CN112397317B - Te-doped 2H @1T MoS2Nano heterogeneous material and preparation method and application thereof - Google Patents
Te-doped 2H @1T MoS2Nano heterogeneous material and preparation method and application thereof Download PDFInfo
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- CN112397317B CN112397317B CN201910754104.4A CN201910754104A CN112397317B CN 112397317 B CN112397317 B CN 112397317B CN 201910754104 A CN201910754104 A CN 201910754104A CN 112397317 B CN112397317 B CN 112397317B
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
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Abstract
The invention provides Te doped 2H @1T MoS2The nanometer heterogeneous phase material and its preparation process and applicationTe anchoring at S position to form Te doped 2H @1T MoS2An ultrathin two-dimensional nanosheet structure. The invention realizes Te doping 2H @1T MoS by a tellurium thermal technology2The Te element can effectively promote the 2H MoS2And activates 2H MoS2Is converted into 1T phase while 2H MoS2And can limit the self-aggregation of Te to provide an anchoring site for Te atoms. Through the synergistic effect of the two materials, the energy storage performance of the heterogeneous junction material as the redox type supercapacitor anode material is improved, and the problem of performance reduction in the circulation process is solved. Specific capacitance after Te doping 1054F g‑1More 1T phases appear in the charging and discharging process, so that the specific capacitance after 10000 cycles reaches 2248F g‑1And a new research idea is provided for the research and development of novel energy storage materials.
Description
Technical Field
The invention belongs to the field of preparation and application of energy storage electrode materials, and particularly relates to Te doped 2H @1T MoS2A heterogeneous junction super capacitor anode material and a preparation method thereof relate to a method for preparing a material by adopting Te heat 2H MoS2Preparation of Te doped 2H @1T MoS by technique2A high-performance super capacitor anode material.
Background
The redox type super capacitor is used as an important electrochemical energy storage device to store energy through redox reaction in an electrochemical process, and a gap between a battery and an electrochemical double-layer capacitor is filled. The advantages of fast charge and discharge, high power density, long cycle life and the like make the composite material play an important role in portable electronic products and hybrid electric vehicles. The distance between two-dimensional molybdenum disulfide layers (0.61nm) is twice that of graphene, so that other ions or molecules can be easily introduced between the layers, and ions or charges can be easily diffused. But due to the stable 2H MoS2Are poor conductors, resulting in very slow transfer kinetics of their electrons; although introducing defects has been used to improve 2H MoS2But are difficult to regulate and control.
Disclosure of Invention
The invention provides a Te doped 2H @ 1T MoS2The preparation method has the characteristics of simple process, high repeatability, stable product performance, short reaction period and the like. Te prepared by the method is doped with 2H @ 1T MoS2Having a native 2H MoS2The specific capacitance of the two-dimensional sheet structure is high, and the energy storage performance is further improved by the transformation from 2H to 1T in the using cycle process.
In order to solve the technical problems, the invention adopts the following technical scheme:
te-doped 2H @1T MoS2A nano heterogeneous junction material, wherein the heterogeneous junction material is formed by anchoring Te at the S position to form Te doped 2H @1T MoS2The energy storage performance can be greatly improved due to the ultrathin two-dimensional nanosheet structure, and the energy gradually rises in circulation.
Te doped 2H @1T MoS2The preparation method of the nano heterogeneous material comprises the following steps:
(1) completely dissolving 0.25-1mmol of ammonium molybdate tetrahydrate and 3.5-14mmol of thiourea in 8.75ml of deionized water, pouring the solution into a Teflon-lined high-temperature reaction kettle, placing the reaction kettle in an electric heating forced air drying box, keeping the temperature at 200 ℃ and 250 ℃, reacting for 10-18h, and naturally cooling to room temperature;
(2) centrifugally separating the product, washing with deionized water and ethanol for several times, and drying in a vacuum drying oven for 6-12H to obtain 2H MoS2；
(3) Collecting dried powder 90-100mg 2H MoS2Grinding with 78-312mg Te powder for 30min, spreading at the bottom of 60mm 30mm magnetic boat, placing in tube furnace, and introducing 10% Ar/H at room temperature2After the gas is cooled for 30min, the temperature is raised to 900 ℃ at the heating rate of 5 ℃/min and maintained for 8h, and then the gas is naturally cooled to the room temperature.
Te doped 2H @1T MoS2The application of the nano heterogeneous junction material in the preparation of the super capacitor anode material. The electrode material is ultrathin two-dimensional Te doped 1T @2H MoS2And (3) heterogeneous phase.
