CN114751455B - Preparation method of modified molybdenum trioxide electrode material - Google Patents
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Abstract
The invention discloses a preparation method of a modified molybdenum trioxide electrode material, which is characterized in that a surfactant is added in the process of preparing banded molybdenum trioxide by adopting a one-step method, the surfactant can form a micelle structure in an aqueous solution, and a crystal face preferential orientation growth process of molybdenum trioxide crystal nucleus in a hydrothermal process is guided to obtain the modified molybdenum trioxide material with structural difference with common banded molybdenum trioxide. Compared with the common banded molybdenum trioxide, the prepared modified molybdenum trioxide material has the advantages that the appearance is changed from a complete banded structure to a novel structure with nano particles attached between nano bands besides the change of the preferential orientation of crystals, the morphology structure increases the infiltration and migration of electrolyte ions in an electrode material, the electron transmission rate is increased, the further improvement of the charge storage capacity is facilitated, so that the molybdenum trioxide material has high specific capacitance and excellent rate capability, and can be used as the electrode material of secondary energy storage devices such as high specific energy supercapacitors, lithium ion batteries and the like.
Description
Technical Field
The invention relates to a preparation method of a modified molybdenum trioxide electrode material, in particular to a method for modifying the molybdenum trioxide material by using a surfactant, which is mainly applied to the field of electrochemical energy storage as a supercapacitor electrode material.
Background
With the rapid development of industrial technology, the reserves of traditional energy sources are continuously reduced, the environmental pollution is increasingly serious, and the development of green sustainable energy sources becomes a research hotspot with global attention. The electrochemical capacitor is used as a novel energy storage device, has high energy density (1-10 Wh/kg), high power density (1 k-100 kW/kg), maintenance-free, high charge and discharge efficiency and long cycle life (up to 10) 5 More than once), the use temperature range is wide, and the method is environment-friendly. Electrode materials are critical to the improvement of capacitor performance. Pseudocapacitors operate based on reversible rapid redox reactions at or near the surface of an electroactive material, which typically have high specific capacitance values. Transition metal oxides are a common pseudocapacitive material. Molybdenum trioxide has attracted extensive research interest by researchers due to the advantages of high electrochemical activity, excellent stability, high theoretical specific capacitance, low cost, environmental friendliness and the like of the simple preparation process. However, the pure molybdenum trioxide has a limited application because of its poor rate of electron transport, resulting in its poor capacitor rate capability. By modifying the structure and morphology of molybdenum trioxide, the charge transmission capacity of the molybdenum trioxide is hopeful to be improved, and the electrochemical performance of the molybdenum trioxide is further improved.
Disclosure of Invention
The invention aims to provide a preparation method of a modified molybdenum trioxide electrode material, which improves the electrochemical performance by changing the structure of the modified molybdenum trioxide electrode material.
1. Preparation of modified molybdenum trioxide electrode material
The method for preparing the modified molybdenum trioxide material comprises the steps of fully reacting molybdenum powder and hydrogen peroxide solution in ice bath until the molybdenum powder and the hydrogen peroxide solution are orange transparent solution, adding deionized water for dilution, and stirring for 30-60 minutes to generate yellow solution; adding a surfactant into the yellow solution, heating and stirring until the surfactant is completely dissolved; then placing the mixed solution into a stainless steel reaction kettle with a tetrafluoroethylene liner, and performing hydrothermal reaction for 10-30 hours at 160-220 ℃; and after the reaction is finished, carrying out suction filtration, washing a product, and drying to obtain the modified molybdenum trioxide material.
The mol ratio of the molybdenum powder to the hydrogen peroxide is 1:3-1:10 (preferably 1:6-1:10); the mass concentration of the hydrogen peroxide solution is 20% -30% (preferably 30%).
The surfactant is selected from one of SDS (sodium dodecyl sulfonate), DBS (sodium dodecyl benzene sulfonate), CTAB (cetyltrimethylammonium bromide), P123 (polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer) or F127 (polyoxyethylene-polyoxypropylene-polyoxyethylene amphiphilic block copolymer), preferably P123 and F127. The concentration of the surfactant in the mixed solution is 0.001-0.05 g/mL (preferably 0.005-0.01 g/mL).
2. Structure of modified molybdenum trioxide material
The morphology and structure of the modified molybdenum trioxide material will be described by taking the common molybdenum trioxide and the modified common molybdenum trioxide prepared in example 1 as examples.
