CN113804736A - Preparation method and application of bismuth/bismuth-oxygen-selenium metal semiconductor heterojunction - Google Patents
Preparation method and application of bismuth/bismuth-oxygen-selenium metal semiconductor heterojunction Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a bismuth/bismuth-oxygen-selenium metal semiconductor heterojunction2O2Se metal semiconductor heterojunction, and further using the heterojunction to prepare a self-powered photodetector. The invention prepares Bi/Bi by a one-step hydrothermal method2O2The Se metal semiconductor heterojunction is simple to operate and controllable in reaction; the content of Bi in the heterojunction can be regulated and controlled by the content of PVP; Bi/Bi2O2The Se metal semiconductor heterojunction self-powered detector is simple to prepare and quick in response, and the separation and transfer of photo-generated electron hole pairs are accelerated by the presence of Bi, so that Bi/Bi2O2The photoelectric detection performance of the Se metal semiconductor heterojunction is superior to that of single Bi2O2A Se material.
Description
Technical Field
The invention belongs to the technical field of photoelectric material and detector preparation, and relates to Bi/Bi2O2A preparation method and application of a Se metal semiconductor heterojunction.
Background
Bismuth oxyselenium (Bi)2O2Se) is a typical bismuth-based oxysulfide semiconductor material, which was first applied in the thermoelectric field. In recent years, Bi is added2O2Intensive research on Se shows that Se has high mobility and excellent environmental stability and can become a photoelectric material with excellent performanceThe material can exert great potential in the aspect of photoelectric detection in the future.
Bi2O2The preparation method of Se comprises a chemical vapor deposition method, a hydrothermal method, a selenization method and the like, wherein the hydrothermal method has simple process and easy operation. However, according to the previous literature reports, Bi prepared by a hydrothermal method2O2The Se material has larger and single size and has certain limit on the detection performance. New materials obtained by means of size control, element doping, noble metal deposition, heterojunction construction and the like are often superior in performance. These have been prepared from Bi2O2Se/CsPbBr3Nanocrystalline heterojunction and Ag surface modified Bi2O2Se and the like. However, Bi/Bi has not been found yet2O2Se metal semiconductor heterojunction.
Among various photoelectric detectors, the self-powered detector has low cost and easy preparation, and can work without an external power supply. Aiming at the application of the heterojunction, Bi/Bi is constructed2O2The Se self-powered detector has important significance.
Disclosure of Invention
The invention aims to provide a preparation method and application of a bismuth/bismuth-oxygen-selenium metal semiconductor heterojunction2O2The Se metal semiconductor heterojunction is simple to operate and controllable in reaction, and further used for preparing a self-powered photoelectric detector, so that the cost is low, the response is rapid, and the Se metal semiconductor heterojunction is superior to Bi under ultraviolet irradiation2O2The photocurrent response of Se has great significance for the preparation of metal semiconductor heterojunction and the application of Se in the aspect of photoelectric detectors.
The purpose of the invention is realized by the following technical scheme:
a method for preparing a bismuth/bismuth-oxygen-selenium metal semiconductor heterojunction is used for preparing Bi/Bi by a one-step hydrothermal method2O2The Se metal semiconductor heterojunction specifically comprises the following steps:
step one, preparing 18-22 mL of PVP solution with the concentration of 0.045-0.055 g/mL, and adding 0.47-0.50 g of Bi (NO) into the solution3)3·5H2O and 8.5-9.5 g of mixed salt to obtain a mixed solution;
step two, preparing 10-15 mL of NaOH solution with the concentration of 0.1 g/mL, and adding 0.039-0.040 g of Se powder and 1-2 mL of hydrazine hydrate (N)2H4·H2O) to obtain a mixed solution;
step three, mixing the two mixed solutions obtained in the step one and the step two together to be used as a precursor solution, and preparing Bi/Bi through a hydrothermal method2O2Se metal semiconductor heterojunction material.
