Synthesis of FeNi nanocone structures for electrochemical filtering
By preparing FeNi nanocone arrays through electrodeposition, the resistance and ion channel problems of filter supercapacitor materials were solved, achieving fast response and high-efficiency filtering performance, which is suitable for AC filtering applications.
Patent Information
- Application Number
- CN202410653556.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-24
- Publication Date
- 2025-11-25
AI Technical Summary
Existing filter supercapacitor materials have high resistance and complex ion transport channels, resulting in poor frequency response performance and making it difficult to meet the requirements for fast response capabilities.
FeNi nanocone arrays were prepared by electrodeposition, with the electrodeposition temperature controlled at 65-80℃, the time at 5-15 min, and the current density at 20-30 mA cm⁻², forming FeNi nanocones with high curvature structures for use as electrodes in supercapacitors.
FeNi nanocone arrays exhibit a high electric field environment in AC filtering, which promotes rapid ion transport, reduces interface resistance, achieves high impedance phase angle and low equivalent series resistance, and improves filtering performance.
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Figure CN121006584A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the field of alternating current filter material preparation. FeNi nano cone arrays are prepared by electrodeposition method, and their filter performance is tested and analyzed to verify their application potential in the field of alternating current filtering. BACKGROUND
[0002] With the continuous development of modern electronic equipment, people's performance requirements for supercapacitors are gradually increasing. Filtered supercapacitors, as an application branch of supercapacitors, have higher requirements for the rapid response capability of the device. In order to realize the performance of the filtered supercapacitor, it is necessary to ensure that the material has small resistance and fast ion transport channel, and at the same time has large specific surface area. At present, the electrode material of the filtered supercapacitor mainly includes carbon nanomaterials with high surface area, but due to the poor conductivity of carbon materials and the complex three-dimensional structure, the distance of ion movement in the material is prolonged, and the frequency response performance of the material is reduced.
[0003] Metal nanocone, as a one-dimensional nanomaterial with high-curvature structure of sharp tip, has good conductivity and unique physical properties. Designing the electrode into the morphology of nanocone can expose more active sites, and more importantly, after applying voltage to the metal nanocone, the sharp tip effect of the nanocone will form a high-intensity local electric field at the top. This effect can accelerate the transmission of ions and charges, thereby improving the rapid response capability of the material. Based on the above unique properties of metal nanocone in electrochemistry, we judge that the application of FeNi nanocone structure material to the field of alternating current filtered supercapacitors has certain research prospects. SUMMARY
[0004] This paper explores the possibility of FeNi nanocone material for alternating current filtered supercapacitors, introduces FeNi nanocone, a nanomaterial with unique electrochemical properties, into the filtering field, and provides a new idea for preparing filtered electrode materials with fast response performance.
[0005] To achieve the above purpose, the electrodeposition temperature, electrodeposition time and electrodeposition current density need to be controlled:
[0006] The electrodeposition temperature requirement must be controlled within 65-80℃, and oil bath heating is required, and the liquid is heated for more than 4 hours before deposition to convert the substance, and the same temperature is maintained during deposition.
[0007] The electrodeposition time requirement is controlled between 5-15min to ensure that the electrode will not affect the electrode performance due to the thick solid layer.
[0008] The electrodeposition current density requirement is controlled between 20-30mA cm-2 thereby regulating the curvature of the FeNi nanotaper.
[0009] Synthesis of FeNi nanotaper structure for electrochemical filtering, comprising the following steps:
[0010] Step 1, FeNi nanotaper electrodeposition liquid configuration: take 50ml deionized water, add 10g NiCl2·6H2O, 2.01g H3BO3, 4.9g NH4Cl, 2g FeCl2·4H2O into the inner, ultrasonic dispersion for 2h to configure the deposition liquid.
[0011] Step 2, FeNi nanotaper electrodeposition preparation: immerse the beaker containing the deposition liquid into the oil bath pot, set the oil bath temperature to 65-80℃, power supply with direct current power supply in the two electrode system, use platinum sheet as the counter electrode, titanium sheet as the anode, control the current density to 10-30mA cm -2 , control the deposition time to 5-15min, make the FeNi nanotaper grow on the surface of the titanium sheet, after the reaction, immerse the titanium sheet with grown FeNi nanotaper into deionized water for soaking and cleaning, and dry to prepare the sample. Under different electrodeposition temperature, current density and electrodeposition time, the nanotaper structure electrode with different morphology can be obtained.
