high-temperature hydrothermal reaction11Fe, the steps are as follows: accurately weighing 0.10g CsPW11Adding Fe salt into a 25mL reaction kettle, and simultaneously adding 10mL distilled water for ultrasonic dispersion to be uniform; the etched surface of the monocrystalline silicon piece is upward, and the monocrystalline silicon piece is slowly placed into a reaction kettle; placing the reaction kettle in an oven, performing hydrothermal reaction at 180 ℃ for 10h, naturally cooling to room temperature after the reaction is finished, taking out a sample in the kettle by using a forceps, slowly flushing out sediments on the surface of a silicon wafer by using distilled water, and drying at 50 ℃ for 6h to obtain the CsPW11Fe/Si composite photoelectric material.
As shown in FIG. 1, CsPW11Fe nano particles are orderly grown in holes etched on the surface of the Si substrate, so that the holes are arranged in a mastoid shape, and the light energy utilization rate is improved. Wherein CsPW11The size of the Fe nano-particles is about 100nm, and the size of holes etched on the surface of the Si substrate is about 2 mu m. On the other hand, by CsPW11The separation efficiency of photon-generated carriers is enhanced by the electron transfer between Fe and Si, and because Si is a p-type semiconductor, the main carriers are holes; and CsPW11Fe is an n-type semiconductor and the main carrier is an electron. When the two are in close contact, transfer of carriers occurs in order to achieve a thermal equilibrium state. After holes diffuse from the p-type semiconductor to the n-type semiconductor, the positive charge in the p-type semiconductor is reduced, leaving immobile centers of negative charge in the p-type semiconductor; similarly, when electrons diffuse from the n-type semiconductor to the p-type semiconductor, immobile centers of positive charge remain in the n-type semiconductor. These excess charges, referred to as space charges, are confined near the contact edge and are divided into positive and negative charges, thereby creating a chargeAn electric field directed from the n-type semiconductor to the p-type semiconductor-a built-in electric field. The presence of the built-in electric field causes a change in energy, i.e. the energy of the electrons on the p-type semiconductor side is increased and the energy of the holes on the n-type semiconductor side is also increased. When thermal equilibrium is reached, the Fermi level (EF) of the p-type and n-type semiconductors is flattened, creating a barrier near the interface, the p-n junction barrier, that blocks further carrier diffusion. The formation of the p-n junction can be confirmed by measuring the Mott-Schottky curve of the heterojunction material. Under the irradiation of visible light, due to Si and CsPW11Fe has a visible light response and is therefore excited and an electron transitions from the conduction band to the valence band. Under the action of a built-in electric field, photo-generated electrons are transferred from the conduction band of Si to CsPW11Conduction band of Fe and holes from CsPW11The valence band of Fe is transferred to the valence band of Si, so that the effective separation of photo-generated electrons and holes is realized, and the photoelectric conversion efficiency is improved.
CsPW11Structural characteristics of Fe/Si heterojunction photoelectric material
It can be seen from FIGS. 2 and 3 that the assembly with Au nanoparticles, which are noble metals, is performed with HF and H2O2Holes with relatively uniform size and regular arrangement are formed on the surface of the silicon wafer etched by the etching solution, and CsPW is formed after high-temperature hydrothermal reaction11And Fe salt is successfully deposited on the surface of the silicon wafer to fill the holes. FIG. 4 shows pure silicon wafer and pure CsPW11XRD pattern of the heterojunction material after Fe recombination. It can be seen that for CsPW11The Fe sample shows that the characteristic diffraction peaks of Keggin type heteropoly acid salt appear at the 2 theta positions of 18.41 degrees, 23.9 degrees, 26.07 degrees, 30.1 degrees, 35.68 degrees and 38.89 degrees, which indicates that CsPW is11Successful synthesis of Fe materials. These characteristic diffraction peaks were all detectable in the XRD pattern of the heterojunction material, indicating CsPW11Fe salt is successfully compounded on the surface of the silicon wafer. Due to CsPW11Fe overlay, characteristic diffraction peaks of silicon were not detected in the composite. FIG. 5 shows CsPW11A mott-schottky diagram of a Fe/Si heterojunction photovoltaic material. From the figure, CsPW can be seen11The Mott-Schottky curve of the Fe/Si heterojunction photoelectric material presents an inverted V shape, which shows that the silicon and the CsPW11Of FeA p-n heterojunction is formed therebetween.
