CN109904004B - Preparation method of SiC nanowire array film and application of SiC nanowire array film in supercapacitor electrode - Google Patents
Preparation method of SiC nanowire array film and application of SiC nanowire array film in supercapacitor electrode Download PDFInfo
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Abstract
The invention relates to a preparation method of a SiC nanowire array film and application of the SiC nanowire array film in a super capacitor electrode, belonging to the technical field of micro-energy manufacturing, wherein the preparation method comprises the following steps: cutting a SiC wafer into SiC chips, and then cleaning, soaking and drying the SiC chips; taking the dried SiC wafer as an anode, contacting the C surface of the SiC wafer with an electrode clamp, immersing the SiC wafer into etching liquid for etching treatment, and taking out the SiC wafer; and contacting the back surface of the C surface of the SiC wafer with the electrode clamp, and immersing the electrode clamp into etching liquid again for stripping treatment to obtain the SiC nanowire array film. The preparation method of the SiC nanowire array film has the advantages of simple process method, good repeatability, simple stripping method, complete stripped SiC nanowire array film and high success rate.
Description
Technical Field
The invention relates to a preparation method of a SiC nanowire array film and application of the SiC nanowire array film in a super capacitor electrode, and belongs to the technical field of micro-energy manufacturing.
Background
In recent years, the technological trend of the development of miniature and portable electronic devices has increased the need for miniature energy storage devices. Small-sized energy systems are crucial for the development of future maintenance-free implantable biosensors, remote and mobile environmental sensors, nano-robots, micro-electromechanical systems (MEMS), and portable and wearable personal electronics. Currently, self-powered micro devices rely primarily on small batteries to provide the required power, and micro batteries such as thin film batteries are rapidly expanding in commercialization and marketization. However, such miniature batteries have the same limitations as large batteries, i.e., limited life and low power consumption. In contrast to battery devices, supercapacitors are not limited by the kinetics of electrochemical charge transfer in batteries, and store charge only at the electrode-electrode interface of the active material by rapid reversible adsorption/desorption of ions. Therefore, the power density is high (10kW/kg), the charging and discharging time is short (several seconds), and the cycle life is long (more than million times).
Silicon carbide (SiC) has a wider band gap and higher electron mobility, has a remarkable application prospect in the field of electrons and sensors, is rapidly called an electrode material with a development prospect due to excellent electrochemical performance, high specific surface area and good compatibility with various electrolytes, and more SiC nano structures are applied to electrodes of super capacitors. Yang et al demonstrate that the nanocrystalline 3C-SiC film synthesized by the microwave plasma chemical vapor deposition technology has application potential as an energy storage electrode material. Alper et al prepared SiC-coated Si nanowire micro supercapacitor electrodes by low-pressure chemical vapor deposition method, and the capacitance value of the electrodes can reach 1.7mF/cm2The performance is kept stable in 1000 charge-discharge cycles. However, the SiC nanostructure electrode prepared at present has a bottleneck problem in the aspect of device miniaturization. In order to ensure the support of the electrode, a current collector with a certain thickness needs to be additionally arranged, so that the thickness of the electrode consisting of the active material and the current collector is remarkably increased, and the miniaturization development of the energy storage device is severely restricted. Therefore, the development of an integrated SiC thin film electrode with high performance becomes a scientific problem to be solved urgently at present.
To improve the photoelectric conversion performance of the thin-film electrode, publication No. 103579404a discloses a Si nanowire thin-film battery and a method for manufacturing the same, in which a Si nanowire layer is formed on a substrate, and a silicon thin film, a doped silicon thin film, and a transparent conductive film are used in cooperation, so that radial collection of carriers is truly achieved, and a Si nanowire thin-film battery with high conversion efficiency is obtained. However, it is still necessary to further study how to further improve the specific capacitance and the cycling stability of the SiC thin film electrode.
Disclosure of Invention
Aiming at the existing problems, the invention provides the SiC nanowire array film and the preparation method thereof, and the SiC nanowire array film is applied to the electrode material of the super capacitor, and the electrode material has good cycling stability and high specific capacitance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a SiC nanowire array film comprises the following steps:
cutting a SiC wafer into SiC chips, and then cleaning, soaking and drying the SiC chips;
taking the dried SiC wafer as an anode, contacting the C surface of the SiC wafer with an electrode clamp, immersing the SiC wafer into etching liquid for etching treatment, and taking out the SiC wafer;
and contacting the back surface of the C surface of the SiC wafer with the electrode clamp, and immersing the electrode clamp into etching liquid again for stripping treatment to obtain the SiC nanowire array film.
