CN114843106B - Preparation method of bismuth oxide heterojunction, bismuth oxide heterojunction broadband photoelectric detector and preparation method thereof - Google Patents
Preparation method of bismuth oxide heterojunction, bismuth oxide heterojunction broadband photoelectric detector and preparation method thereof Download PDFInfo
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- 229910000416 bismuth oxide Inorganic materials 0.000 title claims abstract description 31
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000003792 electrolyte Substances 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- 229910052802 copper Inorganic materials 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000011259 mixed solution Substances 0.000 claims description 26
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 14
- 150000003839 salts Chemical class 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910013553 LiNO Inorganic materials 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
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- 229910052697 platinum Inorganic materials 0.000 claims description 7
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- 229920001021 polysulfide Polymers 0.000 claims description 5
- 239000005077 polysulfide Substances 0.000 claims description 5
- 150000008117 polysulfides Polymers 0.000 claims description 5
- 230000004044 response Effects 0.000 abstract description 12
- 238000001514 detection method Methods 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 4
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- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 238000011161 development Methods 0.000 abstract description 2
- 229910052797 bismuth Inorganic materials 0.000 abstract 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract 1
- 230000001276 controlling effect Effects 0.000 abstract 1
- 239000010949 copper Substances 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
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- 238000002441 X-ray diffraction Methods 0.000 description 3
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- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 3
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- 238000003917 TEM image Methods 0.000 description 2
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/0029—Processes of manufacture
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J1/00—Photometry, e.g. photographic exposure meter
- G01J1/42—Photometry, e.g. photographic exposure meter using electric radiation detectors
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
- H01G9/2036—Light-sensitive devices comprising an oxide semiconductor electrode comprising mixed oxides, e.g. ZnO covered TiO2 particles
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a preparation method of a bismuth oxygroup heterojunction, a bismuth oxygroup heterojunction broadband photoelectric detector and a preparation method thereof, belonging to the technical field of photoelectric detector preparation, wherein the broadband photoelectric detector uses Bi 2 O 2 The Se/BiCuOSe heterojunction is used as a matrix material and is prepared from a working electrode, a counter electrode and electrolyte. The preparation method comprises the following steps: firstly, bi is synthesized in situ by regulating and controlling the proportion of bismuth source and copper source by utilizing a one-step hydrothermal method 2 O 2 Se/BiCuOSe heterojunction; then preparing a working electrode from the obtained product; and finally, connecting the working electrode, the counter electrode and the electrolyte to obtain the bismuth oxide heterojunction broadband photoelectric detector. The device can generate photon absorption and optical response in ultraviolet, visible and near infrared bands, and has a ratio Bi due to the effect of heterojunction 2 O 2 Se has higher responsivity, and the device has quick response and better photoelectric detection performance, thus having great significance for the development of broadband photoelectric detectors.
Description
Technical Field
The invention belongs to the technical field of photoelectric detector preparation, and relates to a preparation method of a bismuth oxide heterojunction, a bismuth oxide heterojunction broadband photoelectric detector and a preparation method thereof.
Background
The photoelectric detector is a photoelectric device for converting optical signals into electric signals, and plays an important role in the aspects of remote sensing, medical imaging, environment monitoring, optical communication and the like, and particularly is a broadband photoelectric detector. The method can acquire electromagnetic wave information of various wave bands such as ultraviolet, visible and infrared emitted or reflected by the detection target, and avoids redundancy caused by switching different detectors in different occasions and environments.
The current broadband photoelectric detector is mainly a silicon-based photoelectric detector, but the characteristics of low light response rate, low-temperature operation and the like limit the photoelectric detectorIts application. In recent years, bismuth oxide-based semiconductor compounds (Bi 2 O 2 X: x=s, se, te) has attracted attention from researchers due to its excellent photoelectric properties, wherein n-type semiconductor Bi 2 O 2 Se has the characteristics of high electron mobility, high responsivity, high response speed and the like. However, the application is inevitably limited by the characteristics of the Bi-based alloy, and therefore, the Bi-based alloy is prepared from Bi 2 O 2 The p-type semiconductor BiCuOSe with Se being a bismuth oxide compound is expected to bring greater responsivity and improve the performance of a single material, but related researches have not been found at present.