[0012] Step 3, assembly of FeNi nanotaper supercapacitor: cut the FeNi nanotaper electrode into a piece with the size of 1.5*2cm, place symmetrically, add a piece of glass fiber diaphragm in the middle, drop 2-3 drops of 1M Na2SO4 electrolyte, and package with the tablet press to obtain the FeNi nanotaper supercapacitor.
[0013] The innovation points and positive effects of the present application are as follows:
[0014] The feasibility of FeNi nanocone structure for AC filtering is studied by analyzing the FeNi nanocone structure and the electrochemical performance of the FeNi nanocone structure under the filtering parameters. Thanks to the particularity of the surface morphology of the FeNi nanocone, it is creatively used in the field of AC filtering, and the performance is combined with the expectation, which shows the potential in the application of AC filtering. The rich high-curvature structure on the surface of the FeNi nanocone can produce an enhanced electric field environment, promote the rapid transfer of ions near the cone, and due to the open structure of its surface, the ions will not be blocked, and after applying voltage, the FeNi nanocone can produce an electric field about 4 times higher than the plane structure, which means that the nanocone array structure has a natural advantage in filtering and can meet the rapid response required by AC filtering. At the same time, in-situ deposition makes the FeNi nanocone closely contact with the substrate, and the interface resistance is small, which ensures that the supercapacitor has a small equivalent series resistance. The supercapacitor based on the FeNi nanocone array shows a high impedance phase angle of -79.4° and a low relaxation time constant of 0.70 ms at 120 Hz, and at the same time, the device has a specific capacitance of 86.8 μFcm -2 and a low equivalent series resistance of 0.68 Ω, which shows good electrochemical performance of the device. In addition, we test the filtering performance of the device at a frequency of 60 Hz, and the results show that the FeNi nanocone supercapacitor can effectively convert AC signals into DC signals, and the ripple coefficient is only 5.2%, which fully illustrates the good AC filtering performance of the device. The present application provides a new idea for the application of metal nanocone structure in the field of AC filtering. BRIEF DESCRIPTION OF DRAWINGS
[0015] Figure 1 are scanning electron microscope images of supercapacitors prepared by FeNi nanocones under different electrodeposition temperatures.
[0016] Figure 2 are electrochemical test diagrams of supercapacitors prepared by FeNi nanocones under different electrodeposition temperatures, wherein a is a Bode plot, b is a Nyquist plot, and c is a phase angle and CA relationship diagram with deposition temperature.
[0017] Figure 3 are AC filtering test diagrams of supercapacitors prepared by FeNi nanocones under different electrodeposition temperatures.
[0018] Figure 4 are scanning electron microscope images of supercapacitors prepared by FeNi nanocones under different electrodeposition times.
[0019] Figure 5 are electrochemical test diagrams of supercapacitors prepared by FeNi nanocones under different electrodeposition times, wherein a is a Bode plot, b is a Nyquist plot, and c is a phase angle and CA relationship diagram with deposition time.A Deposition time dependence graph.
[0020] Figure 6 AC filter test graph of supercapacitors prepared by FeNi nanotaper for different deposition times.
[0021] Figure 7 Scanning electron microscope images of supercapacitors prepared by FeNi nanotaper for different current densities.
[0022] Figure 8 Electrochemical test graphs of supercapacitors prepared by FeNi nanotaper for different current densities, wherein a graph is a Bode graph, b graph is a Nyquist graph, c graph is a phase angle and C A Deposition current density dependence graph.
[0023] Figure 9 AC filter test graph of supercapacitors prepared by FeNi nanotaper for different current densities. DETAILED DESCRIPTION
[0024] In order to make the technical scheme of the present application clearer, the present application will be further described below in combination with examples, and any conclusions and schemes obtained by replacing and routine reasoning of the technical scheme of the present application all belong to the protection scope of the embodiment examples of the present application.
[0025] Example 1:
[0026] Firstly, 1.5 cm x 2 cm titanium sheets were cleaned with deionized water and ethanol respectively for 20 min by ultrasonic cleaning, and the cleaned titanium sheets were dried in a blast drying oven for 1 h.
