CN106206068A - A kind of preparation method of CNT composite nano cerium dioxide electrode material - Google Patents
A kind of preparation method of CNT composite nano cerium dioxide electrode material Download PDFInfo
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- CN106206068A CN106206068A CN201610801025.0A CN201610801025A CN106206068A CN 106206068 A CN106206068 A CN 106206068A CN 201610801025 A CN201610801025 A CN 201610801025A CN 106206068 A CN106206068 A CN 106206068A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- 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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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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
Abstract
The preparation method of a kind of CNT composite nano cerium dioxide electrode material of the present invention, belongs to the technical field of the nano-electrode material being applied to ultracapacitor.The present invention uses Ce (NO3)3·6H2O is as cerium source, by polyvinylpyrrolidone, it is carried out morphology control, meanwhile, the CNT of buying is processed, according to CNT and the suitable mass ratio of ceria, by two kinds of solution mixing, carry out supersound process, after carry out hydro-thermal reaction, finally giving form is that nano ceric oxide granule is attached to the growth of maziness combination electrode material on the carbon nanotubes.Operating procedure of the present invention is simple, preparation cost is cheap, it is to avoid the complex steps of conventional high temperature sintering, it is thus achieved that the combination electrode material that specific capacitance is big.
Description
Technical field
The invention belongs to be applied to the technical field of the nano-electrode material of ultracapacitor.Relate to using ultrasonic and water
Heat treatment prepares CNT (CNTs)/ceria (CeO2) method of nano material.
Background technology
Constantly aggravating along with fossil energy is faced with exhaustion and ecological deterioration day by day, ultracapacitor is novel as one
Environmentally friendly storage bodies tie up to corresponding application and paid attention to and constantly expand.According to the difference of energy storage mechnism, super
Level capacitor can be divided into double layer capacitor and Faradic electricity container.Double layer capacitor is to utilize between electrode and electrolyte
The interfacial electric double layer electric capacity formed stores energy, and its electrode generally uses the material with carbon element of high-specific surface area；Faradic electricity container
It is to utilize quick, the chemisorbed/desorption of high reversible and oxidation/reduction reaction, thus produces more higher than electric double layer capacitance
Specific capacity, its electrode material is mainly metal-oxide and conducting polymer.Electrode is an important composition of ultracapacitor
Part, electrode material is the most important factor determining ultracapacitor performance.The research of electrode material for super capacitor is subject to
The great attention of countries in the world.
Ceria (CeO2) it is rare-earth oxide, there is higher stability and strong oxidizing property, its avirulence, height
Chemical stability and high electron transfer capacity become the excellent selection of electrode material for super capacitor.Ceria price is low
Honest and clean and rich content, remains rare earth element and has the f layer electronic structure of uniqueness, and crystal formation is single.The CeO of nanostructured2Ratio
Surface area is big, and chemism is high, has very much prospect in electrode material for super capacitor application aspect.Additionally, ceria reaches to receive
Meter level not after, its ionic conductivity is the most significantly affected, electronics grain boundary resistance reduce, electrical conductivity improves 4 orders of magnitude
Left and right.But simple CeO2It is applicable to electrode material for super capacitor despite above advantage, but rare earth metal aoxidizes
Thing still has the weakness that electric conductivity is the highest, CeO2Being more suitable for and other materials, the high Material cladding of such as electric conductivity is as super
Level capacitor electrode material is more particularly suitable.CNT (CNTs) has good electric conductivity, due to the structure of CNT
Identical with the lamellar structure of graphite, so having good electric property.The conduction property utilizing CNT can be produced
The composite of a lot of excellent performances.
At present, the rare-earth oxide reported and other substance composite have CeO2/ graphene, CeO2/
CNTs, by other materials and CeO2The composite prepared in certain mass ratio, this material is used for super capacitor electrode
Pole material obtains the electrochemical properties of excellence.Such as Ramchandra S Kalubarme et al. (2013) One step
hydrothermal synthesis of a carbon nanotube/cerium oxide nanocomposite and
its electrochemical properties.Raja Rajendran et al. (2014) Dimensionally
Integrated Nanoarchitectonics for Novel Composite from 0D,1D,and 2D
Nanomaterials:RGO/CNT/CeO2Ternary Nanocomposite withElectrochemical
Performance。
Summary of the invention
The technical problem to be solved in the present invention is, uses the mass ratio that CNT is most suitable with ceria, first
The way carrying out hydro-thermal after ultrasonic prepares CNT composite nano cerium dioxide electrode material；The form of this electrode material is to receive
Rice cerium oxide particles is attached on the CNT of maziness growth, has excellent chemical property.