Disclosure of Invention
The first aim of the invention is to provide a preparation method of bismuth oxide heterojunction, which utilizes a simple one-step hydrothermal method to synthesize Bi in situ 2 O 2 Se/BiCuOSe heterojunction.
The second object of the invention is to provide a bismuth oxide heterojunction broadband photoelectric detector and a preparation method thereof. Bi-based 2 O 2 The Se/BiCuOSe heterojunction constructs the photoelectrochemistry type self-powered photoelectric detector, and the device has the advantages of simplicity in preparation, high response speed, high responsiveness and the like, and has important significance for the development of the broadband photoelectric detector.
The invention aims at realizing the following technical scheme:
the preparation method of the bismuth oxide heterojunction comprises the following steps:
step one, adding Bi (NO) with the mole ratio of (5-24): 1 into PVP solution 3 ) 3 ·5H 2 O and Cu (CH) 3 COO) 2 ·H 2 O and mixed salt to obtain a mixed solution A; wherein the mixed salt comprises LiNO 3 With KNO 3 ；
Step two, adding Se powder and anhydrous Na into the NaOH solution 2 SO 3 Heating to obtain a mixed solution B;
step three, mixing the mixed solution A and the mixed solution B together to be used as a precursor solution, and preparing Bi by a hydrothermal method 2 O 2 Se/BiCuOSe heterojunction.
Further, the concentration of the PVP solution is 0.035-0.040 g/mL, the concentration of the NaOH solution is 0.04-0.06 g/mL, and the volume ratio of the PVP solution to the NaOH solution is 1:1.
Further, in the mixed solution A, bi (NO 3 ) 3 ·5H 2 The concentration of O is 0.042-0.048 mol/L, cu (CH) 3 COO) 2 ·H 2 The concentration of O is 0.002-0.008 mol/L; in the mixed solution B, the concentration of Se powder is 0.02-0.03 mol/L, and the concentration of anhydrous Na is equal to that of the mixed solution B 2 SO 3 The concentration of (C) is 0.05-0.10 mol/L.
Further, in the mixed solution A, the concentration of the mixed salt is 0.4-0.5 g/mL, and the concentration of the mixed salt LiNO is as follows 3 With KNO 3 The mass ratio of (2) is 1:2.
In the second step, the heating temperature is 80-90 ℃ and the heating time is 30-40 min.
In the third step, the temperature of the hydrothermal method is 190-210 ℃ and the time is 20-24 hours.
A bismuth oxide heterojunction broadband photoelectric detector comprises a working electrode, a counter electrode and electrolyte, wherein the base material of the working electrode is Bi 2 O 2 Se/BiCuOSe heterojunction.
A preparation method of a bismuth oxide heterojunction broadband photoelectric detector,
step 1, bi is reacted with 2 O 2 Dispersing Se/BiCuOSe heterojunction in absolute ethyl alcohol, coating on the surface of FTO conductive glass, and drying to obtain a working electrode;
and step 2, connecting the counter electrode and the working electrode through a heat sealing film, and then injecting electrolyte into the cavity to obtain the bismuth oxide heterojunction broadband photoelectric detector.
Further, in the step 1, bi 2 O 2 The mass-volume ratio of the Se/BiCuOSe heterojunction to the absolute ethyl alcohol is 0.01g (1-2) mL.
Further, in the step 2, the counter electrode is a platinum electrode, and the electrolyte is a polysulfide electrolyte.
Compared with the prior art, the invention has the beneficial effects that:
1. hydrothermal method for preparing Bi 2 O 2 The Se/BiCuOSe heterojunction is simple to operate and controllable in reaction, and the product has a larger specific surface area, can absorb more photons, generates larger responsivity, and fully exerts the advantages of the nano material.
2. Narrow bandgap semiconductor Bi 2 O 2 Se and BiCuOSe can form p-n junction due to their different conductivity types, based on Bi 2 O 2 The Se/BiCuOSe heterojunction broadband photoelectric detector can not only meet detection requirements of ultraviolet light, visible light and near infrared light, but also enable the separation efficiency of photogenerated carriers to be higher in the presence of built-in electric fields, and high responsivity and quick response are obtained.
