CN110349754B - Hydrated tungsten trioxide/tungsten self-supporting electrode and preparation method thereof - Google Patents
Hydrated tungsten trioxide/tungsten self-supporting electrode and preparation method thereof Download PDFInfo
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- CN110349754B CN110349754B CN201910462002.5A CN201910462002A CN110349754B CN 110349754 B CN110349754 B CN 110349754B CN 201910462002 A CN201910462002 A CN 201910462002A CN 110349754 B CN110349754 B CN 110349754B
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- H—ELECTRICITY
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- H—ELECTRICITY
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- 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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Abstract
The invention discloses a hydrated tungsten trioxide/tungsten self-supporting electrode and a preparation method thereof, wherein the hydrated tungsten trioxide/tungsten self-supporting electrode is prepared by the following method: and (3) taking a metal tungsten sheet as an anode and a metal titanium sheet as a cathode, and carrying out an anodic oxidation reaction in a sodium dodecyl sulfate-hydrochloric acid mixed electrolyte to obtain the hydrated tungsten trioxide nanosheet/tungsten self-supporting electrode. The hydrated tungsten trioxide nanosheet prepared by the method provided by the invention is uniform in shape and complete in structure, and the nanosheet vertically grows on a tungsten substrate, is firmly combined with a metal tungsten substrate and is not easy to separate; in addition, the method has the advantages of simple process, high preparation repeatability, low requirement on equipment, cheap and easily-obtained related chemicals and great prospect in the aspect of industrial application.
Description
(I) technical field
The invention relates to a hydrated tungsten trioxide/tungsten self-supporting electrode and a preparation method thereof.
(II) background of the invention
As an n-type semiconductor, tungsten trioxide has the advantages of relatively narrow forbidden band width (2.5-2.8 eV), excellent electron transmission speed, good chemical stability and the like, and has wide application prospects in the fields of gas sensing, photocatalysis, energy storage devices and the like. The hydrated tungsten trioxide not only can reduce the internal transmission resistance of electrons in the material, but also can increase the proton exchange rate, and has potential application in the super capacitor.
At present, the literature for preparing the hydrated tungsten trioxide is less, and the hydrothermal method is mainly focused on the preparation. For example, CN201610945842.3 reports a preparation method of tungsten trioxide dihydrate nano sheet powder, which obtains tungsten trioxide dihydrate nano sheet powder through multiple mixing and stirring, high-temperature hydrothermal reaction and subsequent multiple centrifugation processes. However, hydrothermal preparation is not easy for industrial production due to its relatively complicated process, time and energy consumption.
Disclosure of the invention
The invention relates to a hydrated tungsten trioxide/tungsten self-supporting electrode and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
a hydrated tungsten trioxide/tungsten self-supporting electrode is prepared by the following method:
(1) taking a metal tungsten sheet as an anode and a metal titanium sheet as a cathode, wherein the distance between the anode and the cathode is 1-3 cm;
(2) preparing an anodic oxidation electrolyte: weighing sodium dodecyl sulfate, and dissolving the sodium dodecyl sulfate in a hydrochloric acid solution with the mass concentration of 2-10% to prepare an electrolyte with the concentration of 2-60 g/L of sodium dodecyl sulfate;
(3) adjusting the anodic oxidation voltage to 10-30V, setting the temperature to 20-70 ℃, and carrying out constant-voltage reaction for 0.5-5 h in the electrolyte prepared in the step (2);
(4) and taking out the metal tungsten sheet, washing with deionized water, and drying to obtain the hydrated tungsten trioxide/tungsten self-supporting electrode.
The size of the metal tungsten sheet is 10 multiplied by 10mm, and the thickness of the metal tungsten sheet is 0.08 mm; the size of the metal titanium sheet is 20mm multiplied by 20mm, and the thickness is 0.02 mm.
The electrochemical anode oxidation method is characterized in that a metal or alloy product is directly used as an anode, electric conduction is realized through the directional movement of ions in electrolyte, corresponding chemical reaction is generated between the surface of an electrode and the cross section of the electrolyte, and a layer of metal oxide material is directly grown on the surface of the anode. The prepared metal oxide has good contact with a metal matrix, and the chemical stability and the conductivity of the material can be enhanced.