Present invention utilizes the mass ratio using CNT most suitable with ceria, this ratio is different from existing
Ratio employed in technology, prepares performance and is better than the sample of similar composite in other documents.Pass through effects of ion
Carry out the process synthesized, use Ce (NO3)3·6H2O, as cerium source, carries out morphology control by polyvinylpyrrolidone to it,
Meanwhile, process having purchased the CNT returned, by the mixing of two kinds of solution, carry out supersound process, after carry out
Hydro-thermal reaction, finally gives required sample.
The concrete technical scheme of the present invention is as follows.
A kind of preparation method of CNT composite nano cerium dioxide electrode material,
First configuration question response solution: add six nitric hydrate cerium (Ce (NO in deionized water3)3·6H2And poly-second O)
Alkene pyrrolidone (PVP), stirring configuration cerous nitrate aqueous solution, the most in mass ratio six nitric hydrate ceriums: polyvinylpyrrolidone:
Deionized water=8.68～8.69: 0.5: 40；It is sequentially added into CNT (CNTs) and detergent alkylate in deionized water
Sodium sulfonate (SDBS), stirring formation carbon nano tube suspension, the most in mass ratio CNT: dodecylbenzene sodium sulfonate: go
Ionized water=6: 1: 1000～1100；CNT in mass ratio: six nitric hydrate cerium=0.04: 1；
Stirring in configuration question response solution, is stirring 2h.
Next carries out supersound process: mixed nitrate cerium aqueous solution and carbon nano tube suspension, ultrasonic disperse 2h, is mixed
Liquid；
Last Hydrothermal Synthesis: mixed liquor is loaded reactor, reacts 24h at 220 DEG C；It is naturally cooling to room temperature, opens
Reactor, carries out the centrifuge washing of sample, drying, obtains CNT composite nano cerium dioxide electrode material.
Described supersound process, it is therefore an objective to shatter CNT makes it be sufficiently mixed with cerium ion, the most ensuing
Water-heat process cerium ion can preferably be attached on CNT grow.
Described centrifuge washing, can wash 3 times, and dehydrated alcohol is washed 2 times, and centrifugation rotating speed is 10000rpm, every time
Centrifugation time 5min；Described drying, can be washing complete by sample at 60 DEG C down to drying completely.
The pattern of sample is observed by the material sample that the method for the present invention prepares by SEM, can see this sample
Pattern the most special, nano ceric oxide granule be attached on the CNT of maziness growth, and, by with made
The pattern contrast of standby pure ceria, sends out now with in the compound material of CNT, ceria growth more uniform,
Pattern size is more homogeneous, more dispersed, and reunites together unlike pure ceria, and such material is as ultracapacitor
Electrode material can obtain higher specific capacitance, and its reason should be CNT to be had for the ionic charge offer in electrolyte is more
The transport passage of power, the redox reaction relying on ceria to be provided produces faraday's capacitance characteristic, and the carbon of hollow
Nanotube is conducive to the storage of electric charge, and both feature combines and creates the chemical property higher than simple bi-material
Good characteristic so that it is become and have the biggest prospect in electrode material for super capacitor application aspect.
The method of the present invention be use first ultrasonic after carry out the way of hydro-thermal and be prepared sample.Its ingenious feasible part
The method being to use hydrothermal treatment consists, it is to avoid the complex steps of conventional high temperature sintering, however by appropriate CNTs with
CeO2 mass ratio, it is thus achieved that the sizable composite of specific capacitance, the sample prepared by the present invention combines CNT
Excellent electric conductivity and the excellent oxygen ion conduction of ceria and oxygen storage capacity, prepared sample has the highest electrification
Learn activity.
Operating procedure of the present invention is simple, and preparation cost is cheap, it is adaptable to industrial mass production uses.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum that embodiment 1 prepares sample.
Fig. 2 is the scanning electron microscope (SEM) photograph that embodiment 1 prepares under sample low power.
Fig. 3 is the scanning electron microscope (SEM) photograph that embodiment 1 prepares under sample high power,
Fig. 4 is the scanning electron microscope (SEM) photograph of pure ceria.
Fig. 5 is the transmission electron microscope picture that embodiment 1 prepares sample.
Fig. 6 is the cyclic voltammetry curve figure obtained by embodiment 2 carries out electro-chemical test
Fig. 7 is the constant current charge-discharge figure obtained by embodiment 2 carries out electro-chemical test.
Fig. 8 is the cycle life figure obtained by embodiment 2 carries out electro-chemical test.
Fig. 9 is the AC impedance spectrogram before and after embodiment 2 is circulated life test.
Figure 10 is that embodiment 2 sample is at the AC impedance spectrogram done before cycle life test and fitting data figure.