Drawings
Fig. 1: bi (Bi) 2 O 2 XRD pattern of Se/BiCuOSe heterojunction;
fig. 2: bi (Bi) 2 O 2 SEM pictures of Se/BiCuOSe heterojunction;
fig. 3: bi (Bi) 2 O 2 TEM image of Se/BiCuOSe heterojunction;
fig. 4: bi (Bi) 2 O 2 Absorption spectrum of Se/BiCuOSe heterojunction;
fig. 5: bi (Bi) 2 O 2 Photocurrent response of Se/biculose heterojunction broadband detector; (a) For the device illustration, (b-d) is the photocurrent response of the device at 365, 530, 850nm wavelength, respectively, the optical power density is 10mW/cm 2 ；
Fig. 6: bi (Bi) 2 O 2 Electrochemical impedance spectroscopy of Se/BiCuOSe heterojunction broadband detector;
fig. 7: bi (Bi) 2 O 2 Response time of Se/BiCuOSe heterojunction broadband detector;
fig. 8: bi (Bi) 2 O 2 Responsivity of Se/BiCuOSe heterojunction broadband detector.
Detailed Description
The following description of the present invention is provided with reference to the accompanying drawings, but is not limited to the following description, and any modifications or equivalent substitutions of the present invention should be included in the scope of the present invention without departing from the spirit and scope of the present invention.
Detailed description of the preferred embodiments
The preparation method of the bismuth oxide heterojunction comprises the following steps:
step one, preparing PVP solution with the concentration of 0.035-0.040 g/mL, and adding Bi (NO) into the solution 3 ) 3 ·5H 2 O、Cu(CH 3 COO) 2 ·H 2 O and mixed salt to obtain a mixed solution A; wherein the mixed salt comprises LiNO 3 And KNO 3 ，Bi(NO 3 ) 3 ·5H 2 The concentration of O is 0.042-0.048 mol/L, cu (CH) 3 COO) 2 ·H 2 The concentration of O is 0.002-0.008 mol/L, the concentration of mixed salt is 0.4-0.5 g/mL, and the concentration of mixed salt LiNO 3 With KNO 3 The mass ratio of (2) is 1:2;
step two, preparing NaOH solution with the concentration of 0.04-0.06 g/mL, and adding Se powder and anhydrous Na into the solution 2 SO 3 Heating to obtain a mixed solution B; wherein the concentration of Se powder is 0.02-0.03 mol/L, anhydrous Na 2 SO 3 The concentration of (2) is 0.05-0.10 mol/L;
step three, mixing the mixed solution A and the mixed solution B according to the volume ratio of 1:1 to obtain a precursor solution, preparing the precursor solution by a hydrothermal method, and centrifuging, cleaning and drying the precursor solution to obtain Bi 2 O 2 Se/BiCuOSe heterojunction.
Further, in the second step, the heating temperature is 80-90 ℃ and the time is 30-40 min.
In the third step, the temperature of the hydrothermal method is 190-210 ℃ and the time is 20-24 hours.
Detailed description of the preferred embodiments
The preparation method of the bismuth oxide heterojunction comprises the following steps:
step one, preparing PVP solution with concentration of 0.035-0.040 g/mL and adding Bi (NO) 0.41-0.46 g into the solution 3 ) 3 ·5H 2 O、0.01～0.03g Cu(CH 3 COO) 2 ·H 2 O and 8-10 g of mixed salt to obtain a mixed solution A; wherein, the mixed salt packageInclude LiNO 3 And KNO 3 The mass ratio is 1:2;
step two, preparing 20-30mL of NaOH solution with the concentration of 0.04-0.06 g/mL, and adding 0.039-0.040 g Se powder and 0.15-0.20 g anhydrous Na into the solution 2 SO 3 Heating at 80-90 ℃ to obtain a mixed solution B;
step three, mixing the mixed solution A and the mixed solution B together to be used as a precursor solution, preparing the precursor solution by a hydrothermal method, and centrifuging, cleaning and drying the precursor solution to obtain Bi 2 O 2 Se/BiCuOSe heterojunction;
further, the heating temperature in the second step is 80-90 ℃ and the time is 30-40 min.
In the third step, the temperature of the hydrothermal method is 190-210 ℃ and the time is 20-24 hours.