In order to evaluate the performance of the photoelectric conversion material of the present invention, we performed photoelectric performance tests thereon. FIG. 6 shows a pure silicon wafer and CsPW11And (3) an incident monochromatic photon-electron conversion efficiency graph of the Fe/Si heterojunction photoelectric material. From the figure, CsPW can be seen11The incident monochromatic photon-electron conversion efficiency of the Fe/Si composite material is obviously improved compared with that of pure silicon, which indicates that the modification of the silicon chip is successful. Fig. 7 shows that the photocurrent density of the photoelectric material after recombination is obviously enhanced compared with that of pure silicon, which shows that the photoelectric material has better photoresponse and the separation efficiency of photo-generated electron holes.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the present invention, therefore, the present invention is not limited by the appended claims.
Claims (8)
1. CsPW (CsPW-shaped conductor wire)11The Fe/Si heterojunction composite photoelectric material is characterized in that: CsPW11Fe nano particles are orderly grown in holes etched on the surface of the Si substrate and are arranged in a mastoid shape; the CsPW11The size of the Fe nano-particles is 95-105 nm, and the size of holes etched on the surface of the Si substrate is 1-3 mu m.
2. The CsPW of claim 111The Fe/Si heterojunction composite photoelectric material is characterized in that: the CsPW11The size of the Fe nano-particles is 100nm, and the size of holes etched on the surface of the Si substrate is 2 microns.
3. The CsPW of claim 111The Fe/Si heterojunction composite photoelectric material is characterized in that: highly ordered pores in the Si substrate surface are achieved by chemically assisted etching.
4. The CsPW of claim 111The Fe/Si heterojunction composite photoelectric material is characterized in that: CsPW11The Fe and the Si are tightly combined, and a p-n heterojunction is formed.
5. The CsPW of claim 111The preparation method of the Fe/Si heterojunction composite photoelectric material is characterized by comprising the following steps of:
1.CsPW11preparation of Fe
(1)Na7PW11O39The preparation of (1):
separately taking Na2HPO4·12H2O and Na2WO4·2H2Dissolving O in deionized water in a beaker, and then adding concentrated HNO3Adjusting the pH value, stirring and heating to 85 ℃ in an oil bath, keeping the temperature, continuously stirring and heating until the volume of the solution is reduced by half, naturally cooling, adding 80-100 mL of acetone, uniformly stirring, standing for a period of time, removing the upper layer of acetone by using a suction pipe, and repeating the operation until the upper layer of solution is taken to be subjected to a brown ring experiment to show that NO NO exists3 -Evaporating the rest subnatant in oven at 50 deg.C for drying, and grinding to obtain pure white powder, i.e. Na7PW11O39；
(2)Na4PW11O39Fe(III)(H2O) preparation:
taking Na7PW11O39Dissolving in deionized water, and slowly adding dropwise Fe (NO) under stirring and heating in a magnetic stirring oil bath3)3·9H2Stopping heating until precipitate appears in O solution, cooling, filtering, evaporating the filtrate on an oil bath pan at 90 ℃ until the volume is 15-25 mL, cooling, adding acetone, filtering to remove the precipitate, evaporating the acetone, repeating the operation until no precipitate appears, evaporating the acetone at 80 ℃, drying the residual liquid in an oven at 50 ℃, and grinding to obtain light yellow solid powder, namely Na4PW11O39Fe(III)(H2O)；
(3)CsPW11Preparation of Fe:
weighing a certain proportion of Na4PW11O39Fe(III)(H2O) and CsCl are put into two beakers, an appropriate amount of ultrapure water is added for dissolving, and Na is slowly dropped into the dissolved CsCl solution under stirring4PW11O39Fe(III)(H2O) until no yellow precipitate is generated, stopping dripping; filtering and collecting Cs4PW11Fe filter residue is washed by deionized water, dried at room temperature and ground to obtain light yellow powder, namely CsPW11Fe；
2. Preparation of gold sol and pretreatment and etching of silicon wafer
(1) Preparing gold sol:
a flat-bottomed flask equipped with a reflux condenser and a temperature probe was charged with HAuC14Heating the solution under magnetic stirring, and then adding a certain amount of sodium citrate solution into the solution, wherein the adding process of the solution is rapid; the solution gradually changes from colorless transparency to light red in the reaction process, when the solution finally changes into wine red clear transparent solution, the temperature is immediately closed, the heating is stopped, and the solution is continuously stirred at high speed until the reaction is finished, so that the gold sol is obtained;
(2) pretreatment of a silicon wafer:
cutting the silicon wafer, and preparing a monocrystalline silicon wafer after ultrasonic cleaning;
(3) assembly of gold nanoparticles on silicon wafers
(a) Soaking the treated monocrystalline silicon wafer in a prepared PDDA solution for 2h to dissolve PDDA in the aqueous solution, decomposing chloride ions, and modifying the remaining polymer to the surface of the silicon wafer by positively charging;
(b) cleaning the silicon slice modified by PDDA with distilled water;
(c) placing the modified silicon wafer into the prepared gold sol to form a single-layer gold nanoparticle layer which is relatively uniformly dispersed and non-adhered on the surface of the monocrystalline silicon;
(d) after the assembly of the gold nanoparticles is finished, the gold nanoparticles are cleaned by ultrapure water and placed in a constant-temperature drying oven for drying for later use;
(4) chemically assisted etching of silicon surface holes
3.CsPW11Preparation of Fe/Si heterojunction composite photoelectric material
CsPW (pseudo wire quasi-zero) is performed11Adding Fe salt into a reaction kettle, and growing CsPW in the etched holes on the surface of the monocrystalline silicon wafer by adopting a high-temperature hydrothermal reaction11Fe to obtain CsPW11Fe/Si heterojunction composite photoelectric material.
6. The CsPW of claim 511The preparation method of the Fe/Si heterojunction composite photoelectric material is characterized in that the pretreatment of the silicon wafer comprises the following specific steps:
(a) cutting a silicon wafer into squares, sequentially carrying out ultrasonic cleaning in toluene, acetone and ultrapure water, and cleaning with ultrapure water;
(b) h concentration 98%2SO4And 30% H2O2According to the volume ratio of 4:1, treating at 80 ℃ for 10min, and cleaning with ultrapure water;
(c) HF at a concentration of 49% and 40% NH4F, corroding for 90s in a solution with the volume ratio of 1:7, carrying out ultrasonic treatment for 60s, and cleaning with ultrapure water;
(d) at volume ratio of NH3·H2O:H2O2:H2Treating in solution with O ratio of 1:1:6 at 80 deg.C for 15min, and cleaning with ultrapure water;
(e) in the volume ratio of HCl to H2O2:H2Treating in solution with O ratio of 1:1:6 at 85 deg.C for 10min, cleaning with ultrapure water, and blowing with high-purity nitrogen gas.
7. The CsPW of claim 511The preparation method of the Fe/Si heterojunction composite photoelectric material is characterized in that the chemical auxiliary etching of the holes on the surface of the silicon comprises the following specific steps:
(a) the concentration of 30% H2O2Mixing with 45% HF according to the volume ratio of 2:1, and adding 30mL of the etching solution into a 50mL reaction kettle;
(b) placing the monocrystalline silicon wafer assembled with the gold nanoparticles into an etching solution, wherein the etching time is 10min, and the reaction temperature is 50 ℃;
(c) after the reaction is finished, the sample is carefully taken out, repeatedly washed by distilled water and placed in an oven for drying for later use.
8. The CsPW of claim 511The preparation method of the Fe/Si heterojunction composite photoelectric material is characterized in that,the CsPW11The preparation method of the Fe/Si heterojunction composite photoelectric material comprises the following specific steps:
accurately weighing 0.10g CsPW11Adding Fe salt into a 25mL reaction kettle, and simultaneously adding 10mL distilled water for ultrasonic dispersion to be uniform; the etched surface of the monocrystalline silicon piece is upward, and the monocrystalline silicon piece is slowly placed into a reaction kettle; placing the reaction kettle in an oven, performing hydrothermal reaction at 180 ℃ for 10h, naturally cooling to room temperature after the reaction is finished, taking out a sample in the kettle by using a forceps, slowly flushing out sediments on the surface of a silicon wafer by using distilled water, and drying at 50 ℃ for 6h to obtain the CsPW11Fe/Si heterojunction composite photoelectric material.
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