The preparation method is simple and feasible, namely, the film is obtained by peeling the C surface of the SiC wafer. On the SiC wafer, the front surface is a C surface, and the specific composition of the back surface is uncertain. In the step etching process (the essence of the stripping is also etching), the C surface is firstly contacted with the electrode clamp, so that good C surface etching can be formed, at the moment, although partial etching can also occur on the back surface, the etching effect is poor, the required etching effect cannot be obtained, and the back surface film is generally abandoned directly. Although the C surface can obtain a better film after the first etching, the C surface is not easy to strip at the moment, the surface needs to be changed for short-time etching, namely the SiC wafer is turned over, the back surface of the C surface is contacted with the electrode clamp, and a large amount of bubbles are formed at the C surface for etching for several seconds, so that the C surface is promoted to strip by utilizing the escaped bubbles, and a film product is obtained. The finally obtained SiC thin film may have differences due to parameter variations in the manufacturing process. The mass loading of the SiC film is 1.0-7.0mg/cm3。
Preferably, the SiC wafer is industrial grade. That is, the cumulative length of the scratches on the surface of the SiC wafer is less than 1 diameter, the number of the scratches is less than or equal to 3, and the density of the micropipes is less than or equal to 1/cm2。
Preferably, the cleaning is: and respectively carrying out ultrasonic cleaning on the SiC wafer in acetone and deionized water for 10-20 min.
Preferably, the soaking is carried out in an ethanol solution of hydrofluoric acid, and the soaking time is 100-140s, wherein the volume ratio of the hydrofluoric acid to the ethanol is 0.8-1.2: 1. The silicon carbide wafer can be fully cleaned by selecting a proper cleaning reagent and a proper soaking time, so that impurities are prevented from being mixed.
Preferably, the drying is to dry the SiC wafer in an oven at 35-45 ℃ for 8-12 min.
Preferably, the cathode material is a carbon plate.
Preferably, the etching liquid comprises hydrofluoric acid, ethanol and hydrogen peroxide in a volume ratio of 2.5-3.5:6: 1.
Preferably, the volume ratio of the hydrofluoric acid to the ethanol to the hydrogen peroxide in the etching solution is 3:6: 1.
Preferably, the etching treatment time is 10-15min, and the stripping treatment time is 1-5 s.
Preferably, the etching treatment and the stripping treatment are carried out under the same treatment conditions, and both adopt a pulse power supply constant current mode, and the current density is 130mA/cm2. In the etching process, the morphology of the SiC wafer can be regulated and controlled by controlling the etching time, the morphology of the film can be monitored by the SEM technology, and finally the SiC film with the required morphology is accurately obtained.
Preferably, the peeling treatment is a surface-changing peeling method.
Preferably, the appearance of the SiC nanowire array film is a long nanowire.
Further preferably, the long nanowires have a diameter of 18-22 nm.
Compared with the SiC nano array with single appearance prepared by the traditional method, the SiC nano array with single appearance can be better controlled in the anodic oxidation etching process, the appearance change of the SiC nano array can be changed from the nano hole to the nano wire and then to the disordered porous appearance, the length of the nano wire can be controlled, the SiC nano array with longer appearance of the nano wire needs to be selected as a product which can be practically applied, and the appearance of the short nano wire and the disordered porous appearance can cause the reduction of the performance of the product in the application process.
An application of a SiC nanowire array film in a super capacitor electrode, wherein the super capacitor electrode is the SiC nanowire array film.
When the SiC nanowire array film is actually applied to the electrode of the supercapacitor, the SiC nanowire array film can be directly used as the electrode, and the SiC nanowire array film has good self-supporting property.
Preferably, the specific capacitance of the electrode at 10mV/s is 22-25mF/cm2。
The SiC film material stripped by etching can be directly used as an electrode material of a super capacitor without adding additional auxiliary materials or carrying out process treatment such as shape change and the like, so that the structure of the super capacitor is greatly simplified, the space of the capacitor is compressed, the performance of the super capacitor used as a micro power supply is greatly improved, the super capacitor can be conveniently implanted in a smaller space or structure, and the practicability is higher.
Compared with other materials, the invention has the following advantages:
(1) the preparation method of the SiC nanowire array film is simple in process and good in repeatability.
(2) The SiC nanowire array film disclosed by the invention is simple in stripping method, the stripped SiC nanowire array film is complete, and the success rate is high.
