CN114935592A - Preparation method and application of bismuth selenide nanosheet/bismuth selenide nanowire composite material - Google Patents
Preparation method and application of bismuth selenide nanosheet/bismuth selenide nanowire composite material Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a bismuth selenide nanosheet/bismuth selenide nanowire composite material, and belongs to the technical field of preparation of photoelectric materials and detectors. The Bi is prepared by using the one-step solvothermal method with simple and convenient operation and controllable process 2 Se 3 Nanosheet/Bi 3 Se 4 The specific gravity of the two components of the nanowire composite material can be regulated and controlled by adjusting the molar weight of the Se source. The preparation method is simple, the nano-structure is in close contact, the self-powered photoelectric detector prepared by taking the composite material as the working electrode has rapid response, and has stronger photocurrent response in the near infrared-visible-ultraviolet band, compared with the pure-phase Bi-based self-powered photoelectric detector 2 Se 3 The detection performance of the self-powered photoelectric detector prepared by the nanosheets is greatly improved, and the recombination of photo-generated electrons and holes can be effectively inhibited. Bi 2 Se 3 nanosheet/Bi 3 Se 4 The preparation of the nanowire composite material has higher reference value for developing the heterostructure of the Bi-Se binary material in the future.
Description
Technical Field
The invention belongs to the technical field of preparation of photoelectric materials and detectors, and particularly relates to a preparation method and application of a bismuth selenide nanosheet/bismuth selenide nanowire composite material.
Background
Multi-layered bismuth selenide (Bi) as one of the second generation topological insulators 2 Se 3 ) The narrow band gap of the material, which is typical of the material with a band gap of 0.3eV and the surface state of a single dirac cone, enables the possibility of broad spectral detection. Preparation of Bi by solvothermal method in various preparation methods 2 Se 3 The nanosheet has the advantages of clear experimental process, simplicity and convenience in operation and the like, compared with the preparation process of a hydrothermal method, the solvothermal method has lower requirement on reaction temperature and higher experimental safety, the prepared nanosheet is thinner in thickness, moderate in transverse size and higher in light absorption efficiency, and the preparation method is favorable for realizing Bi under limited cost 2 Se 3 The performance of the base photodetector is improved.
In the current report, Bi is used 2 Se 3 The research on preparing the composite material by taking the material as a substrate is more, for example, materials such as silicon nanowires, graphene and bismuth oxyhalide can be combined with the material, but a preparation method of the bismuth selenide/bismuth triselenide composite material is not reported at present. Bismuth triselenide (Bi) 3 Se 4 ) Is another Bi-Se double-element compound, and Bi 2 Se 3 Has a different five-layered (Se-Bi-Se-Bi-Se) microstructure, Bi 3 Se 4 Microscopically, a seven-layered (Se-Bi-Se-Bi-Se-Bi-Se) structure is present. At present, Bi cannot be detected in the research 3 Se 4 The morphology of the material realizes effective regular regulation and control, and the material presents a non-uniform linear structure when the concentration is lower, and the microstructure is suitable for Bi 2 Se 3 The materials are compounded to form Bi 3 Se 4 Nanowire capping Bi 2 Se 3 And (3) a composite structure of the nano-sheets.
Exploring a simple method to prepare Bi 2 Se 3 nanosheet/Bi 3 Se 4 The nanowire composite material is combined with the characteristics of quick photoresponse, low manufacturing cost and the like of a self-powered photoelectric detector to prepare Bi 2 Se 3 Nano-sheet/Bi 3 Se 4 The nanowire composite material has important significance in applying the nanowire composite material to a self-powered photoelectric detector.
Disclosure of Invention
The purpose of the invention is to fill in Bi 2 Se 3 nanosheet/Bi 3 Se 4 The blank of the preparation of the nanowire composite material provides simple Bi 2 Se 3 nanosheet/Bi 3 Se 4 The preparation method of the nanowire composite material is combined with the preparation of the self-powered photoelectric detector to test the photoelectric detection performance of the composite material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a bismuth selenide nanosheet/bismuth selenide nanowire composite material comprises the following steps:
the method comprises the following steps: preparing PVP solution, adding EDTA and Bi 2 O 3 To obtain a mixed solution A, wherein Bi 2 O 3 The mass volume ratio of the EDTA to the PVP solution is 0.22-0.25 g:10ml, and the EDTA and Bi are 2 O 3 The molar ratio is 3: 1;
step two: preparing NaOH solution, and adding Se powder and ascorbic acid into the NaOH solution to obtain mixed solution B, wherein the mass-volume ratio of the Se powder to the NaOH solution is 0.08-0.12 g:10 ml;
step three: mixing the mixed solution A and the mixed solution B together according to the volume ratio of 1:1 to obtain a precursor solution, and preparing Bi by adopting a one-step solvothermal method 2 Se 3 Nanosheet/Bi 3 Se 4 A nanowire composite material.