Fig. 1 and fig. 2 are scanning electron microscope pictures of common molybdenum trioxide and modified common molybdenum trioxide, respectively. As can be seen from the scanning electron microscope pictures, the common molybdenum trioxide mainly consists of a strip-shaped structure with the length of a few micrometers and the width of 200 nm. The modified molybdenum trioxide material is mainly composed of a ribbon structure with a length of several micrometers and nano particles with a particle size of about 200 and nm. Compared with the appearance of common molybdenum trioxide, the structure of the modified molybdenum trioxide is obviously more crushed, a plurality of void structures are increased, and the structure is convenient for the infiltration and rapid transmission of electrolyte ions.
Fig. 3 is an XRD pattern of common molybdenum trioxide and modified molybdenum trioxide. As can be seen from XRD results of FIG. 3, the diffraction peaks of the produced band-shaped molybdenum trioxide are narrow and high, and all the peak positions correspond to the crystal form (. Alpha. -MoO) of pure orthorhombic molybdenum trioxide 3 JCPDS No. 05-0508), and the apparent preferential orientation of the (020), (040), (060) crystal planes, indicating that the structure of the band-shaped molybdenum trioxide is mainly grown in the (010) direction. The XRD test results further show that the modified molybdenum trioxide also accords with the structure of pure orthorhombic molybdenum trioxide. But the diffraction peak intensity is obviously reduced, and the preferential orientation of the crystal structure is also obviously changed, which is moreMeets the standard spectrogram of the molybdenum trioxide with the orthogonal phase. The surfactant P123 plays a remarkable role in the hydrothermal preparation process of molybdenum trioxide, and changes the preferential oriented growth of the crystal structure of the surfactant P123.
Fig. 4 is a Raman diagram of a general molybdenum trioxide and a modified molybdenum trioxide. The Raman plot further demonstrates that the modified molybdenum trioxide material is pure, impurity-free, orthorhombic molybdenum trioxide.
3. Electrochemical performance test
And (3) taking a common molybdenum trioxide material and a modified molybdenum trioxide material as active substances, respectively mixing the active substances with a conductive agent carbon black and a binder polytetrafluoroethylene according to a mass ratio of 8:1:1 to form slurry, coating the slurry on foam nickel, and drying the coated foam nickel at 100 ℃ for 12 hours to obtain the electrode plate to be characterized. The three-electrode system electrochemical workstation is adopted for testing, wherein a saturated calomel electrode is used as a reference electrode, a platinum sheet is used as a counter electrode, the prepared electrode sheet is used as a working electrode, and 1mol/L potassium chloride solution is used as electrolyte.
FIG. 5 shows that the scanning speed of the common molybdenum trioxide and the modified molybdenum trioxide is 5mV s -1 Comparison cyclic voltammogram at time. FIG. 5 shows that the cyclic voltammograms of BMO and BMO@P electrodes both have obvious redox peaks, indicating that the prepared common molybdenum trioxide and modified molybdenum trioxide materials are electrode materials with pseudocapacitive energy storage behavior as the main materials. In addition, the BMO@P electrode exhibits a significantly larger integrated area, which corresponds to the charge storage capacity, which indicates that the modified molybdenum trioxide material has a higher specific capacitance value.
Fig. 6 and 7 are cyclic voltammograms of the common molybdenum trioxide and the modified molybdenum trioxide at different sweep rates, respectively. As the scan speed increases, both cyclic voltammograms deform to some extent due to the limited slow diffusion behavior of electrolyte ions at high scan speeds. In addition, the intensity of the redox peak in the curve also gradually decreases with the increase of the scanning speed, which indicates the slower intercalation dynamics of electrolyte ions in the electrode material at high scanning speed.
FIG. 8 is a graph showing the ratio of the common molybdenum trioxide to the modified molybdenum trioxide at different scanning speedsCapacitance change diagram. And obtaining the rate performance result by calculating the mass ratio capacitance value of the electrode at different scanning speeds. FIG. 8 shows that at a sweep rate of 5mV s -1 The specific capacitance of the BMO electrode was 68.8 Fg -1 （488.5 mF cm -2 ) And the specific capacitance of the BMO@P electrode was 105.7 Fg -1 （708.2 mF cm -2 ). With a further increase in sweep speed to 40 mV s -1 When the specific capacitance of the BMO electrode is reduced to 19.7 Fg -1 （139.9 mF cm -2 ) The specific capacitance of the BMO@P electrode can still be kept at 40.1 Fg -1 （268.7 mF cm -2 ). The results show that the BMO@P electrode has more excellent charge storage capacity.