[0027] Then, 100 ml capacity beakers were taken, 50 ml deionized water was added into each beaker, and then 10 g of NiCl2·6H2O, 2.01 g of H3BO3, 4.9 g of NH4Cl, and 2 g of FeCl2·4H2O were added respectively, and ultrasonic dispersion was performed for 2 h to configure the deposition solution.
[0028] After that, direct current power supply was used for power supply in an oil bath (temperatures were 65℃, 68℃, 70℃, 72℃, 75℃, and 80℃ respectively) environment, platinum sheet was used as a counter electrode, titanium sheet was used as an anode, and FeNi nanotaper was grown on the surface of the titanium sheet under a constant current density of 27 mA cm -2 After that, direct current power supply was used for power supply in an oil bath (temperatures were 65℃, 68℃, 70℃, 72℃, 75℃, and 80℃ respectively) environment, platinum sheet was used as a counter electrode, titanium sheet was used as an anode, and FeNi nanotaper was grown on the surface of the titanium sheet under a constant current density of 27 mA cm
[0029] Figure 1 Scanning electron microscope images of FeNi nanotaper structure electrodes for different deposition temperatures. As Figure 1As shown, when the temperature is increased, the structure of the FeNi nanotaper gradually becomes obvious, and the spherical structure at low temperature gradually evolves into a uniform FeNi nanotaper structure. The length of the FeNi nanotaper is about 200 nm.
[0030] The electrochemical performance of the FeNi nanotaper supercapacitor obtained in this example is shown in Figure 2 The results show that the FeNi nanotaper structure can exhibit good electrochemical performance when the electrodeposition temperature is 65-80°C. With the increase of the deposition temperature, the electrochemical performance of the FeNi nanotaper supercapacitor shows a trend of first increasing and then decreasing.
[0031] Figure 3 The filter performance test diagram of the FeNi nanotaper structure supercapacitor obtained in this example is shown. The results show that the FeNi nanotaper supercapacitor prepared in this scheme can effectively convert the alternating signal into a smooth direct current signal for output.
[0032] Example 2
[0033] First, a titanium sheet with a size of 1.5 cm x 2 cm was ultrasonically cleaned with deionized water and ethanol for 20 min, respectively, and the cleaned titanium sheet was dried in a forced air drying oven for 1 h.
[0034] Then, take a 100 ml capacity beaker, add 50 ml deionized water inside, then add 10 g NiCl2·6H2O, 2.01 g H3BO3, 4.9 g NH4Cl, and 2 g FeCl2·4H2O, respectively, and ultrasonically disperse for 2 h to prepare the deposition solution.
[0035] After that, use a direct current power supply to supply power at an oil bath temperature of 72°C, with a platinum sheet as the counter electrode and a titanium sheet as the anode, at a constant current density of 27 mA cm -2 The reaction was carried out for 5, 7, 10, 12, and 15 min, respectively, to grow the FeNi nanotaper on the surface of the titanium sheet. After the reaction, the titanium sheet with the grown nanotaper was immersed in deionized water for cleaning and drying to prepare the sample, and the FeNi nanotaper electrode was obtained.
[0036] Figure 4 The scanning electron microscope images of the FeNi nanotaper structure electrode under different deposition times are shown. As shown in Figure 4 When the electrodeposition time is prolonged, the FeNi nanotaper gradually grows from the original small cone to a bamboo shoot-shaped nanotaper with a larger base area.
[0037] The electrochemical performance of the FeNi nanotaper supercapacitor obtained in this example is shown in Figure 5The results show that the FeNi nanotaper structure can show good electrochemical performance when the electrodeposition time is 5-15 min. With the increase of the deposition time, the electrochemical performance of the FeNi nanotaper shows a trend of first increasing and then decreasing.
[0038] Figure 6 The filter performance test diagram of the FeNi nanotaper supercapacitor obtained in this embodiment is shown. The results show that the FeNi nanotaper supercapacitor prepared in this scheme can effectively convert the alternating signal into a smooth direct current signal for output.
[0039] Example 3
[0040] First, a 1.5 cm x 2 cm titanium sheet was ultrasonically cleaned with deionized water and ethanol for 20 min, and the cleaned titanium sheet was dried in a forced air drying oven for 1 h.
[0041] Then, take a 100 ml capacity beaker, add 50 ml deionized water, then add 10 g NiCl2·6H2O, 2.01 g H3BO3, 4.9 g NH4Cl, and 2 g FeCl2·4H2O, respectively, and ultrasonic dispersion for 2 h to prepare the deposition solution.
