CN109904004A - A kind of preparation method of SiC nano-array film and its application in supercapacitor electrode - Google Patents
A kind of preparation method of SiC nano-array film and its application in supercapacitor electrode Download PDFInfo
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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Abstract
本发明涉及一种SiC纳米阵列薄膜的制备方法及其在超级电容器电极中的应用，属于微能源制造技术领域，制备方法包括：将SiC晶圆先切割成SiC晶片，再经清洗、浸泡、干燥处理；将干燥后的SiC晶片作为阳极，SiC晶片的C面接触电极夹，浸入刻蚀液中进行刻蚀处理后取出；将SiC晶片C面的背面接触电极夹，再次浸入刻蚀液中进行剥离处理得SiC纳米线阵列薄膜。本发明SiC纳米线阵列薄膜制备方法，工艺方法简单，具有很好的重复性，且剥离方法简单，剥离的SiC纳米线阵列薄膜完整，成功率高。
The invention relates to a preparation method of a SiC nano-array film and its application in supercapacitor electrodes, belonging to the technical field of micro-energy manufacturing. Treatment; using the dried SiC wafer as the anode, the C surface of the SiC wafer contacts the electrode clip, immersed in the etching solution for etching treatment and then taken out; the back of the C surface of the SiC wafer contacts the electrode clip, and is immersed in the etching solution again to carry out The SiC nanowire array film was obtained by peeling. The preparation method of the SiC nanowire array film of the invention has the advantages of simple process method, good repeatability, simple peeling method, complete peeling of the SiC nanowire array film, and high success rate.
Description
Technical field
The present invention relates to a kind of preparation method of SiC nano-array film and its application in electrode of super capacitor,
Belong to micro- technical field of energy production.
Background technique
In recent years, the technological trend of miniature and portable electronic device development is increased to micro power source storage device
It needs.The energy resource system of the small size implantating biological sensors non-maintaining for future, are received long-range and mobile environment sensor
The development of rice robot, MEMS (MEMS) and portable and wearable personal electric product is most important.Currently, from
Power supply micromodule equipment relies primarily on the electric power needed for compact battery provides, and the commercialization of the micro cells such as hull cell and the marketization are presented
Rapid Expansion.However, this kind of minicell and large-sized battery have an identical limitation, i.e. restricted lifetime, low in energy consumption.With battery
Device is compared, and supercapacitor is not limited by battery electrochemical charge-transfer dynamics, is inhaled by the Rapid reversible to ion
Attached/desorption, only stores a charge in the electrode-electric pole interface of active material.Thus there is power density high (10kW/kg), fill
Discharge time short (several seconds), have extended cycle life the unique advantage of (million times or more).
Silicon carbide (SiC) has wider band gap and higher electron mobility, has in electronics and sensor field aobvious
Application prospect is write, and since its electrochemical performance, specific surface area are high, good with the compatibility of various electrolyte, is known as rapidly
A kind of electrode material of great development prospect, more and more SiC nanostructures are applied in electrode of super capacitor.Yang
Et al. demonstrate the synthesis of microwave plasma CVD technology nanocrystalline 3C-SiC film have as energy storage electrode
The application potential of material.Alper et al. is prepared for SiC coated Si nano wire microsuper electricity using Low Pressure Chemical Vapor Deposition
Container electrode, capacitance is up to 1.7mF/cm2, retention property is stablized in 1000 charging-discharging cycles.However preparation at present
SiC nano structure electrode there are bottleneck problems in terms of device miniaturization.For the supportive for guaranteeing electrode, need additional certain
The collector of thickness, therefore significantly increased by the thickness of electrode that active material and collector form, seriously constrain its accumulator
The miniaturization of part.Therefore section's knowledge that integration SiC membrane electrode with high performance becomes urgently to be resolved at present is developed
Topic.
For the photoelectric conversion performance for promoting membrane electrode, publication number 103579404A discloses a kind of Si nano wire film electricity
Pond and preparation method thereof by the way that Si nano wire layer is formed on the substrate, and cooperates silicon thin film, doping type silicon thin film and transparent leads
Electrolemma is truly realized the radial of carrier and collects, obtains the Si nano wire film battery with higher conversion efficiency.But
It is that the specific capacitance and cyclical stability for how further increasing SiC membrane electrode still need to continue deeper into research.