The invention realizes Te doping 2H @1T MoS by a tellurium thermal technology2The Te element can effectively promote the 2H MoS2And activates 2H MoS2Is converted into 1T phase while 2H MoS2And can limit the self-aggregation of Te to provide an anchoring site for Te atoms. Through the synergistic effect of the two materials, the energy storage performance of the heterogeneous junction material as the redox type supercapacitor anode material is improved, and the problem of performance reduction in the circulation process is solved. Specific capacitance after Te doping 1054F g-1More 1T phases appear in the charging and discharging process, so that the specific capacitance after 10000 cycles reaches 2248F g-1And a new research idea is provided for the research and development of novel energy storage materials. In particular, the method comprises the following steps of,
the invention provides Te doped 2H @1T MoS2The preparation method of the positive electrode material of the heterogeneous junction super capacitor comprises the following steps:
(1) completely dissolving 0.25mmol of ammonium molybdate tetrahydrate and 3.5mmol of thiourea in 8.75ml of deionized water, transferring the mixed solution into a Teflon-lined high-temperature reaction kettle, sealing, reacting at 220 ℃ for 18h, and naturally cooling to room temperature. Centrifugally separating the product, washing with deionized water and ethanol for several times, and drying in a vacuum drying oven for 6-12H to obtain 2H MoS2；
(2) Collecting dried powder 96mg 2H MoS2Grinding with 78-468mg Te powder for 30min, spreading at the bottom of 60mm 30mm corundum magnetic boat, placing in a tube furnace, and introducing 10% Ar/H at room temperature2After the gas is cooled for 30min, the temperature is raised to 500 ℃ and 700 ℃ at the heating rate of 5 ℃/min and maintained for 8h, and the gas is naturally cooled to the room temperature.
The invention is in the pair 2H MoS2After doping, not only the 2H MoS is activated2Part of the basal plane is converted into a metal conductive 1T phase, Te also provides better electron conductivity, and the continuously improved performance in the charge-discharge cycle process enables the material to have application prospect in the field of energy storage.
Te doped 2H @1T MoS2The method for researching the energy storage performance of the redox type super capacitor anode material comprises the following steps:
weighing 16mg of active material, dispersing the active material in 500 mu L of ethanol, then adding 20 mu L of PTFE dispersion liquid with the mass fraction of 5% and 3mg of carbon black, and carrying out ultrasonic treatment for 30 min. The sample was drop coated onto clean nickel foam and pressed into a sandwich with another piece of nickel foam. Preparing 2M KOH solution, soaking the prepared foam nickel in the KOH solution, and connecting the foam nickel into a three-electrode system; and respectively testing by using a cyclic voltammetry method and a constant-current charging and discharging method.
Therefore, the invention realizes the Te doping of 2H @1T MoS by adjusting the adding proportion and the reaction time of Te based on the tellurium thermal reaction2And regulating and controlling the composition of the heterogeneous-phase electrode material. The electrode material prepared by the invention greatly improves the energy storage capacity, shows high energy density in a double-electrode system, and the performance of the electrode material is increased along with the cycle process in the cycle performance test. The characteristics show that the electrode material has higher application value in the field of new energy development.
The Te is doped with 2H @ 1T MoS2The composition of (A) was such that the amount of doped Te was 8%. Te prepared by the method is doped with 2H @1T MoS2The doping amount of the middle Te is verified as the optimal doping ratio.
The super capacitor anode material has a good application effect in the aspect of preparing devices, and is a novel electrode material meeting the requirements of new energy.
Compared with the prior art, the invention has the advantages and positive effects that: the invention realizes 2H @1T MoS by a simple tellurium thermal method2The preparation of the hetero-phase is carried out, and Te is doped at the same time, so that the Te doping 2H @ 1T MoS is improved2The conductivity of the composite material improves the energy storage property of the redox supercapacitor anode material, and has application prospects in the fields of portable electronic equipment, new energy automobiles and the like.
Drawings
FIG. 1 is the 2H MoS prepared in example 12Te doping 2H @1T MoS from example 22An X-ray diffraction (XRD) pattern of the product;
FIG. 2 is the 2H MoS prepared in example 12Te doping 2H @1T MoS from example 22Transmission Electron Microscopy (TEM) pictures of the product;
FIG. 3 is prepared as in example 2Te doped 2H @1T MoS2High resolution electron microscopy (HRTEM) images of the product;
FIG. 4 is the 2H MoS prepared in example 12Te doping 2H @1T MoS as in example 2 (above)2(below) X-ray photoelectron spectroscopy (XPS) of the product;
FIG. 5 is the 2H MoS prepared in example 12Te doping 2H @1T MoS as in example 2 (above)2Cyclic voltammograms of the product (bottom) (three electrode system);
FIG. 6 is the 2H MoS prepared in example 12Te doping 2H @1T MoS from example 22Constant current charge-discharge cycle diagram (three-electrode system) of the product;
FIG. 7 is the Te doping 2H @1T MoS of example 32Electrochemical properties of the product.