Further, in the first step, the concentration of the PVP solution is 0.035-0.045 g/ml.
Furthermore, in the second step, the concentration of the NaOH solution is 0.016g/ml, and the molar ratio of the ascorbic acid to the Se powder is 1: 1.
Further, in the third step, the solvent in the solvothermal method is ethylene glycol, the reaction temperature of the solvothermal method is 190-210 ℃, and the reaction time is 23-25 h.
The application of the bismuth selenide nanosheet/bismuth selenide nanowire composite material prepared by the preparation method in a self-powered photoelectric detector specifically comprises the following steps:
step 2, adding Bi 2 Se 3 nanosheet/Bi 3 Se 4 The working electrode and the counter electrode of the nanowire composite material are connected by adopting a heat sealing film, and electrolyte is injected into the inner cavity of the self-powered photoelectric detector to obtain Bi 2 Se 3 Nanosheet/Bi 3 Se 4 The nanowire composite material is a self-powered photodetector.
Further, in the step 1, the mass volume ratio of the bismuth selenide nanosheet/bismuth selenide nanowire composite material to absolute ethyl alcohol is 0.015g: 1-2 ml.
Further, in step 2, the counter electrode is a platinum electrode.
Further, in the step 2, the heat sealing temperature of the heat sealing film is 135-165 ℃.
Further, in step 2, the electrolyte is a polysulfide electrolyte.
Compared with the prior art, the invention has the beneficial effects that:
1. preparation of Bi in solvothermal method 2 Se 3 On the basis of the nanosheet reaction principle, the molar weight of the Se source is only reduced without changing the rest reaction conditions, and Bi can be prepared by a one-step solvothermal method 2 Se 3 nanosheet/Bi 3 Se 4 The nanowire composite material has the advantages of simple method, clear principle, controllable product and Bi in the composite material 3 Se 4 The specific gravity of (b) can be regulated and controlled by the change of the molar quantity of the Se source;
2、Bi 2 Se 3 nanosheet/Bi 3 Se 4 The preparation method of the self-powered photoelectric detector made of the nanowire composite material is simple, the optical response of the device is rapid, and the service life of a current carrier is longLong life through Bi 3 Se 4 Nanowire and Bi 2 Se 3 Binding of nanosheets inhibits recombination of photogenerated carriers, Bi 2 Se 3 nanosheet/Bi 3 Se 4 Pure phase Bi with relatively high performance of self-powered photoelectric detector made of nanowire composite material 2 Se 3 The nanosheet self-powered photodetector is obviously improved.
Drawings
FIG. 1 shows Bi 2 Se 3 nanosheet/Bi 3 Se 4 XRD patterns of the nanowire composites;
FIG. 2 shows Bi 2 Se 3 Nanosheet/Bi 3 Se 4 SEM images of nanowire composites;
FIG. 3 shows Bi 2 Se 3 nanosheet/Bi 3 Se 4 Nanowire composite and Bi 2 Se 3 The current density curve and the current density change relation curve of the nanosheet self-powered photodetector along with the wavelength of the simulated light source, wherein the incident light wavelength is 365nm, 470nm, 530nm, 625nm and 850nm respectively, and the optical power density is 30mW/cm 2 No external bias is applied;
FIG. 4 shows Bi 2 Se 3 nanosheet/Bi 3 Se 4 The response time curve of the nanowire composite self-powered photodetector;
FIG. 5 shows Bi 2 Se 3 Nanosheet/Bi 3 Se 4 Nanowire composite and Bi 2 Se 3 And (3) an open-circuit voltage attenuation curve of the nano-sheet self-powered photoelectric detector.
Detailed Description
The technical solutions of the present invention are further described below with reference to the drawings, 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. The chemical reagents used in the invention are all analytically pure.
