CN107658142B - The preparation method of nitrogen oxygen codope porous carbon/ferriferrous oxide composite material and its application in electrode of super capacitor - Google Patents
The preparation method of nitrogen oxygen codope porous carbon/ferriferrous oxide composite material and its application in electrode of super capacitor Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of nitrogen oxygen codope porous carbon/ferriferrous oxide composite material, following steps：(1) the cyclopentadienyl group iron, hexachlorobutadiene and pyridine for weighing certain part by weight are added in ptfe autoclave liner, mixing；(2) it seals, is put into pyroreaction kettle, screws reaction kettle cover, be placed in baking oven and reacted 6 24 hours in 180 220 DEG C；(3) it is cooled to room temperature, opens reaction kettle, product is placed in baking oven 120 DEG C, drying 6 hours；(4) it takes appropriate amount of sample to be placed in the quartz ampoule middle section of tube furnace, leads to argon gas, empty the air in pipe；Heating rate is 10 DEG C/min, and tubular type furnace temperature is made slowly to heat up, and instrument cools down automatically after maintaining 60 120min, is cooled to, and closes gas, obtains nitrogen oxygen codope porous carbon/ferriferrous oxide composite material；The nitrogen oxygen codope porous carbon/ferriferrous oxide composite material has excellent electric property, for making super capacitor electrode, has huge potentiality in electrochemical field.
Description
Technical field
The present invention provides a kind of composite material and preparation method, purposes, are co-doped with specifically, providing a kind of nitrogen oxygen
The preparation method of miscellaneous porous carbon/ferriferrous oxide composite material and its application in electrode of super capacitor, belong to inorganic work(
It can material and electrochemical energy technical field.
Background technology
In the present information age, people have higher requirement for energy storage device, and ultracapacitor is as a kind of
Energy storage device has relatively simple operation principle, high charge-discharge velocity (power density), good stability and makes
With the service life, to the object as people's extensive concern and research.
But compared with lithium battery, the energy density of ultracapacitor it is still relatively small (Science, 2008.321
(5889):Pp.651-652.), energy density can pass through E=0.5CU2Calculate (C:Specific capacitance, unit F/g；U:Voltage, it is single
Position V), so when voltage is identical, its energy density can be improved by improving specific capacitance.Therefore, research has high than electricity
Hold the substance of characteristic seems extremely important as the electrode material of ultracapacitor, and the electrode material of ultracapacitor is to determine it
Therefore one of the key factor of capacitive property quality prepares while having both high power density, high-energy density, high capacitance capacity
Electrode material with cyclical stability is the key that solve the problems, such as.
Although carbon material have good electric conductivity and chemical stability, it is cheap, prepare it is simple and environmental-friendly
Many advantages, such as, but its specific capacitance highest only has 200F/g, and its tap density is relatively low, causes its volumetric capacitance relatively low, because
And limit its extensive use.The specific capacitance of ruthenic oxide in transition metal oxide is very high, but ruthenium is expensive,
Limit its extensive use in commodity production.Although there is conducting polymer cheap, preparation to be easy, the quasi- electricity of faraday
Hold the advantages that high, but its chemical stability is poor, capacitance fade is very fast.It follows that different types of electrode material individually makes
Used time, there are poorly conductive, it is of high cost, specific capacitance is low and cyclical stability is poor the shortcomings of.The different characteristic system of bond material
It is the direction of current research at the superior composite material of chemical property, composite material is shown more than single electrode material
More advantages can play the advantage of different materials, to improve the overall performance of ultracapacitor.
Invention content
The first purpose of the invention is to provide the nitrogen oxygen codopes of a kind of good specific capacitance, electric conductivity and low cost
Porous carbon/ferriferrous oxide composite material.
Second object of the present invention is to provide a kind of preparation of nitrogen oxygen codope porous carbon/ferriferrous oxide composite material
Method.
Third object of the present invention is to provide a kind of nitrogen oxygen codope porous carbon/ferriferrous oxide composite materials super
Application process in electrode for capacitors.
First goal of the invention to realize the present invention, technical solution is that steps are as follows：
(1) cyclopentadienyl group iron 5-20mmol is weighed, is added in the ptfe autoclave liner of 50mL, adds
Hexachlorobutadiene and pyridine, the additive amount of hexachlorobutadiene are 1-30mL, and the molar ratio of the hexachlorobutadiene and pyridine is 1:
0.03-30, mixing；
(2) it is put into stainless steel high temperature reaction kettle after sealing, screws reaction kettle cover, place it in baking oven in 180-220
DEG C, it reacts 4-20 hours；
(3) cooled to room temperature closes baking oven power supply, opens reaction kettle, the product in kettle is transferred completely into surface
In ware, then drying obtains semi-finished product；
(4) it takes semi-finished product to be placed in porcelain boat, places it in the quartz ampoule middle section of tube furnace, lead to argon gas 30min, empty
Air in pipe；Then temperature and reaction time temperature program are set, heating rate is 10 DEG C/min, keeps tubular type furnace temperature slow
300-500 DEG C is risen to, instrument cools down automatically after maintaining 60-120min, closes gas after being cooled to room temperature, it is more to obtain nitrogen oxygen codope
Hole carbon/ferriferrous oxide composite material.