Summary of the invention
In view of the above problems, the present invention provides a kind of SiC nano-array film and preparation method thereof, and is applied to
Electrode material for super capacitor, good cycling stability, the specific capacitance of the electrode material are high.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of preparation method of SiC nano-array film, described method includes following steps:
SiC wafer is first cut into SiC wafer, then cleaned, immersion, drying process；
Using the SiC wafer after drying as anode, the C face contact electrode holder of SiC wafer is immersed in etching liquid and is performed etching
It is taken out after processing；
By the rear-face contact electrode holder in the face SiC wafer C, it is again dipped into progress lift-off processing in etching liquid and obtains SiC nanowire
Array film.
Of the invention preparation method is simple, i.e., obtains film eventually by the face C of removing SiC wafer.In SiC crystalline substance
On piece, front are the face C, and the specific ingredient in the back side is uncertain.During step etching (essence of removing is also etching), first will
The face C is contacted with electrode holder, the good face C etching can be formed, although partial etching, etching effect can also occur for the back side at this time
It is poor, required etching effect cannot be obtained, back film generally can be directly given up.Although the face C energy after first time etches
Preferable film is obtained, but is not easy to be removed at this time, needs to change face and is etched in short-term, i.e., overturn SiC wafer, by the face C
The back side contacted with electrode holder, etch the several seconds, will form a large amount of bubbles at the face C at this time, and then promote the face C using the bubble of evolution
It is peeling-off, obtain film product.The SiC film that finally obtains can be because of Parameters variation in preparation process and difference.
The mass loading amount of SiC film is 1.0-7.0mg/cm3。
Preferably, the SiC wafer is technical grade.That is 1 diameter of SiC wafer surface scratch cumulative length <, and it is a
Number≤3, micropipe density≤1/cm2。
Preferably, the cleaning are as follows: SiC wafer is carried out ultrasonic cleaning 10- in acetone, deionized water respectively
20min。
Preferably, described be immersed in the ethanol solution of hydrofluoric acid carries out, soaking time 100-140s, wherein hydrogen fluorine
The volume ratio of acid and ethyl alcohol is 0.8-1.2:1.Carbon can sufficiently be cleaned by choosing suitable cleaning reagent and suitable soaking time
SiClx chip avoids being mixed into impurity.
Preferably, the drying is that SiC wafer is placed in in 35-45 DEG C of baking oven dry 8-12min.
Preferably, cathode material is carbon plate.
Preferably, the ingredient of the etching liquid includes hydrofluoric acid, ethyl alcohol, hydrogen peroxide, volume ratio 2.5-3.5:6:1.
Further preferably, in the etching liquid, hydrofluoric acid, ethyl alcohol, hydrogen peroxide volume ratio be 3:6:1.
Preferably, the time of the etching processing is 10-15min, the time of lift-off processing is 1-5s.
Preferably, etching processing is identical as the treatment conditions of lift-off processing, it is all made of pulse power constant current mode, electric current
Density is 130mA/cm2.In etching process, the pattern of SiC wafer can be regulated and controled by control etch period, film morphology can lead to
It crosses SEM technology to be monitored, the final accurate SiC film for obtaining required pattern.
Preferably, the method for the lift-off processing is to change face stripping method.
Preferably, the pattern of the SiC nano-array film is long nano wire.
Further preferably, the diameter of the long nano wire is 18-22nm.
It is different from the SiC nano-array of the single shape of conventional method preparation, anodic oxidation etching process of the invention can
Preferably to control the pattern variation of SiC nano-array, nano wire can be transitioned into from nano-pore again to unordered porous pattern, and receive
Rice noodles length is controllable, and the present invention needs to select has the SiC nano-array of longer nano wire pattern as can practical application
Product, short nano wire pattern and unordered porous pattern will cause the decline of performance during products application.
A kind of application of SiC nanowire array film in electrode of super capacitor, the electrode of super capacitor are SiC
Nano-wire array film.
The present invention can directly make when SiC nanowire array film to be applied to the electrode in supercapacitor
It is used for electrode, because SiC nanowire array film has preferable self-supporting.
