CN111732091A - Preparation method of two-dimensional graphite alkyne nanosheet, working electrode and photoelectric detector - Google Patents
Preparation method of two-dimensional graphite alkyne nanosheet, working electrode and photoelectric detector Download PDFInfo
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Abstract
The invention provides a preparation method of a two-dimensional graphite alkyne nanosheet, which comprises the following steps: providing an ethanol dispersion liquid of the graphyne, transferring the ethanol dispersion liquid of the graphyne to a temperature of 2-15 ℃, performing ultrasonic treatment for 1-7 days, separating the ethanol dispersion liquid of the graphyne subjected to ultrasonic treatment by using a step-by-step centrifugation method, collecting graphyne nanosheets obtained at a speed of 5,000-8,000 r/min, and drying to obtain the two-dimensional graphyne nanosheets. The two-dimensional graphite alkyne nanosheet prepared by the preparation method of the two-dimensional graphite alkyne nanosheet is an ultrathin graphite alkyne nanosheet, the thickness can reach 0.46nm, the process for preparing the ultrathin graphite alkyne nanosheet is simple and rapid, the thickness of the graphite alkyne nanosheet is controllable, and the large-scale preparation of the graphite alkyne nanosheet is easy to realize. The invention also provides a working electrode and a preparation method thereof, and the invention also provides a photoelectric detector.
Description
Technical Field
The invention relates to the field of two-dimensional nano materials and application thereof, in particular to a preparation method of a two-dimensional graphite alkyne nanosheet, and more particularly relates to a preparation method of an ultrathin graphite alkyne nanosheet; the invention also relates to a working electrode comprising the ultrathin graphite alkyne nanosheet and a photoelectric detector comprising the working electrode.
Background
Over the past two decades, two-dimensional (2D) van der waals materials (vdWM), such as Transition Metal Dihalocarbon (TMD), Black Phosphorus (BP), and graphene, have been extensively explored by scientific research. The 2D vdWM has abundant abnormal photoelectric characteristics, and is widely applied to the fields of sensing, catalysis, energy storage, photoelectric detection and the like. Among them, graphene is the most studied 2D vdWM at present. Graphene has very high carrier mobility (-10)5cm2V-1s-1) However, the lack of a band gap in graphene greatly limits its applications. The thickness of TMDs reduced to a single layer showed a direct bandgap, but a relatively wide bandgap and low carrier mobility (-200 cm)2V-1s-1) Preventing their use in the visible region. BP has adjustable band gap (0.3-2.0 eV) and moderate carrier mobility (-10)3cm2V-1s-1) However, BP-based devices typically suffer from poor environmental stability.
In recent years, Photoelectrochemical (PEC) type devices have proven to be an efficient method of collecting solar energy and converting it into electricity, and are favored because of their low cost, simple manufacturing process, environmental friendliness and abundance of raw materials. However, current PEC-type detectors are primarily based on rigid ITO-coated glass substrates, which has hindered the development of flexible PEC-type photodetection. The development of a novel two-dimensional material which can effectively overcome the defects of various materials and has the advantages of various materials and the application of the novel two-dimensional material in the technical field of flexible light detection becomes a big difficulty in the current production research.
Disclosure of Invention
In view of the above, the invention provides a preparation method of a two-dimensional graphite alkyne nanosheet, so as to solve the defect that the existing preparation method is difficult to effectively prepare the two-dimensional graphite alkyne nanosheet in batch. The invention also provides a working electrode, a preparation method of the working electrode and a photoelectric detector, which are used for solving the defects that the existing sensing material and the corresponding photoelectric sensor cannot simultaneously have high carrier mobility, proper band gap, flexibility and the like.
Graphoyne (GDY), an all-carbon nanostructured material that appears after fullerenes, carbon nanotubes and graphene, has attracted considerable interest since its successful large-scale preparation by in-situ cross-coupling. Compared to graphene and other 2D vdWM, GDY has high carrier mobility (-10)4cm2V-1s-1) This provides GDY a great advantage for use as a Photodetector (PD). GDY contain abundant chemical bonds of carbon (sp and sp)2Carbon atom), a highly conjugated 2D planar system, wide interplanar spacing and excellent chemical stability, provide opportunities for constructing flexible GDY photodetectors.