Preferably, the tube furnace temperature rise is 300-500 DEG C, specially 300 DEG C, 400 DEG C, 500 DEG C；It is described
Cyclopentadienyl group iron (Fe (C5H5)2) dosage be 5-20mmol, specially 5mmol, 10mmol, 15mmol, 20mmol.
The molar ratio of the hexachlorobutadiene and pyridine is 1:0.03-30, such as 1:0.03、 1:0.05、1:0.1、1:
0.5、1:1、1:2、1:5、1:10、1:15、1:20、1:25 or 1:30.
The reaction temperature may be, for example, 180 DEG C, 200 DEG C or 220 DEG C, preferably 200 DEG C.
Reaction time is 2-20 hours, be may be, for example, 4 hours, 8 hours, 12 hours, 16 or 20 hours.
The tube furnace temperature rise is 600-800 DEG C, specially 600 DEG C, 700 DEG C, 800 DEG C.
Realize second goal of the invention of the present invention, the technical solution of the present invention is to provide above-mentioned preparation methods to be prepared into
The nitrogen oxygen codope porous carbon/ferriferrous oxide composite material arrived.
The nitrogen oxygen codope porous carbon/ferriferrous oxide composite material has excellent electric property, has good
Specific capacitance, electric conductivity, can be applied to capacitor area, especially ultracapacitor field, have a good application prospect.
Realize the third goal of the invention of the present invention, the invention further relates to a kind of electrode of super capacitor, the super capacitors
The preparation method of device electrode is：By the nitrogen oxygen codope porous carbon/ferriferrous oxide composite material and acetylene black, poly- four
Vinyl fluoride presses 8:1:1 mass ratio is ground uniformly in mortar；Ethyl alcohol is added, mixture is tuned into paste, and by the paste of gained
Object is coated to the circular shaped foam nickel surface of a diameter of 1.5cm, and with dry 10-15min under infrared lamp；Material after drying is pressed
Piece, pressure 5-6MPa, obtains super capacitor electrode.
As described above, the present invention provides a kind of preparation sides of nitrogen oxygen codope porous carbon/ferriferrous oxide composite material
Method and its application in electrode of super capacitor, the nitrogen oxygen codope porous carbon/ferriferrous oxide composite material have
Excellent electric property, can be used for making super capacitor electrode, have huge potentiality in electrochemical field.
Description of the drawings
The morphology characterization of the sample 10-Fe-N-C-400 of 1 gained of Fig. 1 embodiments；
The energy dispersion X-ray spectrum test (EDX) of the sample 10-Fe-N-C-400 of 1 gained of Fig. 2 embodiments；
Fig. 3 embodiments 1, embodiment 5 and the gained of embodiment 6 sample 10-Fe-N-C-400,10-Fe-N-C-300 and
The Raman and XRD diagram spectrum analysis of 10-Fe-N-C-500；
The XPS characterizations of the sample 10-Fe-N-C-400 of 1 gained of Fig. 4 embodiments；
Various samples obtained by Fig. 5 embodiments 1-6 characterize chemical property by cyclic voltammetry；
The sample 10-Fe-N-C-400 of 1 gained of Fig. 6 embodiments characterizes chemical property by constant current charge-discharge test.
Specific implementation mode
The present invention is specifically described below by embodiment, is served only for that invention is further explained, no
It can be interpreted as limiting the scope of the present invention, the technician in the field can be according to the content of foregoing invention to the present invention
Make some nonessential modifications and adaptations.