The invention aims to select a proper electrolyte to directly grow hydrated tungsten trioxide nanosheets on a metal tungsten substrate by a one-step anodic oxidation method, and the hydrated tungsten trioxide/tungsten self-supporting material formed by the hydrated tungsten trioxide/tungsten self-supporting material can be directly used as a super capacitor negative electrode material and shows excellent electrochemical performance. The method is convenient and simple, is easy to operate, and can be used for industrial mass production.
The invention also relates to a method for preparing the hydrated tungsten trioxide/tungsten self-supporting electrode, which comprises the following steps:
(1) taking a metal tungsten sheet as an anode and a metal titanium sheet as a cathode, wherein the distance between the anode and the cathode is 1-3 cm;
(2) preparing an anodic oxidation electrolyte: weighing sodium dodecyl sulfate, and dissolving the sodium dodecyl sulfate in a hydrochloric acid solution with the mass concentration of 2-10% to prepare an electrolyte with the concentration of 2-60 g/L of sodium dodecyl sulfate;
(3) adjusting the anodic oxidation voltage to 10-30V, setting the temperature to 20-70 ℃, and carrying out constant-voltage reaction for 0.5-5 h in the electrolyte prepared in the step (2);
(4) and taking out the metal tungsten sheet, washing with deionized water, and drying to obtain the hydrated tungsten trioxide/tungsten self-supporting electrode.
And ultrasonically cleaning the metal tungsten sheet in acetone, isopropanol, ethanol and deionized water for 15min in sequence, finally cleaning with deionized water, drying, and then taking the metal tungsten sheet as an anode for reaction.
Preferably, the anodic oxidation electrolyte is formulated as follows: 0.04g of sodium dodecyl sulfate and 50mL of 6% hydrochloric acid solution.
Preferably, the anodic oxidation voltage in step (3) is 20V, the temperature is 50 ℃, and the constant-voltage oxidation time is 2 h.
According to the method, a metal tungsten sheet is used as a substrate, an anodic oxidation method is adopted to prepare the hydrated tungsten trioxide nanosheet/tungsten self-supporting electrode in a sodium dodecyl sulfate-hydrochloric acid aqueous solution, and the hydrated tungsten trioxide nanosheet/tungsten electrode material with different sizes and shapes is obtained by regulating and controlling the addition amount of sodium dodecyl sulfate.
The invention has the following beneficial effects: the hydrated tungsten trioxide nanosheet prepared by the method is uniform in shape and complete in structure, and the nanosheet vertically grows on a tungsten substrate, is firmly combined with a metal tungsten substrate and is not easy to separate; in addition, the method has the advantages of simple process, high preparation repeatability, low requirement on equipment, cheap and easily-obtained related chemicals and great prospect in the aspect of industrial application.
(IV) description of the drawings
Fig. 1 is an XRD pattern of the hydrated tungsten trioxide nanosheet/tungsten self-supporting electrode material prepared in example 1;
fig. 2 is an SEM photograph of the hydrated tungsten trioxide nanosheets/tungsten self-supporting electrode material prepared in example 1;
fig. 3 is a constant current charge and discharge performance spectrum of the hydrated tungsten trioxide nanosheet/tungsten self-supporting electrode material prepared in example 1;
fig. 4 is an XRD pattern of the hydrated tungsten trioxide nanosheet/tungsten self-supporting electrode material prepared in example 2;
fig. 5 is an SEM image of hydrated tungsten trioxide nanosheets/tungsten self-supporting electrode material prepared in example 2;
fig. 6 is a constant current charge and discharge spectrum of the hydrated tungsten trioxide nanosheet/tungsten self-supporting electrode material prepared in example 2;
fig. 7 is an XRD pattern of the hydrated tungsten trioxide nanosheet/tungsten self-supporting electrode material prepared in example 3;
fig. 8 is an SEM image of hydrated tungsten trioxide nanosheets/tungsten self-supporting electrode material prepared in example 3;
fig. 9 is a constant current charge and discharge spectrum of the hydrated tungsten trioxide nanosheet/tungsten self-supporting electrode material prepared in example 3;
fig. 10 is an XRD pattern of the hydrated tungsten trioxide nanosheet/tungsten self-supporting electrode material prepared in example 4;
fig. 11 is an SEM image of hydrated tungsten trioxide nanosheets/tungsten self-supporting electrode material prepared in example 4;
fig. 12 is a constant current charge and discharge spectrum of the hydrated tungsten trioxide nanosheet/tungsten self-supporting electrode material prepared in example 4.