In a first aspect, the invention provides a preparation method of a two-dimensional graphite alkyne nanosheet, which comprises the following steps:
providing an ethanol dispersion liquid of the graphyne, transferring the ethanol dispersion liquid of the graphyne to a temperature of 2-15 ℃, performing ultrasonic treatment for 1-7 days, separating the ethanol dispersion liquid of the graphyne subjected to ultrasonic treatment by using a step-by-step centrifugation method, collecting graphyne nanosheets obtained at a speed of 5,000-8,000 r/min, and drying to obtain the two-dimensional graphyne nanosheets.
Preferably, the ethanol dispersion of graphdiyne is prepared by the following method: dispersing graphite alkyne block powder into ethanol, wherein the mass ratio of the graphite alkyne block powder to the ethanol is 1: 16-400, and preparing ethanol primary dispersion liquid of graphite alkyne;
and stirring the ethanol primary dispersion liquid of the graphyne for 10-100 min to prepare the ethanol dispersion liquid of the graphyne.
Preferably, the mass ratio of the graphite alkyne bulk powder to the ethanol is 1: 80;
and stirring the ethanol primary dispersion liquid of the graphdiyne for 30min at the stirring speed of 100-500 rpm.
The two-dimensional graphite alkyne nanosheet prepared by the preparation method of the two-dimensional graphite alkyne nanosheet is an ultrathin graphite alkyne nanosheet, and the thickness of the ultrathin graphite alkyne nanosheet can reach 0.46 nm. The ultrathin graphite alkyne nanosheet prepared by the method has good flexibility, high carrier mobility and a proper band gap. In addition, the process for preparing the ultrathin graphite alkyne nanosheets by the method is simple and rapid, the thickness of the graphite alkyne nanosheets is controllable, and the graphite alkyne nanosheets can be easily prepared on a large scale.
In a second aspect, the present disclosure provides a working electrode comprising a flexible substrate and a two-dimensional graphitic alkyne nanoplate disposed on the flexible substrate.
Preferably, the flexible substrate is a polyethylene terephthalate flexible substrate coated with indium tin oxide.
The working electrode provided by the invention has stable performance (single cycle stability)>10000s), wide band response (300nm-800nm), high responsivity: (>500nA cm-2) Quick response time (<0.1s), etc. In addition, the working electrode provided by the invention can be used in an alkaline environment, and has excellent photoelectric detection performance in the alkaline environment. The working electrode adopts a flexible substrate, and the two-dimensional graphite alkyne nanosheet is also made of a flexible material, so that the working electrode is ensured to have better flexibility.
In a third aspect, the present invention provides a method for preparing a working electrode, comprising the steps of:
providing a two-dimensional graphite alkyne nanosheet, adding the two-dimensional graphite alkyne nanosheet into a polyvinylidene fluoride/dimethylformamide solution, and carrying out ultrasonic treatment for 10-100 min to obtain a precursor mixture;
dripping the precursor mixture on a flexible substrate, and transferring to a temperature of 50-90 ℃ for drying for 6-24 h to prepare a working electrode;
the mass ratio of the two-dimensional graphite alkyne nanosheet to the polyvinylidene fluoride/dimethylformamide solution is 1: 100-1000.
Preferably, 5mg of two-dimensional graphite alkyne nanosheets are provided and added into 1mL of polyvinylidene fluoride/dimethylformamide solution, and ultrasonic treatment is carried out for 30min to prepare a precursor mixture;
the precursor mixture was dropped onto a flexible substrate and transferred to 80 ℃ for drying for 12h to produce a working electrode.
Preferably, the flexible substrate is a polyethylene terephthalate flexible substrate coated with indium tin oxide.