Preferably, specific capacitance of the electrode at 10mV/s is 22-25mF/cm2。
The SiC thin-film material that is stripped out of present invention etching can directly as the electrode material of supercapacitor, without
It needs to add additional auxiliary material or carries out the process such as change in shape, greatly simplifie the composition of supercapacitor,
And the space of capacitor is had compressed, there is significant increase to the performance of the supercapacitor as micro battery, convenient in lesser sky
Between or structure in be implanted into, practicability with higher.
Compared with other materials, the present invention has the advantage that
(1) SiC nanowire array film preparation method of the present invention, process is simple, has repeatability well.
(2) SiC nanowire array film of the present invention, stripping means is simple, and the SiC nanowire array film of removing is complete,
Success rate is high.
(3) present invention can further realize the control of SiC nanowire array film electrode mass loading by etch period
System.
(4) SiC nanowire array film electrode of the present invention can be applied to electrode of super capacitor, specific capacitance with higher
And high rate performance.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) figure that different quality produced by the present invention loads SiC nanowire array film；
Fig. 2 is X-ray diffraction (XRD) figure of SiC nanowire array film obtained by the embodiment of the present invention 1；
Fig. 3 is electronic diffraction power spectrum (EDS) figure of SiC nanowire array film obtained by the embodiment of the present invention 1；
Fig. 4 is that the cyclic voltammetric (CV) of the SiC nanowire array film electrode of different quality produced by the present invention load is bent
Line；
Fig. 5 is that the specific capacitance of the SiC nanowire array film electrode of different quality produced by the present invention load and quality are born
Carry relation curve；
Fig. 6 is that mass loading produced by the present invention is 5.6mg/cm2SiC nanowire array film electrode low power scanning
Electronic Speculum (SEM) figure；
Fig. 7 is that mass loading produced by the present invention is 5.6mg/cm2SiC nanowire array film electrode high power scanning
Electronic Speculum (SEM) figure；
Fig. 8 is that mass loading produced by the present invention is 5.6mg/cm2SiC nanowire array film electrode cyclic voltammetric
(CV) curve；
Fig. 9 is that mass loading produced by the present invention is 5.6mg/cm2SiC nanowire array film electrode constant current charge and discharge
Electric (GCD) curve；
Figure 10 is that mass loading produced by the present invention is 5.6mg/cm2SiC nanowire array film electrode specific capacitance
With the relation curve of current density.
Specific embodiment
The following is specific embodiments of the present invention, and is described with reference to the drawings and further retouches to technical solution of the present invention work
It states, however, the present invention is not limited to these examples.
Embodiment 1
Technical grade SiC wafer is first cut into having a size of 0.7 × 1.5cm2SiC wafer, respectively in acetone, deionized water
In carry out ultrasonic cleaning 15min, then immerse 120s in the mixed solution that volume ratio is the hydrofluoric acid of 1:1, ethyl alcohol, will after taking-up
SiC wafer is placed in 40 DEG C of baking oven dry 10min；
Using the SiC wafer after drying as anode, the C face contact electrode holder of SiC wafer, carbon plate as cathode, immerse by
It is 130mA/cm in current density in the etching liquid for hydrofluoric acid, ethyl alcohol, the hydrogen peroxide mixing that volume ratio is 3:6:12Pulse electricity
It is taken out after flowing down etching processing 13min；
It is again dipped into SiC wafer rear-face contact electrode holder in etching liquid, is 130mA/cm in current density2Pulse
Lift-off processing 10s under electric current obtains SiC nanowire array film.
Embodiment 2
Technical grade SiC wafer is first cut into having a size of 0.7 × 1.5cm2SiC wafer, respectively in acetone, deionized water
In carry out ultrasonic cleaning 15min, then immerse 120s in the mixed solution that volume ratio is the hydrofluoric acid of 1:1, ethyl alcohol, will after taking-up
SiC wafer is placed in 40 DEG C of baking oven dry 10min；
Using the SiC wafer after drying as anode, the C face contact electrode holder of SiC wafer, carbon plate as cathode, immerse by
It is 120mA/cm in current density in the etching liquid for hydrofluoric acid, ethyl alcohol, the hydrogen peroxide mixing that volume ratio is 2.5:6:12Pulse
It is taken out after etching processing 10min under electric current；
It is again dipped into SiC wafer rear-face contact electrode holder in etching liquid, is 120mA/cm in current density2Pulse
Lift-off processing 10s under electric current obtains SiC nanowire array film.