Fig. 9 is a graph showing the impedance of the conventional molybdenum trioxide and the modified molybdenum trioxide. As seen from fig. 9, the bmo@p electrode exhibited a smaller charge transfer resistance than the BMO electrode, and the straight portion of the former at low frequency was more nearly vertical, indicating that the bmo@p electrode had better capacitive performance, consistent with the previous analysis results. The modification of the morphology and structure of the molybdenum trioxide material is illustrated, and the electrochemical performance of the molybdenum trioxide material is obviously improved.
In summary, the invention adopts a one-step method to add the surfactant in the process of preparing the banded molybdenum trioxide, the surfactant can form a micelle structure in the aqueous solution, the crystal face of the molybdenum trioxide crystal nucleus is guided to preferentially orient and grow in the hydrothermal process, meanwhile, the surfactant can play a role in guiding and connecting the crystal face, and finally the modified molybdenum trioxide material with the structural difference with the common banded molybdenum trioxide is obtained. Compared with the common banded molybdenum trioxide, the prepared modified molybdenum trioxide material has the advantages that the appearance is changed from a complete banded structure to a novel structure with nano particles attached between nano bands besides the change of the preferential orientation of crystals, the morphology structure increases the infiltration and migration of electrolyte ions in an electrode material, the electron transmission rate is increased, the further improvement of the charge storage capacity is facilitated, so that the molybdenum trioxide material has high specific capacitance and excellent rate capability, and can be used as the electrode material of secondary energy storage devices such as high specific energy supercapacitors, lithium ion batteries and the like.
Drawings
Fig. 1 is a scanning electron microscope picture of a general band-shaped molybdenum trioxide (BMO).
Fig. 2 is a scanning electron microscope picture of a modified molybdenum trioxide material (bmo@p).
Fig. 3 is an XRD pattern of common molybdenum trioxide and modified molybdenum trioxide.
Fig. 4 is a Raman diagram of a general molybdenum trioxide and a modified molybdenum trioxide.
FIG. 5 is a graph showing that the scanning speed of the common molybdenum trioxide and the modified molybdenum trioxide is 5mVs -1 Comparison cyclic voltammogram at time.
Fig. 6 is a graph of cyclic voltammograms of a conventional molybdenum trioxide at different sweep rates.
FIG. 7 is a cyclic voltammogram of modified molybdenum trioxide at different sweep rates.
Fig. 8 is a graph showing changes in specific capacitance of a general molybdenum trioxide and a modified molybdenum trioxide at different scanning speeds.
Fig. 9 is a graph showing the impedance of the conventional molybdenum trioxide and the modified molybdenum trioxide.
Detailed Description
The preparation, structure and performance of the modified molybdenum trioxide material of the invention are further illustrated by the following specific examples.
Example 1
0.192g of molybdenum powder is weighed and added into a 30% hydrogen peroxide solution of 3.2. 3.2 mL, and the solution is continuously stirred in an ice bath until the solution is orange transparent, then 36.8mL of deionized water is added to dilute the solution, and stirring is continued for 30 minutes; adding 0.32g of P123, and heating to dissolve to transparent solution; transferring the solution into a 100mL tetrafluoroethylene liner, putting the tetrafluoroethylene liner into a stainless steel high-pressure reaction kettle, and keeping the temperature at 200 ℃ for 24 hours; and naturally cooling, filtering, washing the precipitate with deionized water and ethanol respectively, and drying to obtain the novel modified molybdenum trioxide material, which is named BMO@P.
Comparative example: weighing 0.192g of molybdenum powder, adding the molybdenum powder into a hydrogen peroxide solution with the mass fraction of 30% of 3.2 and mL, continuously stirring the solution in an ice bath until the solution is orange transparent, then adding 36.8mL of deionized water to dilute the solution, and continuously stirring the solution for 30 minutes; the solution was transferred to a 100mL tetrafluoroethylene liner and placed in a stainless steel autoclave maintained at 200℃for 24 hours. And naturally cooling, filtering, washing the precipitate with deionized water and ethanol respectively, and drying to obtain the common molybdenum trioxide material, wherein the BMO is marked.