The working electrode prepared by the preparation method of the working electrode has the advantages that functional materials are dispersed and coated uniformly, the prepared working electrode has relatively uniform efficiency, the detection effects of all detection positions (coating positions) of the working electrode are relatively consistent, and the working stability of the working electrode can be effectively guaranteed. In addition, the process of preparing the working electrode by the method is relatively simple and rapid, and large-scale preparation of the working electrode can be realized.
In a fourth aspect, the present invention also provides a photodetector, which includes the aforementioned working electrode.
The photoelectric detector adopts the working electrode, has quite flexibility, and widens the application range of the photoelectric detector. The photoelectric detector also has stable performance (single cycle stability)>10000s), wide band response (300nm-800nm), high responsivity: (>500nA cm-2) Quick response time (<0.1s), and the like, and also has good photoelectric detection performance in an alkaline environment.
Advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of embodiments of the invention.
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In order to more clearly illustrate the contents of the present invention, a detailed description thereof will be given below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is a representation diagram of a two-dimensional graphdiyne nanosheet provided in embodiment 1 of the present invention;
fig. 2 is a schematic diagram of a method for manufacturing a graphite alkyne photodetector according to embodiment 4 of the present invention;
FIG. 3 shows the result of the photoelectric response performance of the photoelectric detector based on the graphdine material;
fig. 4 shows the flexibility and stability test results of the photoelectric detector based on the graphdine material.
Detailed Description
While the following is a description of the preferred embodiments of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
In a first aspect, the invention provides a preparation method of a two-dimensional graphite alkyne nanosheet, which comprises the following steps:
providing an ethanol dispersion liquid of the graphyne, transferring the ethanol dispersion liquid of the graphyne to a temperature of 2-15 ℃, performing ultrasonic treatment for 1-7 days, separating the ethanol dispersion liquid of the graphyne subjected to ultrasonic treatment by using a step-by-step centrifugation method, collecting graphyne nanosheets obtained at a speed of 5,000-8,000 r/min, and drying to obtain the two-dimensional graphyne nanosheets.
Preferably, the ethanol dispersion of graphdiyne is prepared by the following method: dispersing graphite alkyne block powder into ethanol, wherein the mass ratio of the graphite alkyne block powder to the ethanol is 1: 16-400, and preparing ethanol primary dispersion liquid of graphite alkyne;
and stirring the ethanol primary dispersion liquid of the graphyne for 10-100 min to prepare the ethanol dispersion liquid of the graphyne.
Optionally, the mass ratio of the graphite alkyne bulk powder to the ethanol is 1:16, 1:50, 1:80, 1:100, 1:200, and 1: 400.
Most preferably, the mass ratio of the graphite alkyne bulk powder to the ethanol is 1: 80.
Preferably, the ethanol primary dispersion of graphdiyne is stirred for 30min at a speed of 100, 250, 400 or 500 rpm.
In a second aspect, the present disclosure provides a working electrode comprising a flexible substrate and a two-dimensional graphitic alkyne nanoplate disposed on the flexible substrate. The flexible two-dimensional graphite alkyne nanosheets are arranged on the flexible substrate, so that the working electrode can be manufactured into a flexible electrode, and the application range of the working electrode is greatly expanded.
Preferably, the flexible substrate is a polyethylene terephthalate flexible substrate coated with indium tin oxide.
In a third aspect, the present invention provides a method for preparing a working electrode, comprising the steps of:
providing a two-dimensional graphite alkyne nanosheet, adding the two-dimensional graphite alkyne nanosheet into a polyvinylidene fluoride/dimethylformamide solution, and carrying out ultrasonic treatment for 10-100 min to obtain a precursor mixture;
dripping the precursor mixture on a flexible substrate, and transferring to a temperature of 50-90 ℃ for drying for 6-24 h to prepare a working electrode;
the mass ratio of the two-dimensional graphite alkyne nanosheet to the polyvinylidene fluoride/dimethylformamide solution is 1: 100-1000.