Detailed description of the invention
The preparation of embodiment 1 CNT composite nano cerium dioxide electrode material
Specific experiment device of the present invention is as follows: 100mL conical flask two (conical flask A and conical flask B), 250mL conical flask
One (conical flask C), HJ-6 type magnetic force heating stirrer, KQ2200DE type numerical control ultrasonic cleaner, table model high speed centrifuge
H1850。
Experimental drug prepares as follows: six nitric hydrate cerium (Ce (NO3)3·6H2O), polyvinylpyrrolidone (PVP), carbon is received
Mitron (CNTs), dodecylbenzene sodium sulfonate (SDBS), secondary deionized water.
First question response solution it is respectively configured: take 40mL and 60mL secondary deionized water respectively and add conical flask A and taper
In bottle B, weigh 8.6848g six nitric hydrate cerium (Ce (NO3)3·6H2O) configuration 0.5mol/L cerous nitrate in conical flask A is added molten
Liquid, adds 0.5g polyvinylpyrrolidone (PVP), stirs 2h, by accounting for six nitric hydrate cerium (Ce (NO3)3·6H2O) quality
4wt% weighs CNT (CNTs) 0.348g, and weighs dodecylbenzene sodium sulfonate (SDBS) 0.058g (in mass ratio
MCNTs:MSDBS=6:1), CNT (CNTs) and dodecylbenzene sodium sulfonate (SDBS) are sequentially added into conical flask B,
Stirring 2h forms carbon nano tube suspension；
Secondly, liquid mixing in conical flask A, conical flask B is added in conical flask C, ultrasonic disperse 2h, obtain mixing molten
Liquid, the purpose of this process is that CNT is sufficiently mixed by shatter CNT with cerium ion, the most ensuing hydro-thermal mistake
Journey cerium ion can preferably be attached on CNT grow；
Finally loading in still by mixed solution, putting into baking oven, oven temperature and time is adjusted to 220 DEG C respectively, and 24h is carried out instead
Should.Reaction terminates, and temperature is down to room temperature naturally, opens reactor, sample uses the method for centrifugation wash, secondary
Water washs 3 times, and absolute ethanol washing 2 times, rotating speed is 10000rpm, each centrifugation time 5min.After washing, sample is existed
60 DEG C down to drying completely.Finally obtain CNT composite nano cerium dioxide electrode material.
The XRD figure spectrum of the CNT composite nano cerium dioxide electrode material prepared is shown in Fig. 1, sample as seen from Figure 1
The existence at Zhong Youtan peak, XRD peak, it was demonstrated that compound for ceria/CNT has been carried out.Fig. 2 and Fig. 3 provides carbon and receives
The scanning electron microscope (SEM) photograph of mitron composite nano cerium dioxide electrode material.Scanning electron microscope (SEM) photograph (Fig. 2) from low power it can be seen that
Under the effect of CNT, ceria is that the uniform and scattered CNT that depends on grows；From high power
Scanning electron microscope (SEM) photograph (Fig. 3) it is clear that, ceria is coated on CNT outgrowth, with the CNT of duration length
Unroll and inhibit ceria overgrowth, to reach to be formed the purpose of nanometer materials.Fig. 5 provides prepared CNT
The transmission electron microscope picture of composite nano cerium dioxide electrode material sample.
As a comparison, Fig. 4 provides the scanning electron microscope (SEM) photograph of pure ceria.The ceria prepared by hydro-thermal method, granule
Reuniting together, bad dispersibility, granular size differs, and grows uneven.
The test of embodiment 2 CNT composite nano cerium dioxide electrode material
The material that embodiment 1 prepares is fabricated to working electrode.The concrete preparation process of working electrode: select acetylene black to make
For conductive agent, testing sample is mixed with acetylene black 8:1 in mass ratio and puts in mortar, add dehydrated alcohol for making it the most mixed
Closing, be fully ground form slurry shape, with little spoon uniform application in nickel foam, be baked at 60 DEG C, employing Manual tablet pressing machine will
Electrode slice is depressed into 6Mpa and keeps 1min, increase electrode material to contact with nickel foam.
Carrying out the used work station of electro-chemical test is Bio-Logic Model VMP3 16Channel model, is used
Method of testing be three electrode test methods, platinum plate electrode is as to electrode, and calomel electrode coats as reference electrode, foam nickel screen
Testing sample is as working electrode.Treating the project that side sample carries out testing has cyclic voltammetry (CV), constant current charge-discharge to survey
Examination (GCD), ac impedance measurement (EIS) and the test of cycle life.Test result is given by Fig. 6 to Figure 10.
Fig. 6 is that sample carries out the cyclic voltammetry curve figure obtained by electro-chemical test as electrode material, can from Fig. 6
Go out cyclic voltammetry (CV) test result, sweep speed than electric capacity at the cyclic voltammetric of 1mV/s and be issued to 818Fg-1, and along with scanning
The increase of speed, material reduces than electric capacity.But, it is up to 200mVs at scanning speed-1Time still there is 183Fg-1Ratio electricity
Hold.