(3) According to the invention, the control of the mass load of the SiC nanowire array thin film electrode can be further realized through the etching time.
(4) The SiC nanowire array film electrode can be applied to a super capacitor electrode and has higher specific capacitance and rate capability.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of SiC nanowire array films with different mass loads prepared by the present invention;
FIG. 2 is an X-ray diffraction (XRD) pattern of the SiC nanowire array film prepared in example 1 of the present invention;
FIG. 3 is an Electron Diffraction Spectroscopy (EDS) chart of the SiC nanowire array film prepared in example 1 of the present invention;
FIG. 4 is a Cyclic Voltammetry (CV) curve of SiC nanowire array thin film electrodes with different mass loads prepared by the present invention;
FIG. 5 is a curve of the relationship between the specific capacitance and the mass load of SiC nanowire array thin-film electrodes with different mass loads, which are manufactured by the present invention;
FIG. 6 shows that the mass loading of 5.6mg/cm is obtained by the present invention2Sodium SiCLow power Scanning Electron Microscope (SEM) images of the nanowire array thin film electrodes;
FIG. 7 shows that the mass loading of 5.6mg/cm is obtained according to the present invention2A high power Scanning Electron Microscope (SEM) image of the SiC nanowire array thin film electrode;
FIG. 8 shows that the mass loading of 5.6mg/cm is obtained according to the present invention2Cyclic Voltammetry (CV) curves of the SiC nanowire array thin film electrode of (1);
FIG. 9 shows that the mass loading of 5.6mg/cm is obtained according to the present invention2The constant current charging and discharging (GCD) curve of the SiC nanowire array thin film electrode;
FIG. 10 shows that the mass loading of 5.6mg/cm is obtained according to the present invention2The specific capacitance of the SiC nanowire array thin film electrode is in a relation curve with the current density.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
Example 1
Cutting an industrial grade SiC wafer into a size of 0.7 × 1.5.5 cm2Respectively carrying out ultrasonic cleaning on the SiC wafer in acetone and deionized water for 15min, then immersing the SiC wafer in a mixed solution of hydrofluoric acid and ethanol with the volume ratio of 1:1 for 120s, taking out the SiC wafer, and drying the SiC wafer in a drying oven at 40 ℃ for 10 min;
immersing the dried SiC wafer serving as an anode, a C surface of the SiC wafer contacting an electrode holder and a carbon plate serving as a cathode into an etching solution mixed by hydrofluoric acid, ethanol and hydrogen peroxide in a volume ratio of 3:6:1, wherein the current density is 130mA/cm2Etching for 13min under the pulse current, and taking out;
contacting the back surface of the SiC wafer with an electrode clamp, and immersing the electrode clamp into the etching solution again at a current density of 130mA/cm2Stripping for 10s under the pulse current to obtain the SiC nanowire array film.
Example 2
Cutting an industrial grade SiC wafer into a size of 0.7 × 1.5.5 cm2Respectively carrying out ultrasonic cleaning on the SiC wafer in acetone and deionized water for 15min, and then immersing the SiC wafer in the deionized water according to the volume ratio1:1, taking out the SiC wafer from the mixed solution of hydrofluoric acid and ethanol for 120s, and drying the SiC wafer in a drying oven at 40 ℃ for 10 min;
immersing the dried SiC wafer serving as an anode, a C surface of the SiC wafer contacting an electrode holder and a carbon plate serving as a cathode in an etching solution mixed by hydrofluoric acid, ethanol and hydrogen peroxide in a volume ratio of 2.5:6:1 at a current density of 120mA/cm2Etching for 10min under the pulse current, and taking out;
contacting the back of the SiC wafer with an electrode clamp, and immersing the electrode clamp into the etching solution again at a current density of 120mA/cm2Stripping for 10s under the pulse current to obtain the SiC nanowire array film.
Example 3
Cutting an industrial grade SiC wafer into a size of 0.7 × 1.5.5 cm2Respectively carrying out ultrasonic cleaning on the SiC wafer in acetone and deionized water for 15min, then immersing the SiC wafer in a mixed solution of hydrofluoric acid and ethanol with the volume ratio of 1:1 for 120s, taking out the SiC wafer, and drying the SiC wafer in a drying oven at 40 ℃ for 10 min;
immersing the dried SiC wafer serving as an anode, a C surface of the SiC wafer contacting an electrode holder and a carbon plate serving as a cathode in an etching solution mixed by hydrofluoric acid, ethanol and hydrogen peroxide in a volume ratio of 3.5:6:1 at a current density of 140mA/cm2Etching for 15min under the pulse current, and taking out;
contacting the back surface of the SiC wafer with an electrode clamp, and immersing the electrode clamp into the etching solution again at a current density of 140mA/cm2Stripping for 10s under the pulse current to obtain the SiC nanowire array film.