The electrode plate is manufactured according to the method, and the electrochemical performance of the electrode plate is tested. BMO electrode is scanned at a speed of 5mV s -1 The specific capacitance at the time was 68.8 Fg -1 （488.5 mF cm -2 ) As the sweep rate increases to 40 mV s -1 The specific capacitance value is reduced to 19.7 Fg -1 （139.9 mF cm -2 ). BMO@P electrode has a scanning speed of 5mV s -1 The specific capacitance at the time was 105.7 Fg -1 （708.2 mF cm -2 ) As the sweep rate increases to 40 mV s -1 The specific capacitance of the electrode can still be kept at 40.1 Fg -1 （268.7 mF cm -2 ）。
Example 2
0.192g of molybdenum powder is weighed and added into a 30% hydrogen peroxide solution of 3.2. 3.2 mL, and the solution is continuously stirred in an ice bath until the solution is orange transparent, then 36.8mL of deionized water is added to dilute the solution, and stirring is continued for 30 minutes; adding 0.32g of P123, and heating to dissolve to transparent solution; transferring the solution into a 100mL tetrafluoroethylene liner, putting the tetrafluoroethylene liner into a stainless steel high-pressure reaction kettle, and keeping the temperature at 180 ℃ for 20 hours; naturally cooling, filtering, washing the precipitate with deionized water and ethanol, and drying to obtain the modified molybdenum trioxide material.
The electrode plate is manufactured according to the method, and the electrochemical performance of the electrode plate is tested. BMO@P electrode has a scanning speed of 5mV s -1 The specific capacitance at the time was 101.2 Fg -1 （688.2 mF cm -2 ）。
Example 3
0.192g of molybdenum powder is weighed and added into a 30% hydrogen peroxide solution of 3.2. 3.2 mL, and the solution is continuously stirred in an ice bath until the solution is orange transparent, then 36.8mL of deionized water is added to dilute the solution, and stirring is continued for 30 minutes; 0.40g of P123 is added, and the mixture is heated and dissolved into transparent solution; the solution was transferred to a 100mL tetrafluoroethylene liner and placed in a stainless steel autoclave maintained at 200℃for 24 hours. Naturally cooling, filtering, washing the precipitate with deionized water and ethanol, and drying to obtain the modified molybdenum trioxide material.
The electrode plate is manufactured according to the method, and the electrochemical performance of the electrode plate is tested. BMO@P electrode has a scanning speed of 5mV s -1 The specific capacitance at the time was 104.2 Fg -1 （698.1 mF cm -2 ）。
Example 4
0.192g of molybdenum powder is weighed and added into a 30% hydrogen peroxide solution of 3.2. 3.2 mL, and the solution is continuously stirred in an ice bath until the solution is orange transparent, then 36.8mL of deionized water is added to dilute the solution, and stirring is continued for 30 minutes; then 0.32g F127 is added, and the mixture is heated and dissolved into transparent solution; transferring the solution into a 100mL tetrafluoroethylene liner, putting the tetrafluoroethylene liner into a stainless steel high-pressure reaction kettle, and keeping the temperature at 200 ℃ for 24 hours; naturally cooling, filtering, washing the precipitate with deionized water and ethanol, and drying to obtain the modified molybdenum trioxide material.
The electrode plate is manufactured according to the method, and the electrochemical performance of the electrode plate is tested. BMO@P electrode has a scanning speed of 5mV s -1 The specific capacitance at the time was 98.7 Fg -1 （671.2 mF cm -2 ）。
Claims (4)
1. The preparation method of the modified molybdenum trioxide electrode material comprises the steps of fully reacting molybdenum powder and hydrogen peroxide solution in ice bath until the molybdenum powder and the hydrogen peroxide solution are orange transparent solution, adding deionized water for dilution, and stirring for 30-60 minutes to generate yellow solution; adding a surfactant into the yellow solution, heating and stirring until the surfactant is completely dissolved; then placing the mixed solution into a stainless steel reaction kettle with a tetrafluoroethylene liner, and performing hydrothermal reaction for 10-30 hours at 160-220 ℃; after the reaction is finished, carrying out suction filtration, washing a product, and drying to obtain a modified molybdenum trioxide material;
the surfactant is selected from polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123) or polyoxyethylene-polyoxypropylene-polyoxyethylene amphiphilic block copolymer (F127).
2. The method for preparing the modified molybdenum trioxide electrode material according to claim 1, characterized in that: the mol ratio of the molybdenum powder to the hydrogen peroxide is 1:3-1:10.
3. The method for preparing the modified molybdenum trioxide electrode material according to claim 1, characterized in that: the mass concentration of the hydrogen peroxide solution is 20% -30%.
4. The method for preparing the modified molybdenum trioxide electrode material according to claim 1, characterized in that: the concentration of the surfactant in the mixed solution is 0.001-0.05 g/mL.
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