[0042] Then, under the oil bath temperature of 72℃, use a direct current power supply to supply power, use a platinum sheet as a counter electrode, and a titanium sheet as an anode. The FeNi nanotaper grows on the surface of the titanium sheet at a current density of 20 mA cm -2 , 23 mA cm -2 , 25 mA cm -2 , 27 mA cm -2 , and 30 mA cm -2 for 12 min. After the reaction, the titanium sheet with the grown FeNi nanotaper is immersed in deionized water for cleaning and drying to prepare a sample, and a FeNi nanotaper electrode is obtained.
[0043] Figure 7 The scanning electron microscope images of the FeNi nanotaper structure electrodes under different deposition current densities are shown. As shown in Figure 7 , the angles of the three FeNi nanotapers are 44°, 36°, and 22°, respectively. With the increase of the current density, the nanotaper tip shows a trend of increasing sharpness and curvature.
[0044] The electrochemical performance of the FeNi nanotaper supercapacitor obtained in this embodiment is shown in Figure 8 . The results show that the nanotaper structure supercapacitor can show good electrochemical performance when the electrodeposition current density is 20-30 mA cm -2 . With the increase of the reaction time, the electrochemical performance of the FeNi nanotaper supercapacitor shows a trend of first increasing and then decreasing.
[0045] Figure 9 The FeNi nanotaper supercapacitor prepared in this embodiment was tested for filter performance. The results show that the FeNi nanotaper supercapacitor prepared by the present scheme can effectively convert alternating current signals into smooth direct current signals for output.
[0046] Note: The specific embodiments of the present application are described above. It should be understood that the present application is not limited to the above specific embodiments, and various modifications or changes can be made by those skilled in the art within the scope of the claims, which does not affect the essential content of the present application.
Claims
1. The morphology of FeNi nanocones was controlled by adjusting electrodeposition parameters. The feasibility of using FeNi nanocone structures for AC filtering was analyzed, and their filtering performance was tested and analyzed. The specific steps included: 1) Preparation of FeNi nanocone structure electrode deposition solution: Prepare a cleaning solution by mixing acetone, isopropanol, and water in a certain proportion, and ultrasonically clean the titanium sheet. After cleaning, dry it in an oven for later use. Take 50 ml of deionized water, add 10 g NiCl2·6H2O, 2.01 g H3BO3, 4.9 g NH4Cl, and 2 g FeCl2·4H2O, and ultrasonically disperse for 2 h to prepare the deposition solution. 2) FeNi nanocone structure electrodes were prepared on titanium sheets by electrodeposition: a two-electrode system was used in an oil bath environment, powered by a DC power supply, with a platinum sheet as the counter electrode and a titanium sheet as the anode. FeNi nanocones were grown on the surface of the titanium sheet under a constant current density. After the reaction, the titanium sheet with FeNi nanocones was immersed in deionized water for cleaning, dried and sampled to obtain the FeNi nanocone structure. 3) Using the prepared electrodes as the positive and negative counter electrodes, a diaphragm is added in the middle, electrolyte is injected and the plates are pressed and encapsulated to obtain FeNi nanocone supercapacitors.
2. The FeNi nanocone surface morphology control and its application in supercapacitor filtering as described in claim 1, characterized in that, The cleaning solution is prepared with acetone, isopropanol and water in a ratio of 1:1:1, and the ultrasonic cleaning time is 10-20 minutes.
3. The FeNi nanocone surface morphology control and its application in supercapacitor filtering as described in claim 1, characterized in that, The oil bath temperature during the FeNi nanocone electrodeposition stage is 65-80℃.
4. The FeNi nanocone surface morphology control and its application in supercapacitor filtering as described in claim 1, characterized in that, The deposition time for the FeNi nanocone electrodeposition stage is 5-15 min.
5. The FeNi nanocone surface morphology control and its application in supercapacitor filtering as described in claim 1, characterized in that, The deposition current density during the FeNi nanocone electrodeposition stage is 20-30 mA / cm². -2 .
6. The FeNi nanocone surface morphology control and its application in supercapacitor filtering as described in claim 1, characterized in that, The diaphragm is made of glass fiber and has a thickness of 675 μm.
7. The FeNi nanocone surface morphology control and its application in supercapacitor filtering as described in claim 1, characterized in that, The injected electrolyte is 1M Na2SO4.