Detailed description of the preferred embodiments
Bi is synthesized in situ by using one-step hydrothermal method by bismuth oxide heterojunction broadband photoelectric detector 2 O 2 The Se/BiCuOSe heterojunction is formed by coating the material on the surface of FTO conductive glass to serve as a working electrode, and then performing hot-pressing connection on the working electrode, a counter electrode and a polysulfide electrolyte. The preparation method comprises the following steps:
step 1, bi obtained by the preparation of the first embodiment or the second embodiment 2 O 2 Dispersing Se/BiCuOSe heterojunction in absolute ethyl alcohol, coating on the surface of FTO conductive glass, and drying to obtain a working electrode;
and 2, connecting the counter electrode with the working electrode obtained in the step 1 through a heat sealing film, and then injecting electrolyte to obtain the bismuth oxide heterojunction broadband photoelectric detector.
Further, bi as described in step 1 2 O 2 The ratio of the mass of Se/BiCuOSe heterojunction to the volume of absolute ethyl alcohol is 0.01g (1-2) mL.
Further defined, the drying temperature in step 1 is 60-80 ℃.
Further defined, the heat sealing temperature of the heat sealing film in step 1 is 140 to 160 ℃.
Further defined, the counter electrode in step 1 is a platinum electrode (formed by coating a conductive surface of FTO with platinum), and the electrolyte is a polysulfide electrolyte.
Example 1:
the embodiment provides a bismuth oxide heterojunction broadband photoelectric detector, which firstly synthesizes Bi in situ by a one-step hydrothermal method 2 O 2 Se/BiCuOSe heterojunction; then coating the conductive glass on the surface of FTO conductive glass to serve as a working electrode; finally, the working electrode and the counter electrode are connected in a hot-pressing mode, and electrolyte is injected into the inner cavity. The specific implementation steps are as follows:
step one: 0.75g PVP (k 30) was weighed into 20mL deionized water and magnetically stirred for 15min to give PVP solution, 0.4365g Bi (NO 3 ) 3 ·5H 2 O、0.02g Cu(CH 3 COO) 2 ·H 2 O、3g LiNO 3 And 6g KNO 3 Adding the mixture into PVP solution, and continuing magnetic stirring for 15min to obtain mixed solution A.
Step two: 0.0395g Se powder, 1g NaOH and 0.15g anhydrous Na 2 SO 3 Added into 20mL of deionized water and heated at 90 ℃ for 30min to obtain a mixed solution B.
Step three: mixing the two mixed solutions obtained in the second step and the third step together, magnetically stirring for 30min to obtain a precursor solution, adding the obtained precursor solution into a reaction kettle with a 100mL polytetrafluoroethylene lining, reacting at 200 ℃ for 24h, 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 2 O 2 Se/BiCuOSe heterojunction.
Step four: 0.01g Bi 2 O 2 The Se/BiCuOSe heterojunction is dispersed in 1mL of absolute ethyl alcohol, ultrasonic treatment is carried out for 20min to obtain suspension, the suspension is coated on the surface of FTO conductive glass with the size of 2cm multiplied by 1.5cm, and the working electrode is obtained by drying at 60 ℃.
Step five: connecting the working electrode and the platinum electrode through a heat sealing film at 150 ℃ to form a cavity inside, and injecting polysulfide electrolyte into the cavity to obtain Bi 2 O 2 Se/BiCuOSe heterojunction broadband photoelectric detectionAnd (3) a device.
FIG. 1 is Bi 2 O 2 XRD patterns of Se/BiCuOSe heterojunctions, diffraction peaks at 23.97 °, 29.24 °, 31.83 °, 32.57 °, 44.30 °, 46.71 °, 53.18 °, 56.22 °, 57.62 °, 66.48 ° and 68.15 ° correspond to Bi, respectively 2 O 2 The (101), (004), (103), (110), (114), (200), (211), (116), (213), (206) and (220) crystal planes of Se standard cards (PDF # 73-1316); another diffraction peak at 30.44 corresponds to the (102) crystal plane of BiCuOSe (PDF # 82-1073). The results indicate the presence of Bi in the product 2 O 2 Se and biculose.
FIG. 2 is Bi 2 O 2 SEM image of Se/BiCuOSe heterojunction, microstructure of product is in tetragonal lamellar structure, and the microstructure of product is equal to Bi 2 O 2 The fact that the crystal structures of Se and BiCuOSe are tetragonal is consistent, and the dispersibility and uniformity are good.