Fig. 7 provides sample and carries out the constant current charge-discharge figure obtained by electro-chemical test as electrode material, though test result
So draw more slightly lower compared with the ratio electric capacity that cyclic voltammetry (CV) is measured than electric capacity, but test than same type of material constant current charge-discharge
Method (GCD) gained is more slightly higher than electric capacity, and multiplying power property curve is more mild, electric current density 1Ag-1Lower test result
For 558Fg-1, when electric current density is increased to 30Ag-1, sample specific capacitance is down to 243Fg-1, it was demonstrated that the electrochemical properties of this sample
Relatively stable.
The present invention uses constant current charge-discharge test that sample is circulated life test, and finds that sample is carrying out 2000 times
After circulation, specific capacitance only has the decay of 4.7%.Fig. 8 provides sample and carries out electro-chemical test gained as electrode material
The cycle life figure arrived, as shown in Figure 8, after the constant current charge-discharge carrying out 2000 times is tested, the ratio capacitance fade of sample is also
Not quite, prove the stability of sample prepared by this invention further, illustrate that this material has in terms of electrode material for super capacitor
There is good application prospect.
Fig. 9 is that sample is circulated the AC impedance spectrogram before and after life test as electrode material, is carrying out 2000 times
Constant current charge-discharge test before and after, impedance variation is the most not very big.
Figure 10 is sample at the AC impedance spectrogram done before cycle life test and fitting data figure, inserts in Figure 10
Equivalent circuit diagram, is shown that by fitting data the resistance value of sample is the most little, R1Value is 0.091 ohm, and CPE value is 0.9 ohm, R2
Value is 1 ohm, RwIt it is 1.4 ohm.
Claims (2)
1. the preparation method of a CNT composite nano cerium dioxide electrode material, it is characterised in that
First configuration question response solution: add six nitric hydrate cerium and polyvinylpyrrolidones, stirring configuration in deionized water
Cerous nitrate aqueous solution, the most in mass ratio six nitric hydrate ceriums: polyvinylpyrrolidone: deionized water=8.68～8.69: 0.5
∶40；Being sequentially added into CNT and dodecylbenzene sodium sulfonate in deionized water, stirring forms carbon nano tube suspension,
CNT the most in mass ratio: dodecylbenzene sodium sulfonate: deionized water=6: 1: 1000～1100；Carbon nanometer in mass ratio
Pipe: six nitric hydrate cerium=0.04: 1；
Next carries out supersound process: mixed nitrate cerium aqueous solution and carbon nano tube suspension, ultrasonic disperse 2h, obtains mixed liquor；
Last Hydrothermal Synthesis: mixed liquor is loaded reactor, reacts 24h at 220 DEG C；It is naturally cooling to room temperature, opens reaction
Still, carries out the centrifuge washing of sample, drying, obtains CNT composite nano cerium dioxide electrode material.
The preparation method of CNT composite nano cerium dioxide electrode material the most according to claim 1, its feature exists
In, described centrifuge washing, is washing 3 times, and dehydrated alcohol is washed 2 times, and centrifugation rotating speed is 10000rpm, each centrifugation time
5min；Described drying, be washing complete by sample at 60 DEG C down to drying completely.
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Cited By (3)
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| CN108807943A (en) * | 2018-07-19 | 2018-11-13 | 齐鲁工业大学 | A kind of hollow-core construction CeO2@C core-shell structure copolymer nanocomposites and the preparation method and application thereof |
| CN110734724A (en) * | 2018-10-19 | 2020-01-31 | 嘉兴学院 | Preparation method of epoxy resin heat-conducting glue |
| CN115231604A (en) * | 2022-08-31 | 2022-10-25 | 华中科技大学 | Microstructure-controllable nano cerium dioxide catalyst based on photothermal hydrolysis hydrogen production |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108807943A (en) * | 2018-07-19 | 2018-11-13 | 齐鲁工业大学 | A kind of hollow-core construction CeO2@C core-shell structure copolymer nanocomposites and the preparation method and application thereof |
| CN108807943B (en) * | 2018-07-19 | 2020-12-25 | 齐鲁工业大学 | CeO with hollow structure2@ C core-shell nano composite material and preparation method and application thereof |
| CN110734724A (en) * | 2018-10-19 | 2020-01-31 | 嘉兴学院 | Preparation method of epoxy resin heat-conducting glue |
| CN110734724B (en) * | 2018-10-19 | 2021-12-21 | 嘉兴学院 | Preparation method of epoxy resin heat-conducting adhesive |
| CN115231604A (en) * | 2022-08-31 | 2022-10-25 | 华中科技大学 | Microstructure-controllable nano cerium dioxide catalyst based on photothermal hydrolysis hydrogen production |
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Application publication date: 20161207 |