Example 4
Cutting an industrial grade SiC wafer into a size of 0.7 × 1.5.5 cm2Respectively carrying out ultrasonic cleaning on the SiC wafer in acetone and deionized water for 15min, then immersing the SiC wafer in a mixed solution of hydrofluoric acid and ethanol with the volume ratio of 1:1 for 120s, taking out the SiC wafer, and drying the SiC wafer in a drying oven at 40 ℃ for 10 min;
immersing the dried SiC wafer serving as an anode, a C surface of the SiC wafer contacting an electrode holder and a carbon plate serving as a cathode into an etching solution mixed by hydrofluoric acid, ethanol and hydrogen peroxide in a volume ratio of 3:6:1 at a current densityIs 100mAcm-2Etching for 13min under the pulse current, and taking out;
contacting the back surface of the SiC wafer with an electrode holder, and immersing the electrode holder into the etching solution again at a current density of 100mA/cm2Stripping for 10s under the pulse current to obtain the SiC nanowire array film.
Example 5
Cutting an industrial grade SiC wafer into a size of 0.7 × 1.5.5 cm2Respectively carrying out ultrasonic cleaning on the SiC wafer in acetone and deionized water for 15min, then immersing the SiC wafer in a mixed solution of hydrofluoric acid and ethanol with the volume ratio of 1:1 for 120s, taking out the SiC wafer, and drying the SiC wafer in a drying oven at 40 ℃ for 10 min;
immersing the dried SiC wafer serving as an anode, a C surface of the SiC wafer contacting an electrode holder and a carbon plate serving as a cathode into an etching solution mixed by hydrofluoric acid, ethanol and hydrogen peroxide in a volume ratio of 3:6:1, wherein the current density is 130mA/cm2Etching for 13min under the pulse current, and taking out;
the back surface of the C surface of the SiC wafer was brought into contact with the electrode holder and immersed again in an etching solution at a current density of 130mA/cm2Stripping for 15s under the pulse current to obtain the SiC nanowire array film.
Example 6
The only difference from example 1 is that example 6 employs only the ethanol soaking treatment.
Example 7
The difference from the embodiment 1 is only that the etching solution of the embodiment 7 is composed of ethanol and hydrofluoric acid in a volume ratio of 1: 2.
Example 8
The difference from the embodiment 1 is only that the etching solution of the embodiment 8 is composed of hydrofluoric acid and hydrogen peroxide in a volume ratio of 6: 1.
Example 9
The only difference from example 1 is that the etching treatment time of example 9 was 9 min.
Example 10
The only difference from example 1 is that the etching treatment time of example 10 was 16 min.
Example 11
The only difference from example 1 is that the time for the stripping treatment in example 11 was 0.5 s.
Example 12
The only difference from example 1 is that the time for the stripping treatment in example 12 was 18 seconds.
Comparative example 1
The only difference from example 1 is that the morphology of the SiC thin film of comparative example 1 is nanoporous.
Comparative example 2
The only difference from example 1 is that the morphology of the SiC thin film of comparative example 2 is short nanowires.
Comparative example 3
The only difference from example 1 is that the morphology of the SiC film of comparative example 3 is a disordered nanotopography.
The SiC films obtained in examples 1 to 12 and comparative examples 1 to 3 were used as electrodes of a supercapacitor, performance tests were performed in a three-electrode system with an Ag/AgCl electrode as a reference electrode, a platinum sheet electrode as a counter electrode, and a 2MKCl solution as an electrolyte, and specific capacitance, rate capability, and cycle stability were tested, and the results are shown in table 1:
table 1: performance of SiC films obtained in examples 1 to 12 and comparative examples 1 to 3 as electrodes
| Specific capacitance (mF/cm)2) | Rate capability | Stability of circulation | |
| Example 1 | 22.1 | 48.8％ | 95.5％ |
| Example 2 | 18.4 | 47.5％ | 94.8％ |
| Example 3 | 21.0 | 50.4％ | 96.7％ |
| Example 4 | 11.9 | 50.1％ | 95.4％ |
| Example 5 | 23.6 | 62.3％ | 96.5％ |
| Example 6 | / | / | / |
| Example 7 | / | / | / |
| Example 8 | / | / | / |
| Example 9 | 14.7 | 49.6％ | 95.3％ |
| Example 10 | 19.3 | 50.2％ | 96.2％ |
| Example 11 | / | / | / |
| Example 12 | 23.6 | 62.3％ | 94.9％ |
| Comparative example 1 | 14.4 | 40.0％ | 80.6％ |
| Comparative example 2 | 16.3 | 42.4％ | 85.4％ |
| Comparative example 3 | 20.7 | 58.4％ | 90.9％ |
Among them, examples 6, 7 and 8 hardly undergo etching reaction, and example 11 has too short peeling time to peel off a SiC nanowire film, and thus electrochemical tests cannot be performed.