Preferably, 5mg of two-dimensional graphite alkyne nanosheets are provided and added into 1mL of polyvinylidene fluoride/dimethylformamide solution, and ultrasonic treatment is carried out for 30min to prepare a precursor mixture;
the precursor mixture was dropped onto a flexible substrate and transferred to 80 ℃ for drying for 12h to produce a working electrode.
Preferably, the flexible substrate is a polyethylene terephthalate flexible substrate coated with indium tin oxide.
In a fourth aspect, the present invention provides a photodetector comprising the aforementioned working electrode.
The following describes in detail the preparation method of the two-dimensional ultrathin graphite alkyne nanosheet and the prepared two-dimensional ultrathin graphite alkyne nanosheet by the examples.
Example 1
A preparation method of a two-dimensional ultrathin graphite alkyne nanosheet comprises the following steps:
step 1: 1mg of graphite alkyne block powder is dispersed in 100mL of ethanol, mixed and stirred for 30min at the stirring speed of 350rpm to prepare ethanol dispersion liquid of graphite alkyne
Step 2: and transferring the ethanol dispersion liquid of the graphdiyne to a water bath environment with the temperature of 8 ℃, and carrying out water bath ultrasonic treatment for 4 days.
And step 3: separating the ethanol dispersion liquid of the graphdiyne subjected to water bath ultrasound by using a stepwise centrifugation method, wherein the initial centrifugation speed is 3000r/min, centrifuging for 5min, and then collecting the precipitate under the centrifugation condition of 3000 r/min; and gradually increasing the rotating speed at the speed of 1000r/min every time, and simultaneously collecting corresponding precipitates at the rotating speed, thereby obtaining the graphite alkyne nanosheets with different thicknesses.
And 4, step 4: and collecting the graphite alkyne nanosheets obtained at the speed of 5,000-8,000 r/min, and drying in a drying oven at the temperature of 60 ℃ for 12h to obtain the two-dimensional ultrathin graphite alkyne nanosheets.
As shown in fig. 1, is the result of physicochemical test of the two-dimensional ultrathin graphite alkyne nanoplate prepared in example 1. In fig. 1, a is the prepared graphite alkyne nanosheet, the size of the graphite alkyne nanosheet is about 60nm, and b is a high-resolution scanning picture of the graphite alkyne nanosheet, which shows that the graphite alkyne lattice spacing is 0.46nm, and meanwhile, the graphite alkyne material embedded in the graphite alkyne nanosheet has good crystallinity on the surface of the selected electron diffraction picture. Panel c is a photograph of a prepared graphyne flexible photodetector, and from panel d, it can be seen that the graphyne coating has a thickness of about 15 μm. The thickness of the prepared graphite alkyne nanosheet is 1.2nm as can be seen from an e-picture atomic force scanning microscope. From the uv absorption spectrum (f), it can be seen that the uv absorption of the graphdine material hardly changed significantly after one month. From the Raman spectrum of the graph g, it can be seen that the graphdine has 4 shock absorption peaks at 1373, 1578, 1937 and 2141cm-1. From the photoelectron spectrum, sp/sp can be seen2The ratio of hybrid carbon is 2:1, which is consistent with the graphdine material.
Example 2
A preparation method of a two-dimensional ultrathin graphite alkyne nanosheet comprises the following steps:
step 1: 1mg of graphite alkyne block powder is dispersed in 500mL of ethanol, mixed and stirred for 10min at the stirring speed of 500rpm to prepare ethanol dispersion liquid of graphite alkyne
Step 2: and transferring the ethanol dispersion liquid of the graphdiyne to a water bath environment with the temperature of 15 ℃, and carrying out water bath ultrasonic treatment for 1 day.
And step 3: separating the ethanol dispersion liquid of the graphdiyne subjected to water bath ultrasound by using a stepwise centrifugation method, wherein the initial centrifugation speed is 4000r/min, centrifuging for 5min, and then collecting the precipitate under the centrifugation condition of 4000 r/min; and gradually increasing the rotating speed at the speed of 500r/min every time, and simultaneously collecting corresponding precipitates at the rotating speed, thereby obtaining the graphite alkyne nanosheets with different thicknesses.