Instrument, drug used in following embodiments is as follows
1.1 instruments such as table 1
1.2 drugs such as table 2
Embodiment 1
(1) cyclopentadienyl group iron (Fe (C are weighed5H5)2) 10mmol, measure 2mL hexachlorobutadienes (C4Cl6) and 28mL pyrroles
Pyridine is added in the ptfe autoclave liner of 50mL, respectively as source of iron and carbon source, mixing；
(2) it is put into stainless steel high temperature reaction kettle after sealing, screws reaction kettle cover, placed it in anti-in 200 DEG C in baking oven
It answers 6 hours；
(3) cooled to room temperature closes baking oven power supply, opens reaction kettle, the product in kettle is transferred completely into glass
In surface plate, 120 DEG C are placed in baking oven, drying 6 hours, by the sample collection after drying in reagent bottle；
(4) it takes appropriate amount of sample to be placed in porcelain boat, places it in the quartz ampoule middle section of tube furnace, lead to argon gas 30min, row
Air in net pipe；Then temperature and reaction time temperature program are set, heating rate is 10 DEG C/min, keeps tubular type furnace temperature slow
Slow to rise to 400 DEG C, instrument cools down automatically after maintaining 90min, and gas is closed after being cooled to room temperature, obtain nitrogen oxygen codope porous carbon/
Ferriferrous oxide composite material is labeled as 10-Fe-N-C-400；
Embodiment 2-4
With the step in embodiment 1, in addition to cyclopentadienyl group iron (Fe will be weighed inside (1) step in embodiment 1
(C5H5)2) amount replace with outside 5mmol, 15mmol, 20mmol, other operations are constant, and the label for obtaining material is followed successively by 5-
Fe-N-C-400、15-Fe-N-C-400、 20-Fe-N-C-400；
Embodiment 5-6
With the step in embodiment 1, in addition to by tubular type furnace temperature inside (4) step in embodiment 1 rise to 300 DEG C, 500
Outside DEG C, other operations are constant, to which the label to material is followed successively by 10-Fe-N-C-300,10-Fe-N-C-500；
Embodiment 7
The preparation method of a kind of super capacitor electrode, the super capacitor electrode is：By the nitrogen oxygen codope porous carbon/
Ferriferrous oxide composite material presses 8 with acetylene black, polytetrafluoroethylene (PTFE):1:1 mass ratio is ground uniformly in mortar；Ethyl alcohol is added,
Mixture is tuned into paste, and the paste of gained is coated to the circular shaped foam nickel surface of a diameter of 1.5cm, and and infrared lamp
Lower baking 10-15min；Material after drying carries out tabletting, and pressure 5-6MPa obtains super capacitor electrode.
Below to nitrogen oxygen codope porous carbon/ferriferrous oxide composite material and capacitor made from the embodiment of the present invention
Electrode carries out performance characterization：
(1) morphology characterization of the sample 10-Fe-N-C-400 of 1 gained of embodiment
To nitrogen oxygen codope porous carbon/ferriferrous oxide composite material sample 10-Fe-N-C-400 of 1 gained of embodiment
The microscopic sdIBM-2+2q.p.approach of multiple and different means has been carried out, it is as a result as follows：
Fig. 1 (a) (b) is scanning electron microscope (SEM) photographs of the sample 10-Fe-N-C-400 under different amplification, can from figure
Go out, material obtained is the irregular ball of some polymerizations, and the size of ball is uneven, is porous structure, there is particle on the surface of ball
Substance is tentatively inferred as the compound containing Fe.Fig. 1 (c) (d) is that sample 10-Fe-N-C-400 is saturating under different amplification
Electron microscope is penetrated, from the graph, it is apparent that the integral color of ball is uniform, therefore, the ball of composition material is medicine ball, particulate matter
Matter is in the form of a column the surface for being evenly distributed on ball.
(2) the energy dispersion X-ray spectrum test (EDX) of the sample 10-Fe-N-C-400 of 1 gained of embodiment
The EDX energy spectrum diagrams of Fig. 2 porous carbons/ferriferrous oxide composite material sample 10-Fe-N-C-400, as seen from the figure sample
In contained element species and its relative amount, contain five kinds of elements of Fe, N, C, O, Cl in the sample of preparation, copper is from surveying
The copper mesh specimen frame arrived used in the process of examination.
(3) embodiment 1, embodiment 5 and the gained of embodiment 6 sample 10-Fe-N-C-400,10-Fe-N-C-300 and
The Raman and XRD diagram spectrum analysis of 10-Fe-N-C-500
Fig. 3 (a) be sample 10-Fe-N-C-400 by treatment of different temperature,
The Raman analysis spectrogram of 10-Fe-N-C-300 and 10-Fe-N-C-500, three kinds of materials are all in 1340cm-1With
1570cm-1Nearby there are two characteristic peaks of carbon, the respectively peaks D and the peaks G, it can be seen from the figure that composite material 10-Fe-
The peaks D of N-C-300 are with the peaks D and the intensity ratio ID/IG at the peaks G that the intensity ratio ID/IG at the peaks G is 0.77,10-Fe-N-C-400
0.91, the 10-Fe-N-C-500 peaks D and the intensity ratio I at the peaks GD/IGBe 0.81, it can be seen that the peaks D of 10-Fe-N-C-400 with
The intensity ratio I at the peaks GD/IGHighest illustrates that the defect of its carbon material surface is most, and active site is most, and chemical property is best；
Fig. 3 (b) is sample 10-Fe-N-C-400,10-Fe-N-C-300 and 10-Fe-N- by treatment of different temperature
The XRD spectrum of C-500, as seen from the figure, 2 angles θ of three materials are 11.7 ° and 26.4 ° and correspond to oxidized form graphite C respectively
(001) (002) crystal face of crystal face and graphited C, 2 θ of the angle of diffraction be 18.3 °, 30.1 °, 35.4 °, 43.1 °, 53.4 °,
47.2 °, 56.9 °, 62.5 ° and 73.9 ° correspond to Fe respectively3O4(111), (220), (311), (400), (422), (331),
(511), (440) and (533) crystal face matches with standard card JCPDS NO.65-3107.As seen from the figure, with temperature
The raising of degree enhances the crystallinity of sample.