Detailed description of the invention
Bi 2 Se 3 nanosheet/Bi 3 Se 4 Method for preparing nanowire composite material, and Bi 2 Se 3 nanosheet/Bi 3 Se 4 The nanowire composite material is made of Bi 2 Se 3 Nanosheet and Bi 3 Se 4 The nanowire is prepared by adopting a one-step solvothermal method, and Bi 2 Se 3 The surface of the nano sheet is greatly coated with Bi 3 Se 4 The nanowire covers the composite structure, and the composite structure is in close contact. The method specifically comprises the following steps:
the method comprises the following steps: preparing PVP solution with the concentration of 0.035-0.045 g/ml, and adding EDTA and Bi into the PVP solution 2 O 3 Obtaining a mixed solution A; wherein Bi 2 O 3 The mass volume ratio of the EDTA to the PVP solution is 0.22-0.25 g:10ml, and the EDTA and Bi are 2 O 3 The molar ratio is 3: 1;
step two: preparing NaOH solution with the concentration of 0.016g/ml, and adding Se powder and ascorbic acid into the NaOH solution to obtain mixed solution B; wherein the mass volume ratio of the Se powder to the NaOH solution is 0.08-0.12 g:10 ml; the molar ratio of the ascorbic acid to the Se powder is 1: 1;
step three: mixing the mixed solution A and the mixed solution B together according to the volume ratio of 1:1 to obtain a precursor solution, performing a one-step solvothermal method to obtain a product, wherein the reaction temperature is 190-210 ℃, the reaction time is 23-25 h, performing centrifugal washing on the product for 3 times by using absolute ethyl alcohol and deionized water respectively, and drying to obtain Bi 2 Se 3 nanosheet/Bi 3 Se 4 A nanowire composite.
Further, in the third step, the solvent in the solvothermal method is ethylene glycol.
Detailed description of the invention
An application of the bismuth selenide nanosheet/bismuth selenide nanowire composite material prepared by the preparation method in the first embodiment in a self-powered photodetector specifically includes the following steps:
step 2, adding Bi 2 Se 3 nanosheet/Bi 3 Se 4 The working electrode and the counter electrode of the nanowire composite material are connected by adopting a heat sealing film, and electrolyte is injected into the inner cavity of the self-powered photoelectric detector to obtain Bi 2 Se 3 nanosheet/Bi 3 Se 4 The nanowire composite material is a self-powered photodetector.
Further, in the step 1, the mass volume ratio of the bismuth selenide nanosheet/bismuth selenide nanowire composite material to absolute ethyl alcohol is 0.015g: 1-2 ml.
Further, in step 2, the counter electrode is a platinum electrode.
Further, in the step 2, the heat sealing temperature of the heat sealing film is 135-165 ℃.
Further, in step 2, the electrolyte is a polysulfide electrolyte.
Example 1:
this example provides a Bi 2 Se 3 nanosheet/Bi 3 Se 4 The preparation method of the nanowire composite material adopts a solvothermal method. The specific implementation steps are as follows:
the method comprises the following steps: 0.4g PVP (k16-18) was weighed into 10mL ethylene glycol and stirred on a magnetic stirrer for 10min to give a 0.04g/mL PVP solution, 0.438g EDTA and 0.232gBi 2 O 3 Adding the mixed solution into the PVP solution, and continuously stirring for 30min to obtain a beige mixed solution A;
step two: weighing 0.16g of NaOH, adding the NaOH into 10ml of ethylene glycol, stirring for 1h to obtain 0.016g/ml of NaOH solution, adding 0.102g of Se powder and 0.264g of ascorbic acid into the NaOH solution, and continuously stirring for 30min to obtain a black mixed solution B;
step three: mixing the mixed solution A and the mixed solution B, and stirring for 30min to obtain a precursor solution for reaction; transferring the precursor solution into a 50ml polytetrafluoroethylene liner, putting the liner into a reaction kettle, reacting for 24 hours at 200 ℃, and after the reaction is finished, using deionized water to the productAnd absolute ethyl alcohol are respectively centrifugally cleaned for 3 times, and Bi is obtained after drying 2 Se 3 nanosheet/Bi 3 Se 4 A nanowire composite material.
Bi 2 Se 3 nanosheet/Bi 3 Se 4 The XRD spectrum of the nanowire composite material is shown in figure 1, and the material contains Bi 2 Se 3 And Bi 3 Se 4 Two substances, wherein diffraction peaks at 29.4 DEG, 40.3 DEG and 43.7 DEG correspond to Bi respectively 2 Se 3 The (015), (1010) and (110) crystal planes of (A), and Bi 2 Se 3 The standard card PDF #33-0214 is identical, and the Bi is proved 2 Se 3 Presence of (a); diffraction peaks at 28.9 °, 39.7 ° and 42.7 ° positions respectively correspond to Bi 3 Se 4 Crystal planes of (107), (0114) and (110), and Bi 3 Se 4 The standard card PDF #29-0245 is identical, and proves that Bi 3 Se 4 Is present. Thus, it is shown that Bi has been synthesized 2 Se 3 /Bi 3 Se 4 A composite material.