Detailed Description
The invention provides Te doped 2H @1T MoS2A preparation method of a redox supercapacitor positive electrode material.
(1) Completely dissolving 2.5mmol of ammonium molybdate tetrahydrate and 35mmol of thiourea in 87.5mL of deionized water, transferring the solution into a Teflon-lined high-temperature reaction kettle, sealing the reaction kettle, reacting for 18 hours at 220 ℃, and naturally cooling to room temperature.
(2) Washing the product with deionized water and ethanol for several times, centrifuging, and drying in vacuum drying oven for 6-12H to obtain 2H MoS2。
(3) Collecting dried powder 96mg 2H MoS2Grinding with 78-468mg Te powder for 30min, placing at the bottom of 60mm 30mm corundum magnetic boat, and placing in a tube furnace. Continuously introducing 10% Ar/H2After the gas is exhausted for 30min, the temperature is raised to 700 ℃ at the heating rate of 5 ℃/min and maintained for 8h, and the gas is naturally cooled to the room temperature.
Te doped 2H @1T MoS2The energy storage performance of the redox type super capacitor anode material is researched: weighing 16mg of active material, dispersing the active material in 500 mu L of ethanol, then adding 20 mu L of PTFE dispersion liquid with the mass fraction of 5% and 3mg of carbon black, and carrying out ultrasonic dispersion for 30 min. After the sample is dripped on the cleaned foamed nickel, another piece of foamed nickel is pressed into a sandwich structure. Preparing 2M KOH solution, and soaking the prepared foam nickelAnd soaking the glass fiber in the solution, connecting a three-electrode system, and respectively testing by using a cyclic voltammetry method and a constant current charging and discharging method.
The active material is replaced by active carbon to prepare an active carbon cathode, and the active carbon cathode and the anode material form a double-electrode system to carry out tests by a cyclic voltammetry method and a constant-current charging and discharging method.
And (3) forming a device by the anode and cathode electrodes and the solid electrolyte PVA @ KOH, and testing the device.
The present invention will be described in further detail with reference to the following drawings and specific examples.
Example 1
2H MoS2The preparation and performance of (A):
(1) completely dissolving 2.5mmol of ammonium molybdate tetrahydrate and 35mmol of thiourea in 87.5ml of deionized water, pouring the solution into a Teflon-lined high-temperature reaction kettle, reacting for 18h at 220 ℃, and naturally cooling to room temperature.
(2) Centrifugally separating the product, washing with deionized water and ethanol for several times, and drying in a vacuum drying oven for 6-12H to obtain 2H MoS2。
Te doped 2H @1T MoS2The energy storage performance of the redox type super capacitor anode material is researched: the method comprises the following steps: weighing 16mg of active material, dispersing the active material in 500 mu L of ethanol, then adding 20 mu L of PTFE dispersion liquid with the mass fraction of 5% and 3mg of carbon black, and carrying out ultrasonic dispersion for 30 min. After the sample is dripped on the cleaned foamed nickel, another piece of foamed nickel is pressed into a sandwich structure. Preparing 2M KOH solution, soaking the prepared foam nickel in the KOH solution, and connecting the foam nickel into a three-electrode system. And respectively testing by using a cyclic voltammetry method and a constant-current charging and discharging method.
Example 2
Te doped 2H @1T MoS with energy storage performance2And (4) preparation and performance test.
(1) Completely dissolving 2.5mmol of ammonium molybdate tetrahydrate and 35mmol of thiourea in 88mL of deionized water, pouring the solution into a Teflon-lined high-temperature reaction kettle, placing the reaction kettle in an electric heating blowing dry box, keeping the temperature at 220 ℃, reacting for 18h, and naturally cooling to room temperature.
(2) Product ofCentrifugally separating, washing with deionized water and ethanol for several times, and drying in a vacuum drying oven for 6-12H to obtain 2H MoS2。
(3) Collecting dried powder 96mg 2H MoS2Grinding with 78-468mg Te powder for 30min, spreading on the bottom of a corundum magnetic boat with the diameter of 60mm x 30mm, and placing in a tube furnace. Continuously introducing 10% Ar/H at room temperature2After the gas is exhausted for 30min, the temperature is raised to 700 ℃ at the heating rate of 5 ℃/min and maintained for 8h, and then the gas is naturally cooled to the room temperature.
The electrochemical test procedure of the obtained electrode material was the same as that of example 1.
Example 3
Te doped 2H @1T MoS2And (4) preparation and performance test.
(1) Completely dissolving 2.5mmol of ammonium molybdate tetrahydrate and 35mmol of thiourea in 87.5ml of deionized water, pouring the solution into a Teflon-lined high-temperature reaction kettle, putting the reaction kettle into an electric heating forced air drying oven, reacting for 18 hours at 220 ℃, and naturally cooling to room temperature.