FIG. 3 is Bi 2 O 2 TEM image of Se/BiCuOSe heterojunction, as can be seen from FIGS. 3a-b, bi 2 O 2 The Se/BiCuOSe heterojunction is of a tetragonal sheet structure, has smaller transverse dimension and mostly is about 200nm as the SEM image. A larger specific surface area may absorb more photons, resulting in greater responsivity. FIGS. 3c-e are high resolution images of the product, where the pitch isLattice fringes of (2) corresponding to Bi 2 O 2 The (103) crystal face of Se with a spacing of +.>The lattice fringes of (2) correspond to the (102) crystal plane of biculose and respectively correspond to the strongest diffraction peak in the XRD pattern. This result indicates Bi 2 O 2 The close contact between Se and biculose can provide a path for the transfer of electrons and holes. As shown in FIG. 3e, bi, cu, O, se four elements exist in the product and are uniformly distributed, proving Bi 2 O 2 Successful synthesis of Se/BiCuOSe heterojunction.
FIG. 4 is Bi 2 O 2 Absorption of Se/BiCuOSe heterojunctionThe spectrum is collected, and the ultraviolet light and the near infrared light are absorbed to a certain extent, which is similar to Bi 2 O 2 Se and biculose are related to their narrow bandgap characteristics. The theoretical band gap of the former is 0.8eV, the theoretical band gap of the latter is 0.75eV, and the cut-off wavelength of the latter is about 1550 nm.
FIG. 5 is Bi 2 O 2 Photocurrent response of Se/biculose heterojunction broadband photodetector. As shown in fig. 5a, the broadband photodetector is composed of three parts, namely a working electrode, a platinum electrode and an electrolyte. When receiving illumination, electrons generated by excitation on the working electrode flow to the platinum electrode through an external loop, and the inside is conducted by the redox couple in the electrolyte. As can be seen from FIGS. 5b-c, bi 2 O 2 The Se/BiCuOSe heterojunction broadband photoelectric detector has larger photoelectric current response in ultraviolet, visible and near infrared, and the values of the Se/BiCuOSe heterojunction broadband photoelectric detector are 91.97, 76.53 and 62.86 mu A/cm < 2 >, respectively. With Bi 2 O 2 Se has a greater responsivity than Se.
FIG. 6 is Bi 2 O 2 Electrochemical impedance spectroscopy of Se/BiCuOSe heterojunction broadband photodetectors. The radius of the electrochemical impedance of the device is related to the separation efficiency of the electron-hole pairs in the device, and the smaller the radius is, the higher the separation efficiency of the electron-hole pairs is. From this, bi 2 O 2 The Se/BiCuOSe heterojunction has smaller electrochemical impedance, which is probably that electrons and holes in the built-in electric field inside the heterojunction are transferred to different materials, and the internal carrier ratio of the Se/BiCuOSe heterojunction is Bi 2 O 2 Se separation is faster and can bring about a larger photocurrent response.
FIG. 7 is Bi 2 O 2 The response time of a Se/biculose heterojunction broadband photodetector is generally defined as the rise time when the photocurrent rises from an initial value to 63% of the maximum value, and the decay time when the photocurrent decays from the maximum value to 37% of the value. From the figure, bi 2 O 2 The rise time and fall time of the Se/BiCuOSe heterojunction are 5ms and 4ms respectively, which indicates that the device responds rapidly.
FIG. 8 is Bi 2 O 2 Responsivity of Se/BiCuOSe heterojunction broadband photoelectric detector in various wave bands of ultraviolet, visible and near infraredThe device has larger responsivity, the value of the device is in the order of 6-10 mA/W, and the detection requirements under different environments can be realized.
Claims (10)
1. The preparation method of the bismuth oxide heterojunction is characterized by comprising the following steps of:
step one, adding Bi (NO) with the molar ratio of (5-24): 1 into PVP solution 3 ) 3 ·5H 2 O and Cu (CH) 3 COO) 2 ·H 2 O and mixed salt to obtain a mixed solution A; wherein the mixed salt comprises LiNO 3 With KNO 3 ；
Step two, adding Se powder and anhydrous Na into the NaOH solution 2 SO 3 Heating to obtain a mixed solution B;
step three, mixing the mixed solution A and the mixed solution B together to be used as a precursor solution, and preparing Bi by a hydrothermal method 2 O 2 Se/BiCuOSe heterojunction.
2. The method for preparing the bismuth oxide heterojunction according to claim 1, wherein the method comprises the following steps: the concentration of the PVP solution is 0.035-0.040 g/mL, the concentration of the NaOH solution is 0.04-0.06 g/mL, and the volume ratio of the PVP solution to the NaOH solution is 1:1.