And 4, step 4: and collecting the graphite alkyne nanosheets obtained at the speed of 5,000-8,000 r/min, and drying in a drying oven at the temperature of 50 ℃ for 24 hours to obtain the two-dimensional ultrathin graphite alkyne nanosheets.
Example 3
The preparation method of the two-dimensional ultrathin graphite alkyne nanosheet comprises the following steps:
step 1: 1mg of graphite alkyne block powder is dispersed in 250mL of ethanol, mixed and stirred for 100min at the stirring speed of 100rpm to prepare ethanol dispersion liquid of graphite alkyne
Step 2: and transferring the ethanol dispersion liquid of the graphdiyne to a water bath environment at the temperature of 2 ℃, and carrying out water bath ultrasonic treatment for 7 days.
And step 3: separating the ethanol dispersion liquid of the graphdiyne subjected to water bath ultrasound by using a stepwise centrifugation method, wherein the initial centrifugation speed is 3000r/min, centrifuging for 10min, and then collecting the precipitate under the centrifugation condition of 3000 r/min; and gradually increasing the rotating speed at the speed of 1000r/min every time, and simultaneously collecting corresponding precipitates at the rotating speed, thereby obtaining the graphite alkyne nanosheets with different thicknesses.
And 4, step 4: and collecting the graphite alkyne nanosheets obtained at the speed of 5,000-8,000 r/min, and drying in a drying oven at the temperature of 80 ℃ for 6 hours to obtain the two-dimensional ultrathin graphite alkyne nanosheets.
A working electrode and a photoelectric detection device based on a two-dimensional ultrathin graphite alkyne nanosheet are prepared as follows in example 4.
Example 4
As shown in fig. 2, the preparation method of the working electrode and the photodetector based on the two-dimensional ultrathin graphite alkyne nanosheet comprises the following steps:
step 1: 1mg of the two-dimensional ultrathin graphitic acetylene nanoplatelets prepared in example 1 was added to 1mL of polyvinylidene fluoride/dimethylformamide (PVDF/DMF) solution and sonicated for 30 minutes to form a homogeneous mixture.
Step 2: the 300 μ L of the mixture was then dropped onto a glass surface coated with Indium Tin Oxide (ITO) and placed in a vacuum oven at 80 degrees celsius overnight to form the working electrode of the photodetector, which was further assembled into a photodetector.
The working electrode test method comprises the following steps: in a photoelectrochemical type photoelectric detection system, ITO glass coated with two-dimensional ultrathin graphite alkyne nanosheets, platinum wires and Ag/AgCl are respectively used as a working electrode, a counter electrode and a reference electrode. Aqueous solutions of HCl, KCl and KOH at different pH values were used as electrolytes. The apparatus was illuminated with different wavelengths (350nm, 400 nm, 475nm, 550nm and 650nm) and the optical power intensities of these illumination lights were assigned to orders I, II, III, IV and V.
As shown in fig. 3, 3a represents the linear sweep voltammetry curve of the flexible graphite alkyne photodetector in the dark and under a certain Illumination (IV), and it can be seen that the photocurrent is continuously increased with the continuous increase of the bias voltage. As can be seen from the 3b graph, in the 0.1M KOH electrolyte solution, the photoresponse performance of the graphdine flexible photodetector increases with increasing applied bias voltage, and shows an increasing trend with increasing incident light power. It was also found that the photodetection performance of the KOH electrolyte at a bias voltage of 0.6V showed a tendency to increase and decrease with the concentration of the KOH electrolyte (as shown in fig. 3 c), which is mainly due to the adsorption of OH ions. Meanwhile, as can be seen from the 3d graph, the surface contact resistance is also different at different concentrations of the KOH electrolyte solution. The curve of the photocurrent when the optical power is taken as IV against the optical power shows that the photocurrent is continuously increased with the increase of the optical power, but the optical detectivity is opposite (as shown in fig. 3e and 3 f), which indicates that the prepared graphite alkyne flexible photodetector is more suitable for being used under low optical power.