(2) Centrifugally separating the product, washing with deionized water and ethanol for several times, and drying in a vacuum drying oven for 6-12H to obtain 2H MoS2。
(3) Collecting dried powder 96mg 2H MoS2Grinding with 78-312mg Te powder for 30min, spreading on the bottom of a corundum magnetic boat with the diameter of 60mm x 30mm, and placing in a tube furnace. Continuously introducing 10% Ar/H at room temperature2After the gas is exhausted for 30min, the temperature is raised to 700 ℃ at the heating rate of 5 ℃/min and maintained for 8h, and the gas is naturally cooled to the room temperature.
Te doped 2H @1T MoS2The energy storage performance of the redox type super capacitor anode material is researched:
the method comprises the following steps: weighing 16mg of active material, dispersing the active material in 500 mu L of ethanol, then adding 20 mu L of PTFE dispersion liquid with the mass fraction of 5% and 3mg of carbon black, and carrying out ultrasonic dispersion for 30 min. After the sample is dripped on the cleaned foamed nickel, another piece of foamed nickel is pressed into a sandwich structure. Preparing 2M KOH solution, soaking the prepared foam nickel in the KOH solution, connecting the foam nickel into a three-electrode system, and respectively testing by using a cyclic voltammetry method and a constant-current charging and discharging method.
The active material is replaced by active carbon to prepare an active carbon cathode, and the active carbon cathode and the anode material form a double-electrode system to carry out tests by a cyclic voltammetry method and a constant-current charging and discharging method.
And (3) forming a device by the anode and cathode electrodes and the solid electrolyte PVA @ KOH, and testing the device.
Wherein the content of the first and second substances,
FIG. 1 shows the X-ray diffraction patterns of examples 1 and 2, consisting of 2H MoS2Doping reaction with different Te proportion. As can be seen from the graph, the amount of Te used was 272mg, and the sample contained unreacted Te powder.
FIG. 2 is a TEM image of examples 1 and 2, in which (a) is 2H MoS2And (b) - (c) are products doped with different Te ratios. It can be seen from the figure that the more Te is used, the more severely the sample morphology is destroyed.
FIG. 3 is the Te doping 2H @1T MoS prepared in example 22High resolution electron microscopy of the product shows the presence of both 1T phase and 2H phase in the product.
FIG. 4 is the 2H MoS prepared in example 12Te doping 2H @1T MoS from example 22The X-ray photoelectron spectrum of the product shows that the 2H MoS is prepared simply2Doping Mo peak and Te with 2H @1T MoS2The Mo peak position of (a) is shifted, and the source of the shift is the generation of 1T phase in the sample.
FIG. 5 is the 2H MoS prepared in example 12Te doping 2H @1T MoS from example 22Cyclic voltammograms of the product (three-electrode system) indicate that the reaction is based on a pseudocapacitance mechanism.
FIG. 6 is the 2H MoS prepared in example 12Te doping 2H @1T MoS from example 22Constant current charge-discharge cycle profile (three-electrode system) of the product, revealing that the prepared Te is doped with 2H @1T MoS in the cycle process2The performance is further improved during cyclic charge and discharge.
FIG. 7 is Te doped 2H @1T MoS of example 32Electrochemical properties of the product and devices.
Claims (2)
1. Te-doped 2H @1T MoS2Method for preparing nano heterogeneous material, and heterogeneous junction materialForming Te doped 2H @1T MoS for Te anchoring at S position2The preparation method of the ultrathin two-dimensional nanosheet structure is characterized by comprising the following steps:
(1) completely dissolving 0.25-1mmol of ammonium molybdate tetrahydrate and 3.5-14mmol of thiourea in 8.75ml of deionized water, pouring the solution into a Teflon-lined high-temperature reaction kettle, placing the reaction kettle in an electric heating forced air drying box, keeping the temperature at 200 ℃ and 250 ℃, reacting for 10-18h, and naturally cooling to room temperature;
(2) centrifugally separating the product, washing with deionized water and ethanol for several times, and drying in a vacuum drying oven for 6-12H to obtain 2H MoS2；
(3) Collecting 90-100mg dried powder 2H MoS2Grinding with 78-312mg Te powder for 30min, spreading at the bottom of 60mm 30mm magnetic boat, placing in tube furnace, and introducing 10% Ar/H at room temperature2After the gas is cooled for 30min, the temperature is raised to 900 ℃ at the heating rate of 5 ℃/min and maintained for 8h, and then the gas is naturally cooled to the room temperature.
2. The Te doped 2H @1T MoS as claimed in claim 12The application of the nano heterogeneous material prepared by the preparation method of the nano heterogeneous material in the aspect of preparing the positive electrode material of the super capacitor.
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