3. The method for preparing the bismuth oxide heterojunction according to claim 1, wherein the method comprises the following steps: in the mixed solution A, bi (NO 3 ) 3 ·5H 2 The concentration of O is 0.042-0.048 mol/L, cu (CH) 3 COO) 2 ·H 2 The concentration of O is 0.002-0.008 mol/L; in the mixed solution B, the concentration of Se powder is 0.02-0.03 mol/L, and the concentration of anhydrous Na is equal to 0.02-0.03 mol/L 2 SO 3 The concentration of (C) is 0.05-0.10 mol/L.
4. The method for preparing the bismuth oxide heterojunction according to claim 1, wherein the method comprises the following steps: in the mixed solution A, the concentration of the mixed salt is 0.4-0.5 g/mL, and the concentration of the mixed salt LiNO is as follows 3 With KNO 3 The mass ratio of (2) is 1:2.
5. The method for preparing the bismuth oxide heterojunction according to claim 1, wherein the method comprises the following steps: in the second step, the heating temperature is 80-90 ℃ and the heating time is 30-40 min.
6. The method for preparing the bismuth oxide heterojunction according to claim 1, wherein the method comprises the following steps: in the third step, the temperature of the hydrothermal method is 190-210 ℃ and the time is 20-24 hours.
7. A bismuth oxide heterojunction broadband photoelectric detector is characterized by comprising a working electrode, a counter electrode and electrolyte, wherein the base material of the working electrode is Bi 2 O 2 Se/BiCuOSe heterojunction, said Bi 2 O 2 Se/BiCuOSe heterojunction is Bi prepared by the preparation method of any one of claims 1-6 2 O 2 Se/BiCuOSe heterojunction.
8. A preparation method of a bismuth oxide heterojunction broadband photoelectric detector is characterized by comprising the following steps:
step 1, bi is reacted with 2 O 2 Dispersing Se/BiCuOSe heterojunction in absolute ethyl alcohol, coating on the surface of FTO conductive glass, and drying to obtain a working electrode; the Bi is 2 O 2 Se/BiCuOSe heterojunction is Bi prepared by the preparation method of any one of claims 1-6 2 O 2 Se/BiCuOSe heterojunction;
and step 2, connecting the counter electrode and the working electrode through a heat sealing film, and then injecting electrolyte into the cavity to obtain the bismuth oxide heterojunction broadband photoelectric detector.
9. The method for preparing the bismuth oxide heterojunction broadband photoelectric detector is characterized by comprising the following steps of: in the step 1, bi 2 O 2 The mass-volume ratio of the Se/BiCuOSe heterojunction to the absolute ethyl alcohol is 0.01-g (1-2) mL.
10. The method for preparing the bismuth oxide heterojunction broadband photoelectric detector is characterized by comprising the following steps of: in the step 2, the counter electrode is a platinum electrode, and the electrolyte is a polysulfide electrolyte.
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| CN103855232A (en) * | 2012-12-07 | 2014-06-11 | 通用电气公司 | Photovoltaic device and manufacturing method thereof |
| CN104043390A (en) * | 2014-06-20 | 2014-09-17 | 浙江大学 | Small-size high-specific-surface-area nano heterostructure hollow sphere and preparation method thereof |
| CN113758562A (en) * | 2021-09-08 | 2021-12-07 | 哈尔滨工业大学 | Wide spectrum detector based on copper selenide nanotube or copper selenide/bismuth sulfide nanotube composite material and preparation method thereof |
| CN113804736A (en) * | 2021-09-15 | 2021-12-17 | 哈尔滨工业大学 | Preparation method and application of bismuth/bismuth-oxygen-selenium metal semiconductor heterojunction |
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| CN103855232A (en) * | 2012-12-07 | 2014-06-11 | 通用电气公司 | Photovoltaic device and manufacturing method thereof |
| CN104043390A (en) * | 2014-06-20 | 2014-09-17 | 浙江大学 | Small-size high-specific-surface-area nano heterostructure hollow sphere and preparation method thereof |
| CN113758562A (en) * | 2021-09-08 | 2021-12-07 | 哈尔滨工业大学 | Wide spectrum detector based on copper selenide nanotube or copper selenide/bismuth sulfide nanotube composite material and preparation method thereof |
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