FIG. 1 is a microscopic topography of a thin film obtained according to different etching times, the transverse direction is comparison of the same etching time and different magnifications, and the longitudinal direction (from top to bottom) is the topography change of the sample along with the increase of the etching time, namely the change from a nanopore, a middle topography, a short nanowire, a long nanowire to a disordered porous topography;
FIG. 2 is an XRD pattern of the SiC film of example 1, showing that the phase composition of the film is 4H-SiC and has high crystallinity;
fig. 3 is an EDS spectrum of the SiC thin film in example 1, and it is found that the ratio of Si element to C element is close to 1:1, indicating that the etched sample is still SiC;
FIG. 4 is a Cyclic Voltammetry (CV) curve for SiC thin film electrodes of different mass loading, all CV curves being close to rectangular, indicating that the SiC thin film electrode has double layer capacitance characteristics;
FIG. 5 is a graph showing the relationship between the specific capacitance and the sweep rate of SiC thin film electrodes with different mass loadings, and it can be seen that the specific capacitance is 5.6mg/cm at the same sweep rate2The SiC thin film electrode has higher specific capacitance;
FIGS. 6 and 7 show the mass loading of 5.6mg/cm2The SEM image of the SiC film sample shows that the microscopic appearance of the SiC film is a SiC nanowire array, and the diameter of the SiC film is about 20 nm;
FIG. 8 is a mass loading of 5.6mg/cm2The CV curve of the SiC nanowire array thin-film electrode under different scanning speeds is calculated, and the specific capacitance of the thin-film electrode under the scanning speed of 10mV/s can reach 23.6mF/cm2；
FIG. 9 shows a mass loading of 5.6mg/cm2The SiC nanowire array thin film electrode has the current density of 0.3mA/cm2Increased to 2.4mA/cm2The corresponding constant current charging and discharging (GCD) curve does not have obvious IR drop, and the curve symmetry is good, which shows that the thin film electrode has small internal resistance and high coulombic efficiency;
fig. 10 is a graph of the relationship between the specific capacitance and the current density calculated from the constant current charge/discharge curve of fig. 9, and it is understood that the electrode has a good rate capability.
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
Claims (4)
1. A preparation method of a SiC nanowire array film is characterized by comprising the following steps:
cutting a SiC wafer into SiC chips, and then cleaning, soaking and drying the SiC chips;
taking the dried SiC wafer as an anode, contacting the C surface of the SiC wafer with an electrode clamp, immersing the SiC wafer into etching liquid for etching treatment, and taking out the SiC wafer after the etching treatment for 10-15 min;
the back side of the C surface of the SiC wafer is contacted with an electrode clamp and is immersed into etching liquid again for stripping treatment to obtain the SiC nanowire array film, the stripping treatment method is a face-changing stripping method, the stripping treatment time is 1-15s, the film is in the shape of long nanowires, the diameter of the long nanowires is 18-22nm, the etching treatment and the stripping treatment are carried out under the same treatment conditions, a pulse power supply constant current mode is adopted, the current density is 130mA/cm2The etching liquid comprises ethanol, hydrofluoric acid and hydrogen peroxide in a volume ratio of 2.5-3.5:6: 1.
2. The method for preparing the SiC nanowire array film as claimed in claim 1, wherein the soaking is performed in an ethanol solution of hydrofluoric acid for 100-140s, wherein the volume ratio of hydrofluoric acid to ethanol is 0.8-1.2: 1.
3. An application of the SiC nanowire array film in a supercapacitor electrode, which is characterized in that the supercapacitor electrode is the SiC nanowire array film prepared by the preparation method of the SiC nanowire array film in claim 1.
4. Use of the SiC nanowire array film of claim 3 in supercapacitor electrodes, wherein the electrodes are at 10mVs-1The specific capacitance of the lower electrode is 22-25mFcm-2。
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