The bismuth/bismuth-oxygen-selenium metal semiconductor heterojunction material prepared by the method can be used for preparing Bi/Bi2O2The Se metal semiconductor heterojunction self-powered photoelectric detector is prepared by the following specific steps:
(1) mixing Bi/Bi2O2Dispersing the Se metal semiconductor heterojunction material in absolute ethyl alcohol, then spin-coating the surface of the FTO conductive glass by using a spin coater, drying, and repeating spin-coating and drying for 3-5 times to obtain a working electrode;
(2) connecting the working electrode and the counter electrode through a heat sealing film, and then injecting electrolyte to obtain Bi/Bi2O2Se metal semiconductor heterojunction self-powered photodetectors.
In the invention, all the chemical reagents are analytically pure.
In the present invention, the mixed salt is LiNO3And KNO3，LiNO3With KNO3The mass ratio of (A) to (B) is 1: 2.
In the present invention, the hydrazine hydrate is present at a concentration of 80% by volume.
In the present invention, Bi (NO)3)3·5H2The molar ratio of O to Se powder is 2: 1.
In the invention, the temperature of the hydrothermal method is 190-210 ℃, and the time is 20-24 h.
In the present invention, Bi/Bi2O2The mass volume ratio of the Se metal semiconductor heterojunction material to the absolute ethyl alcohol is 0.01 g: 1-2 mL.
In the invention, the setting rotation speed and time of the spin coater are respectively 800 rpm and 10 s, and the drying temperature is 60-80 ℃.
In the invention, the counter electrode is a platinum electrode, and the electrolyte is polysulfide electrolyte.
In the invention, the heat sealing temperature is 140-160 ℃.
Compared with the prior art, the invention has the following advantages:
1. Bi/Bi is prepared by a one-step hydrothermal method2O2The Se metal semiconductor heterojunction is simple to operate and controllable in reaction; the content of Bi in the heterojunction can be regulated and controlled by the content of PVP;
2、Bi/Bi2O2the Se metal semiconductor heterojunction self-powered detector is simple to prepare and quick in response, and the separation and transfer of photo-generated electron hole pairs are accelerated by the presence of Bi, so that Bi/Bi2O2The photoelectric detection performance of the Se metal semiconductor heterojunction is superior to that of single Bi2O2A Se material.
Drawings
FIG. 1 shows Bi/Bi2O2XRD pattern of Se metal semiconductor heterojunction;
FIG. 2 shows Bi/Bi2O2SEM images of Se metal semiconductor heterojunctions;
FIG. 3 shows Bi/Bi2O2Se metal semiconductor heterojunction and Bi2O2Current density curve of Se, wherein the incident light wavelength is 365 nm and the light power is 15 mW/cm-2；
FIG. 4 shows Bi/Bi2O2Response time of the Se metal semiconductor heterojunction;
FIG. 5 shows Bi/Bi2O2Se metal semiconductor heterojunction and Bi2O2Electrochemical impedance spectrum of Se.
Detailed Description
The technical solutions of the present invention are further described below with reference to the following examples, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Example 1
This example provides a Bi/Bi2O2The preparation method of the Se metal semiconductor heterojunction adopts a one-step hydrothermal method to directly synthesize Bi/Bi2O2The Se metal semiconductor heterojunction comprises the following specific preparation steps:
the method comprises the following steps: weigh 1 g PVP (k 30), add it to 20 mL deionized water, and magnetically stir for 15 min to give a 0.05 g/mL PVP solution.
Step two: 0.485 g of Bi (NO)3)3·5H2O、3 g LiNO3And 6g KNO3And (4) adding the PVP into the PVP solution obtained in the step one, and continuing to stir for 15 min by magnetic force to obtain a milky mixed solution.
Step three: 1 mL of hydrazine hydrate is dropwise added into 10 mL of deionized water, and the mixture is uniformly stirred to obtain a diluted hydrazine hydrate solution.
Step four: and (3) adding 1 g of NaOH and 0.0395 g of Se powder into the hydrazine hydrate solution obtained in the third step, and carrying out ultrasonic treatment for 10 min to obtain a grape color mixed solution.
Step five: and (4) mixing the two mixed solutions obtained in the step two and the step four together, and magnetically stirring for 30 min to obtain a precursor solution.