As shown in fig. 4a, the prepared graphdine flexible photodetector can be bent and twisted at a certain angle. 4b-4c show the photo-electric response performance curves of the flexible graphite alkyne photodetector at different twisting and bending times, and it can be seen that the flexible graphite alkyne photodetector still shows better photo-electric response performance after 1,000 cycles (as shown in fig. 4 d). Meanwhile, as shown in FIGS. 4e-4f, stability studies ON the graphoyne flexible photodetector found that after 1,000 bends and one month in 0.5M KOH electrolyte solution, a continuously repeatable ON/OFF response pattern was still visible, demonstrating the excellent long-term stability of the detector.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (9)
1. A preparation method of a two-dimensional graphite alkyne nanosheet is characterized by comprising the following steps:
providing an ethanol dispersion liquid of the graphyne, transferring the ethanol dispersion liquid of the graphyne to a temperature of 2-15 ℃, performing ultrasonic treatment for 1-7 days, separating the ethanol dispersion liquid of the graphyne subjected to ultrasonic treatment by using a step-by-step centrifugation method, collecting graphyne nanosheets obtained at a speed of 5,000-8,000 r/min, and drying to obtain the two-dimensional graphyne nanosheets.
2. A method of preparing a two-dimensional graphitic acetylene nanoplatelet according to claim 1 wherein the ethanolic dispersion of graphitic acetylene is prepared by the following method: dispersing graphite alkyne block powder into ethanol, wherein the mass ratio of the graphite alkyne block powder to the ethanol is 1: 16-400, and preparing ethanol primary dispersion liquid of graphite alkyne;
and stirring the ethanol primary dispersion liquid of the graphyne for 10-100 min to prepare the ethanol dispersion liquid of the graphyne.
3. A method of preparing two-dimensional graphitic acetylene nanoplatelets according to claim 2, wherein the ratio of the mass of graphitic acetylene bulk powder to the mass of ethanol is 1: 80;
and stirring the ethanol primary dispersion liquid of the graphdiyne for 30min at the stirring speed of 100-500 rpm.
4. A working electrode is characterized by comprising a flexible substrate and two-dimensional graphite alkyne nanosheets arranged on the flexible substrate.
5. The working electrode of claim 4 wherein the flexible substrate is a polyethylene terephthalate flexible substrate coated with indium tin oxide.
6. A method of making a working electrode, comprising the steps of:
providing a two-dimensional graphite alkyne nanosheet, adding the two-dimensional graphite alkyne nanosheet into a polyvinylidene fluoride/dimethylformamide solution, and carrying out ultrasonic treatment for 10-100 min to obtain a precursor mixture;
dripping the precursor mixture on a flexible substrate, and transferring to a temperature of 50-90 ℃ for drying for 6-24 h to prepare a working electrode;
the mass ratio of the two-dimensional graphite alkyne nanosheet to the polyvinylidene fluoride/dimethylformamide solution is 1: 100-1000.
7. The method of making a working electrode according to claim 6, comprising the steps of:
providing 5mg of two-dimensional graphite alkyne nanosheets, adding the two-dimensional graphite alkyne nanosheets into 1mL of polyvinylidene fluoride/dimethylformamide solution, and carrying out ultrasonic treatment for 30min to obtain a precursor mixture;
the precursor mixture was dropped onto a flexible substrate and transferred to 80 ℃ for drying for 12h to produce a working electrode.
8. The method of making a working electrode according to claim 6, wherein the flexible substrate is a polyethylene terephthalate flexible substrate coated with indium tin oxide.
9. A photodetector comprising the working electrode of claim 4 or 5.
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| CN113666361B (en) * | 2021-08-27 | 2022-09-30 | 郑州大学 | By using supercritical CO 2 Method for preparing graphite oxide alkyne nanosheet |
| CN115020518A (en) * | 2022-06-10 | 2022-09-06 | 哈尔滨工业大学 | Infrared photoelectric detector based on bismuth-oxygen-sulfur micro-flower array or bismuth-oxygen-sulfur nanoflower and preparation method thereof |
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