(V) detailed description of the preferred embodiments
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
example 1:
a metal tungsten sheet (Alfa Angsa chemical Co., Ltd., purity 99.999%, the same below) (10 mm. times.20 mm, thickness 0.08mm) was cleaned by ultrasonic cleaning in acetone, isopropanol, ethanol and deionized water for 20min in sequence. Preparing 50mL of hydrochloric acid solution with the mass concentration of 6%; to the above solution, 0.04g of sodium lauryl sulfate (Aladdin chemical Co., Ltd., powder, the same applies hereinafter) was accurately weighed. Placing a metal tungsten sheet (the purity of 99.99 percent, the same below) (20mm multiplied by 20mm, the thickness of 0.2mm) as an anode and a metal titanium sheet (the purity of 99.99 percent, the same below) as a cathode into a prepared sodium dodecyl sulfate-hydrochloric acid electrolyte, keeping the electrode distance at 2cm, controlling the temperature of the electrolyte at 50 ℃, and carrying out constant-pressure oxidation for 2 hours under the voltage of 20 v; after the reaction, washing the metal tungsten sheet with deionized water, and drying to obtain the hydrated tungsten trioxide nanosheet/tungsten self-supporting electrode.
XRD of the prepared material is shown in figure 1, and phase matching shows that the prepared nanosheet is mainly hydrated tungsten trioxide; the microstructure and morphology of the prepared material are shown in FIG. 2, and it can be seen that a large number of lamellar structures with uniform morphology and uniform thickness vertically grow on the tungsten substrate. Constant current charge and discharge performance as shown in fig. 3, the mass specific capacity of the electrode material was calculated to be 129F/g by charging and discharging at a current density of 3A/g.
Example 2:
the metal tungsten sheet (10mm multiplied by 20mm, thickness 0.08mm) is cleaned by ultrasonic cleaning in acetone, isopropanol, ethanol and deionized water for 20min in sequence for standby. Preparing 50mL of hydrochloric acid solution with the mass concentration of 6%; 0.08g of sodium lauryl sulfate was accurately weighed and added to the above solution. Placing a metal tungsten sheet as an anode and a metal titanium sheet (20mm multiplied by 20mm, thickness of 0.2mm) as a cathode into prepared sodium dodecyl sulfate-hydrochloric acid electrolyte, keeping the electrode spacing at 2cm, controlling the temperature of the electrolyte at 50 ℃, and carrying out constant-pressure oxidation for 2h under 20v voltage; after the reaction, washing the metal tungsten sheet with deionized water, and drying to obtain the hydrated tungsten trioxide nanosheet/tungsten self-supporting electrode.
XRD of the prepared material is shown in figure 4, and phase matching shows that the prepared nanosheet is mainly hydrated tungsten trioxide; the microstructure and the morphology of the prepared material are shown in fig. 5, and it can be seen that a large number of flaky structures with uniform morphology vertically grow on a tungsten substrate, and the thickness of the nanosheet is about 50nm and is uniform through measurement. The substance grown on the surface of the prepared electrode was scraped off and weighed, and its mass was 0.6 mg. As shown in FIG. 6, it can be seen that the mass-to-volume ratio of the electrode material obtained by calculation of charging and discharging at a current density of 3A/g is 206F/g, which shows excellent electrochemical performance.
Example 3:
the metal tungsten sheet (10mm multiplied by 20mm, thickness 0.08mm) is cleaned by ultrasonic cleaning in acetone, isopropanol, ethanol and deionized water for 20min in sequence for standby. Preparing 50mL of hydrochloric acid solution with the mass concentration of 6%; accurately 0.12g of sodium lauryl sulfate was weighed into the above solution. Placing a metal tungsten sheet as an anode and a metal titanium sheet (20mm multiplied by 20mm, thickness of 0.2mm) as a cathode into prepared sodium dodecyl sulfate-hydrochloric acid electrolyte, keeping the electrode spacing at 2cm, controlling the temperature of the electrolyte at 50 ℃, and carrying out constant-pressure oxidation for 2h under 20v voltage; after the reaction, washing the metal tungsten sheet with deionized water, and drying to obtain the hydrated tungsten trioxide nanosheet/tungsten self-supporting electrode.