Step six: adding the precursor solution obtained in the fifth step into a reaction kettle with a 100 mL polytetrafluoroethylene inner container, reacting for 24 h at 200 ℃, alternately centrifuging and washing for three times by using deionized water and absolute ethyl alcohol after the reaction is finished, drying and collecting to obtain Bi/Bi2O2Se metal semiconductor heterojunction.
FIG. 1 shows Bi/Bi2O2As can be seen from FIG. 1, the XRD pattern of the Se metal semiconductor heterojunction contains Bi and Bi2O2Two Se components, wherein diffraction peaks at 29.2 degrees, 31.7 degrees and 32.5 degrees respectively correspond to Bi2O2The (004), (103) and (110) crystal faces of Se conform to the PDF #73-1316 of a standard card; diffraction peaks at 27.2 degrees, 37.9 degrees and 39.6 degrees respectively correspond to (012), (104) and (110) crystal faces of Bi and correspond to PDF #85-1329 of a standard card; this indicates that Bi/Bi is synthesized2O2Se metal semiconductor heterojunction.
FIG. 2 shows Bi/Bi2O2SeAs can be seen from FIG. 2, the SEM image of the heterojunction of a metal semiconductor shows Bi/Bi2O2The Se metal semiconductor heterojunction is small in size but irregular in shape.
Example 2
This example provides a Bi/Bi-based solution2O2The method for preparing the self-powered detector of the Se metal semiconductor heterojunction comprises the following steps of:
the method comprises the following steps: 0.01 g of Bi/Bi2O2And dispersing the Se metal semiconductor heterojunction material in 1 mL of absolute ethyl alcohol, and carrying out ultrasonic treatment for 20 min to obtain a suspension.
Step two: setting the parameters of a spin coater as the rotating speed of 800 rpm and the time of 10 s, spin-coating the suspension obtained in the first step on FTO conductive glass with the size of 2 cm multiplied by 1.5 cm, drying at the temperature of 60 ℃, and repeating spin-coating and drying for 3 times to obtain the working electrode.
Step three: and connecting the working electrode and the platinum electrode through a heat sealing film at 150 ℃, forming a cavity inside, and injecting polysulfide electrolyte into the cavity to obtain the self-powered photoelectric detector.
Example 3
This example provides a Bi/Bi2O2Method for testing Se metal semiconductor heterojunction self-powered photoelectric detector for showing Bi/Bi2O2The heterojunction performance of Se metal semiconductor is superior to that of Bi2O2Se is tested therewith; firstly, using light with the wavelength of 365 nm of ultraviolet as a simulated light source for irradiating for 10 s, then turning off the light source for 10 s as a period, and under the conditions that the bias voltage is 0V and the light power is 15 mW/cm2Measuring the variation of current density under the condition of (1), and performing switching cycle for 10 periods in total; then, Bi/Bi was tested2O2Se metal semiconductor heterojunction and Bi2O2The electrochemical impedance of Se researches the separation and transfer efficiency of photo-generated electron-hole pairs in the material.
FIG. 3 shows Bi/Bi2O2Se metal semiconductor heterojunction and Bi2O2Se Current Density Curve, FIG. 3 showsKnown as Bi alone2O2Se material ratio, Bi/Bi2O2The Se metal semiconductor heterojunction has larger photocurrent response, and the current density is 61.2 muA/cm2Is about Bi2O2The Se photocurrent density was 9 times higher.
FIG. 4 shows Bi/Bi2O2The response time of the Se metal semiconductor heterojunction self-powered detector is shown in FIG. 4, and the rising time and the falling time of the detector are respectively 6 ms and 10 ms, wherein the response time is measured by taking the time required for the current value to rise to 63% of the maximum value as the rising time of the device and the time required for the current value to fall to 37% of the maximum value as the falling time of the device, which shows that Bi/Bi2O2The Se metal semiconductor heterojunction self-powered photoelectric detector has high response speed and forms large photocurrent response in a short time.