Bi 2 Se 3 nanosheet/Bi 3 Se 4 The SEM image of the nanowire composite material is shown in FIG. 2, and it can be seen that Bi 3 Se 4 Nanowire and Bi 2 Se 3 Nanosheet contact, Bi 3 Se 4 The length of the nano-wire is 200-800 nm and the nano-wire is covered on Bi 2 Se 3 The surfaces of the nano sheets form a composite structure.
Example 2:
this example provides a Bi 2 Se 3 nanosheet/Bi 3 Se 4 A self-powered photoelectric detector made of nano-wire composite material is composed of working electrode, counter electrode and electrolyte. The specific implementation steps are as follows:
step 1: 0.015g of Bi 2 Se 3 Nanosheet/Bi 3 Se 4 The nanowire composite material is dispersed in 1ml of absolute ethyl alcohol, and ultrasonic treatment is carried out for 15min to obtain black suspension of the composite material. Uniformly dripping the suspension on the surface of the FTO substrate, and drying to obtain Bi 2 Se 3 nanosheet/Bi 3 Se 4 A nanowire composite working electrode.
Step 2: at 150 ℃, Bi is heated and sealed by a heat sealing film 2 Se 3 nanosheet/Bi 3 Se 4 The working electrode of the nanowire composite material is combined with a platinum counter electrode, polysulfide electrolyte is injected into a cavity of a self-powered photoelectric detector, and Bi is obtained 2 Se 3 nanosheet/Bi 3 Se 4 The nanowire composite material is a self-powered photodetector.
To more clearly show Bi 2 Se 3 Nanosheet/Bi 3 Se 4 Nanowire composites compared to Bi 2 Se 3 The photoelectric property of the nano-sheet is improved by adding Bi 2 Se 3 The nano-sheet is used as a working electrode material, is also prepared into a photoelectric detector for testing, and is Bi 2 Se 3 Nanosheet/Bi 3 Se 4 Nanowire composites were compared. Under the condition of not connecting external bias, the optical power is respectively 30mW/cm 2 365nm ultraviolet light, 470nm blue light, 530nm green light, 625nm red light and 850nm near infrared light are used as simulation light sources, the device is irradiated for 10s first and then is stopped to irradiate for 10s, 10 cycles are carried out in total, and the change condition of light response current generated by the device is measured. And respectively irradiating the two photoelectric detectors by using 365nm purple light simulation light sources for 10s, then closing the light sources, testing the attenuation condition of open-circuit voltage along with time, and researching the recombination rate of photogenerated carriers.
Bi 2 Se 3 nanosheet/Bi 3 Se 4 Nanowire composite self-powered photodetector and Bi 2 Se 3 The current density curve of the nano-sheet self-powered photoelectric detector is shown in figure 3, and can be seen from the figure, the current density curve is related to pure-phase Bi 2 Se 3 Nanosheet phase, Bi 2 Se 3 nanosheet/Bi 3 Se 4 The nanowire composite material shows stronger photocurrent response under illumination of various tested wave bands, wherein the photocurrent density under ultraviolet light (365nm) reaches the maximum and is 38.8 mu A/cm 2 Is about Bi 2 Se 3 Photocurrent density15 times of the total weight of the powder.
Bi 2 Se 3 nanosheet/Bi 3 Se 4 The response time of the nanowire composite self-powered photodetector under the irradiation of ultraviolet light (365nm) is shown in fig. 4, the rise time of the device is the time required by the response current from the rise to 63% of the maximum value, and the decay time is the time required by the response current from the fall to 37% of the maximum value, and as can be seen from the figure, the rise time and the decay time of the composite photodetector are respectively 40ms and 37ms, which shows that the photodetector has a relatively high optical response speed and can generate a relatively strong photocurrent in a relatively short time.
Bi 2 Se 3 nanosheet/Bi 3 Se 4 Nanowire composite self-powered photodetector and Bi 2 Se 3 The open-circuit voltage attenuation curve of the nanosheet self-powered photodetector under the irradiation of ultraviolet light (365nm) is shown in figure 5, and can be seen from the figure, the open-circuit voltage attenuation curve is in contact with pure-phase Bi 2 Se 3 In contrast, Bi 2 Se 3 nanosheet/Bi 3 Se 4 The self-powered photoelectric detector of the nanowire composite material has higher photogenerated voltage, which is consistent with a current density curve, and the attenuation of the open-circuit voltage of the self-powered photoelectric detector is far slower than that of Bi after the irradiation of a light source is stopped 2 Se 3 The nano-sheet photoelectric detector shows that the construction of a composite structure enables the recombination of photo-generated electrons and holes to be inhibited, and the service life of a current carrier to be prolonged.