XRD of the prepared material is shown in figure 7, and phase matching shows that the prepared nanosheet is mainly hydrated tungsten trioxide; the microstructure and morphology of the prepared material are shown in FIG. 8, and it can be seen that a large number of lamellar structures with uniform morphology and uniform thickness vertically grow on the tungsten substrate. The constant current charge and discharge performance is shown in fig. 9, and it can be seen that the mass specific capacity of the electrode material is calculated to be 150F/g when the electrode material is charged and discharged at a current density of 3A/g.
Example 4:
the metal tungsten sheet (10mm multiplied by 20mm, thickness 0.08mm) is cleaned by ultrasonic cleaning in acetone, isopropanol, ethanol and deionized water for 20min respectively for standby. Preparing 50mL of hydrochloric acid solution with the mass concentration of 6%; to the above solution, 0.16g of sodium lauryl sulfate was accurately weighed. Placing a metal tungsten sheet as an anode and a metal titanium sheet (20mm multiplied by 20mm, thickness of 0.2mm) as a cathode into prepared sodium dodecyl sulfate-hydrochloric acid electrolyte, keeping the electrode spacing at 2cm, controlling the temperature of the electrolyte at 50 ℃, and carrying out constant-pressure oxidation for 2h under 20v voltage; after the reaction, washing the metal tungsten sheet with deionized water, and drying to obtain the hydrated tungsten trioxide nanosheet/tungsten self-supporting electrode.
XRD of the prepared material is shown in figure 10, and phase matching shows that the prepared nanosheet is mainly hydrated tungsten trioxide; the microstructure and morphology of the prepared material are shown in fig. 11, and it can be seen that a large number of lamellar structures with uniform morphology and uniform thickness vertically grow on the tungsten substrate. Constant current charge and discharge performance as shown in fig. 12, it can be seen that the mass specific capacity of the electrode material calculated by charging and discharging at a current density of 3A/g is 130F/g.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. A hydrated tungsten trioxide/tungsten self-supporting electrode is prepared by the following method:
(1) taking a metal tungsten sheet as an anode and a metal titanium sheet as a cathode, wherein the distance between the anode and the cathode is 1-3 cm;
(2) preparing an anodic oxidation electrolyte: the anodic oxidation electrolyte is prepared from the following components: 0.04g of sodium dodecyl sulfate and 50mL of hydrochloric acid solution with the mass concentration of 6 percent;
(3) adjusting the anodic oxidation voltage to 10-30V, setting the temperature to 20-70 ℃, and carrying out constant-voltage reaction for 0.5-5 h in the electrolyte prepared in the step (2);
(4) and taking out the metal tungsten sheet, washing with deionized water, and drying to obtain the hydrated tungsten trioxide/tungsten self-supporting electrode.
2. The hydrated tungsten trioxide/tungsten self-supporting electrode according to claim 1 wherein the metallic tungsten plate has dimensions of 10 x 10mm and a thickness of 0.08 mm; the size of the metal titanium sheet is 20mm multiplied by 20mm, and the thickness is 0.2 mm.
3. A method of making the hydrated tungsten trioxide/tungsten self-supporting electrode of claim 1, the method comprising:
(1) taking a metal tungsten sheet as an anode and a metal titanium sheet as a cathode, wherein the distance between the anode and the cathode is 1-3 cm; the metal tungsten sheet is sequentially ultrasonically cleaned in acetone, isopropanol, ethanol and deionized water for 15min, finally cleaned by the deionized water and dried, and then used as an anode for reaction;
(2) preparing an anodic oxidation electrolyte: the anodic oxidation electrolyte is prepared from the following components: 0.04g of sodium dodecyl sulfate and 50mL of hydrochloric acid solution with the mass concentration of 6 percent;
(3) adjusting the anodic oxidation voltage to 10-30V, setting the temperature to 20-70 ℃, and carrying out constant-voltage reaction for 0.5-5 h in the electrolyte prepared in the step (2);
(4) and taking out the metal tungsten sheet, washing with deionized water, and drying to obtain the hydrated tungsten trioxide/tungsten self-supporting electrode.
4. The method of claim 3, wherein the anodic oxidation voltage in step (3) is 20V, the temperature is 50 ℃, and the constant voltage oxidation time is 2 h.
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