Embodiment 3
Technical grade SiC wafer is first cut into having a size of 0.7 × 1.5cm2SiC wafer, respectively in acetone, deionized water
In carry out ultrasonic cleaning 15min, then immerse 120s in the mixed solution that volume ratio is the hydrofluoric acid of 1:1, ethyl alcohol, will after taking-up
SiC wafer is placed in 40 DEG C of baking oven dry 10min；
Using the SiC wafer after drying as anode, the C face contact electrode holder of SiC wafer, carbon plate as cathode, immerse by
It is 140mA/cm in current density in the etching liquid for hydrofluoric acid, ethyl alcohol, the hydrogen peroxide mixing that volume ratio is 3.5:6:12Pulse
It is taken out after etching processing 15min under electric current；
It is again dipped into SiC wafer rear-face contact electrode holder in etching liquid, is 140mA/cm in current density2Pulse
Lift-off processing 10s under electric current obtains SiC nanowire array film.
Embodiment 4
Technical grade SiC wafer is first cut into having a size of 0.7 × 1.5cm2SiC wafer, respectively in acetone, deionized water
In carry out ultrasonic cleaning 15min, then immerse 120s in the mixed solution that volume ratio is the hydrofluoric acid of 1:1, ethyl alcohol, will after taking-up
SiC wafer is placed in 40 DEG C of baking oven dry 10min；
Using the SiC wafer after drying as anode, the C face contact electrode holder of SiC wafer, carbon plate as cathode, immerse by
It is 100mAcm in current density in the etching liquid for hydrofluoric acid, ethyl alcohol, the hydrogen peroxide mixing that volume ratio is 3:6:1-2Pulse electricity
It is taken out after flowing down etching processing 13min；
It is again dipped into SiC wafer rear-face contact electrode holder in etching liquid, is 100mA/cm in current density2Pulse
Lift-off processing 10s under electric current obtains SiC nanowire array film.
Embodiment 5
Technical grade SiC wafer is first cut into having a size of 0.7 × 1.5cm2SiC wafer, respectively in acetone, deionized water
In carry out ultrasonic cleaning 15min, then immerse 120s in the mixed solution that volume ratio is the hydrofluoric acid of 1:1, ethyl alcohol, will after taking-up
SiC wafer is placed in 40 DEG C of baking oven dry 10min；
Using the SiC wafer after drying as anode, the C face contact electrode holder of SiC wafer, carbon plate as cathode, immerse by
It is 130mA/cm in current density in the etching liquid for hydrofluoric acid, ethyl alcohol, the hydrogen peroxide mixing that volume ratio is 3:6:12Pulse electricity
It is taken out after flowing down etching processing 13min；
It is again dipped into the rear-face contact electrode holder in the face SiC wafer C in etching liquid, is 130mA/cm in current density2's
Lift-off processing 15s under pulse current obtains SiC nanowire array film.
Embodiment 6
Difference with embodiment 1 is only that embodiment 6 is only with ethyl alcohol immersion treatment.
Embodiment 7
Difference with embodiment 1 is only that the etching liquid of embodiment 7 is the ethyl alcohol of volume ratio 1:2, hydrofluoric acid composition.
Embodiment 8
Difference with embodiment 1 is only that the etching liquid of embodiment 8 is the hydrofluoric acid of volume ratio 6:1, hydrogen peroxide composition.
Embodiment 9
Difference with embodiment 1 is only that the time of the etching processing of embodiment 9 is 9min.
Embodiment 10
Difference with embodiment 1 is only that the time of the etching processing of embodiment 10 is 16min.
Embodiment 11
Difference with embodiment 1 is only that the time of the lift-off processing of embodiment 11 is 0.5s.
Embodiment 12
Difference with embodiment 1 is only that the time of the lift-off processing of embodiment 12 is 18s.