FIG. 5 shows Bi/Bi2O2Se metal semiconductor heterojunction and Bi2O2Electrochemical impedance spectrum of Se, as can be seen from FIG. 5, with Bi2O2Se phase ratio, Bi/Bi2O2Se metal semiconductor heterojunctions have lower resistance because the presence of Bi promotes Bi2O2The separation and transfer of the light-induced electron hole pairs on the Se surface improve the photocurrent response of the Se surface.
Claims (10)
1. A preparation method of a bismuth/bismuth-oxygen-selenium metal semiconductor heterojunction is characterized by comprising the following steps:
step one, preparing 18-22 mL of PVP solution with the concentration of 0.045-0.055 g/mL, and adding 0.47-0.50 g of Bi (NO) into the solution3)3·5H2O and 8.5-9.5 g of mixed salt to obtain a mixed solution;
step two, preparing 10-15 mL of NaOH solution with the concentration of 0.1 g/mL, and adding 0.039-0.040 g of Se powder and 1-2 mL of hydrazine hydrate into the solution to obtain a mixed solution;
step three, mixing the two mixed solutions obtained in the step one and the step two together to be used as a precursor solution, and preparing Bi/Bi through a hydrothermal method2O2Se metal semiconductor heterojunction material.
2. The method for preparing the bismuth/bismuth-oxygen-selenium metal semiconductor heterojunction as claimed in claim 1, wherein the mixed salt is LiNO3And KNO3，LiNO3With KNO3The mass ratio of (A) to (B) is 1: 2.
3. The method for preparing a bismuth/bismuth oxyselenium metal semiconductor heterojunction as claimed in claim 1, wherein the volume concentration of hydrazine hydrate is 80%.
4. The method for preparing a bismuth/bismuth oxyselem metal semiconductor heterojunction as claimed in claim 1, wherein said Bi (NO) is3)3·5H2The molar ratio of O to Se powder is 2: 1.
5. The method for preparing the bismuth/bismuth-oxygen-selenium metal semiconductor heterojunction as claimed in claim 1, wherein the temperature of the hydrothermal method is 190-210 ℃ and the time is 20-24 h.
6. Bi/Bi prepared by the method of any one of claims 1 to 5 in preparation of Bi/Bi2O2The Se metal semiconductor heterojunction self-powered photoelectric detector is applied.
7. The method for preparing Bi/Bi by using bismuth/bismuth oxyselenium metal semiconductor heterojunction material as claimed in claim 62O2The Se metal semiconductor heterojunction self-powered photoelectric detector is applied to, and is characterized in that the Bi/Bi2O2The preparation method of the Se metal semiconductor heterojunction self-powered photoelectric detector comprises the following steps:
(1) mixing Bi/Bi2O2Dispersing the Se metal semiconductor heterojunction material in absolute ethyl alcohol, then spin-coating the surface of the FTO conductive glass by using a spin coater, drying, and repeating spin-coating and drying for 3-5 times to obtain a working electrode;
(2) connecting the working electrode and the counter electrode through a heat sealing film, and injectingElectrolytic solution to obtain Bi/Bi2O2Se metal semiconductor heterojunction self-powered photodetectors.
8. The method for preparing Bi/Bi by using bismuth/bismuth oxyselenium metal semiconductor heterojunction material as claimed in claim 62O2The Se metal semiconductor heterojunction self-powered photoelectric detector is applied to, and is characterized in that the Bi/Bi2O2The mass volume ratio of the Se metal semiconductor heterojunction material to the absolute ethyl alcohol is 0.01 g: 1-2 mL.
9. The method for preparing Bi/Bi by using bismuth/bismuth oxyselenium metal semiconductor heterojunction material as claimed in claim 62O2The Se metal semiconductor heterojunction self-powered photoelectric detector is characterized in that the set rotating speed and the set time of the glue machine are respectively 800 rpm and 10 s, and the drying temperature is 60-80 ℃.
10. The application of the bismuth/bismuth oxyselenide metal semiconductor heterojunction material in the preparation of a bismuth/bismuth oxyselenide metal semiconductor heterojunction self-powered photodetector as claimed in claim 6, wherein the counter electrode is a platinum electrode, the electrolyte is a polysulfide electrolyte, and the heat sealing temperature is 140-160 ℃.
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