The invention adopts a solvothermal method to prepare Bi 2 Se 3 Polyvinylpyrrolidone (PVP) and Ethylene Diamine Tetraacetic Acid (EDTA) are added as surfactants in the preparation process of the nano-sheets, and Bi is subjected to 2 Se 3 Regulating and controlling the growth of the nanosheets; reducing the molar ratio of the Se source to 85 percent of the original value, keeping the rest conditions unchanged, and preparing Bi by a one-step solvothermal method 2 Se 3 Nanosheet/Bi 3 Se 4 A nanowire composite; adding Bi 2 Se 3 Nanosheet and Bi 2 Se 3 Nanosheet/Bi 3 Se 4 Respectively dripping the nanowire composite material on the surface of the FTO substrate to serve as a working electrode, and injecting electrolyte solution into the internal cavity of the self-powered photoelectric detector to obtain the nano-wire composite materialTo Bi 2 Se 3 Nanosheet and Bi 2 Se 3 nanosheet/Bi 3 Se 4 The nanowire composite material is two self-powered photodetectors. Relative to Bi 2 Se 3 The nano-sheet photoelectric detector has rapid response, has stronger photocurrent response in infrared-visible-ultraviolet wave band response, greatly improves the detection performance, can effectively inhibit the recombination of photo-generated electrons and holes, and has important significance for the preparation of different Bi-Se double-element compound composite materials and the development of photoelectric detectors.
Claims (10)
1. A preparation method of a bismuth selenide nanosheet/bismuth selenide nanowire composite material is characterized by comprising the following steps:
the method comprises the following steps: preparing PVP solution, adding EDTA and Bi 2 O 3 To obtain a mixed solution A, wherein Bi 2 O 3 The mass volume ratio of the EDTA to the PVP solution is 0.22-0.25 g:10ml, and the EDTA and Bi are 2 O 3 The molar ratio is 3: 1;
step two: preparing NaOH solution, and adding Se powder and ascorbic acid into the NaOH solution to obtain mixed solution B, wherein the mass-volume ratio of the Se powder to the NaOH solution is 0.08-0.12 g:10 ml;
step three: mixing the mixed solution A and the mixed solution B together according to the volume ratio of 1:1 to obtain a precursor solution, and preparing Bi by adopting a one-step solvothermal method 2 Se 3 nanosheet/Bi 3 Se 4 A nanowire composite.
2. The production method according to claim 1, characterized in that: in the first step, the concentration of the PVP solution is 0.035-0.045 g/ml.
3. The method of claim 1, wherein: in the second step, the concentration of the NaOH solution is 0.016g/ml, and the molar ratio of the ascorbic acid to the Se powder is 1: 1.
4. The production method according to claim 1, characterized in that: in the third step, the solvent in the solvothermal method is ethylene glycol, the reaction temperature of the solvothermal method is 190-210 ℃, and the reaction time is 23-25 h.
5. The application of the bismuth selenide nanosheet/bismuth selenide nanowire composite material prepared by the preparation method of any one of claims 1 to 4 in a self-powered photodetector.
6. Use according to claim 5, characterized in that it comprises the following steps:
step 1, dispersing a bismuth selenide nanosheet/bismuth selenide nanowire composite material into absolute ethyl alcohol to obtain a dispersion liquid, uniformly and dropwisely coating the dispersion liquid on the surface of an FTO conductive substrate, and drying to prepare Bi 2 Se 3 nanosheet/Bi 3 Se 4 A nanowire composite working electrode;
step 2, adding Bi 2 Se 3 Nanosheet/Bi 3 Se 4 The working electrode and the counter electrode of the nanowire composite material are connected by adopting a heat sealing film, and electrolyte is injected into the inner cavity of the self-powered photoelectric detector to obtain Bi 2 Se 3 Nanosheet/Bi 3 Se 4 The nanowire composite material is a self-powered photodetector.
7. Use according to claim 6, characterized in that: in the step 1, the mass-to-volume ratio of the bismuth selenide nanosheet/bismuth selenide nanowire composite material to absolute ethyl alcohol is 0.015g: 1-2 ml.
8. Use according to claim 6, characterized in that: in step 2, the counter electrode is a platinum electrode.
9. Use according to claim 6, characterized in that: in the step 2, the heat sealing temperature of the heat sealing film is 135-165 ℃.
10. Use according to claim 6, characterized in that: in the step 2, the electrolyte is polysulfide electrolyte.
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