Comparative example 1
Difference with embodiment 1 is only that the pattern of the SiC film of comparative example 1 is nano-pore.
Comparative example 2
Difference with embodiment 1 is only that the pattern of the SiC film of comparative example 2 is short nano wire.
Comparative example 3
Difference with embodiment 1 is only that the pattern of the SiC film of comparative example 3 is unordered nanotopography.
The SiC film that embodiment 1-12, comparative example 1-3 are obtained is as the electrode of supercapacitor, in three-electrode system
Under, using Ag/AgCl electrode as reference electrode, platinum plate electrode is to electrode, and 2MKCl solution is electrolyte, is tested for the property, and is surveyed
Its specific capacitance, high rate performance, cyclical stability are tried, the results are shown in Table 1:
Table 1: the performance when SiC film that embodiment 1-12, comparative example 1-3 are obtained is as electrode
| Specific capacitance (mF/cm2) | High rate performance | Cyclical stability | |
| Embodiment 1 | 22.1 | 48.8% | 95.5% |
| Embodiment 2 | 18.4 | 47.5% | 94.8% |
| Embodiment 3 | 21.0 | 50.4% | 96.7% |
| Embodiment 4 | 11.9 | 50.1% | 95.4% |
| Embodiment 5 | 23.6 | 62.3% | 96.5% |
| Embodiment 6 | / | / | / |
| Embodiment 7 | / | / | / |
| Embodiment 8 | / | / | / |
| Embodiment 9 | 14.7 | 49.6% | 95.3% |
| Embodiment 10 | 19.3 | 50.2% | 96.2% |
| Embodiment 11 | / | / | / |
| Embodiment 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% |
Wherein, embodiment 6,7 and 8 is difficult that etching reaction occurs, and 11 splitting time of embodiment is too short can not to be removed to obtain SiC
Nano wire film, therefore electro-chemical test can not be carried out.
Fig. 1 is the microscopic appearance figure of the film obtained according to different etch periods, is laterally identical etch period, difference
The comparison of enlargement ratio, longitudinal (from top to bottom) be as the pattern of the increased sample of etch period changes, i.e., from nano-pore, in
Between pattern, short nano wire, long nano wire to unordered porous pattern variation；
Fig. 2 is the XRD spectrum of SiC film in embodiment 1, shows that coordinating for the film is divided into 4H-SiC, and is had higher
Crystallinity；
Fig. 3 is the EDS map of SiC film in embodiment 1, it is known that Si element and C element ratio show to etch close to 1:1
Sample afterwards is still SiC；
Fig. 4 is cyclic voltammetric (CV) curve of the SiC membrane electrode of different quality load, and all CV curves are all close to square
Shape shows that SiC membrane electrode has electric double layer capacitance characteristic；
Fig. 5 is the specific capacitance of the SiC membrane electrode of different quality load and the relational graph for sweeping speed, it is known that sweeps speed identical
Under, 5.6mg/cm2SiC membrane electrode have higher specific capacitance；
Fig. 6 and Fig. 7 is mass loading 5.6mg/cm2SiC film sample SEM figure, show the microscopic appearance of SiC film
For SiC nanowire array, diameter is about 20nm；
Fig. 8 is mass loading 5.6mg/cm2SiC nanowire array film electrode sweep CV curves under speed in difference, by
This calculates the specific capacitance of the membrane electrode in the case where 10mV/s sweeps speed up to 23.6mF/cm2；
Fig. 9 is mass loading 5.6mg/cm2SiC nanowire array film electrode in current density from 0.3mA/cm2Increase
To 2.4mA/cm2When corresponding constant current charge-discharge (GCD) curve, have no apparent IR drop, and curve symmetry is good, shows this
Membrane electrode internal resistance is smaller, and coulombic efficiency is high；
Figure 10 is the relation curve of the specific capacitance and current density that are calculated by the constant current charge-discharge curve of Fig. 9, it is known that
Electrode has good high rate performance.
It is skilled to this field although present invention has been described in detail and some specific embodiments have been cited
For technical staff, as long as it is obvious for can making various changes or correct without departing from the spirit and scope of the present invention.
Claims (9)
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