(4) the XPS characterizations of the sample 10-Fe-N-C-400 of 1 gained of embodiment
Fig. 4 (a) is the complete scanning figures of XPS of hole carbon/ferriferrous oxide composite material sample 10-Fe-N-C-400.From figure
In as can be seen that the composite material contain five kinds of elements of Fe, N, C, O, Cl.Wherein oxygen element, be due to sample in air by
Oxidation generates Fe3O4And introduce.Several element of Fe, the content of N, C, O, Cl are respectively 18.34%, 5.87%, 52.85,
15.89%, 7.04%.It is the C1s spectrograms of gained 10-Fe-N-C-400 composite materials as shown in Fig. 4 (b), bond energy exists
284.8eV is C=C keys, and 285.8eV is C=N keys, and 287.5eV is C-N keys and 289eV is C-O keys.As shown in Fig. 4 (c), it is
The N1s spectrograms of gained 10-Fe-N-C-400 composite materials, bond energy are pyridine nitrogen in 398.8eV, and 401eV is graphited nitrogen.
It is the Fe2p spectrograms of gained 10-Fe-N-C-400 composite materials as shown in Fig. 4 (d), bond energy is Fe in 711.3eV3O4,
718.5eV is Fe3+, 724.9eV Fe.It is the O1s spectrograms of gained 10-Fe-N-C-400 composite materials as shown in Fig. 4 (e),
Bond energy is Fe in 530eV3O4, 531.4eV and 533.2eV are C-O keys.
(5) the various samples obtained by embodiment 1-6 characterize chemical property by cyclic voltammetry
Fig. 5 (a) is sample 10-Fe-N-C-400,10-Fe-N-C- that composite material passes through that treatment of different temperature obtains
CV curves of the 300 and 10-Fe-N-C-500 in the case where sweeping speed and being 20mv/s, it can be seen from the figure that in potential window -1.1-0V models
In enclosing, the area that the CV curves of 10-Fe-N-C-400 are surrounded is maximum, by capacitance calculation formula Cm=S/2 (m △ Vv) can
Know, the capacitance of 10-Fe-N-C-400 composite materials is maximum, is 177.7F/g, 10-Fe-N-C-300 and 10-Fe-N-C-
The quality of 500 composite materials is respectively 101.5F/g and 144.9F/g than capacitance.
Fig. 5 (b) is CV curve of the Fe-N-C-400 composite materials of different iron contents in the case where sweeping speed and being 20mv/s, from figure
As can be seen that in potential window -1.1-0V ranges, the area that the CV curves of 10-Fe-N-C-400 are surrounded is maximum, shows
Its capacitance is maximum, is 177.7F/g, and the quality specific capacitance of 5-Fe-N-C-400 and 15-Fe-N-C-400 composite materials is respectively
133.9F/g and 137.2F/g, in conclusion the capacitive property of 10-Fe-N-C-400 is best.
Fig. 5 (c) and (d) sweep the CV curves under speed for 10-Fe-N-C-400 composite materials in difference, can be obtained by calculating
Go out, with increase 1mv/s, 2mv/s, 5mv/s, 10mv/s, 20mv/s, 50mv/s, 100mv/s, the 200mv/s of sweep speed,
Its corresponding quality specific capacitance is gradually reduced 297.2F/g, 280.3F/g, 248F/g, 216.2F/g, 177.7F/g, 126F/g,
84F/g and 54.7F/g.Thus it will be evident that there is oxidation peak in -0.75V or so, apparent pseudo capacitance is shown
Performance.
(6) the sample 10-Fe-N-C-400 of 1 gained of embodiment characterizes chemical property by constant current charge-discharge test
Fig. 6 is constant current charge-discharge curve of the sample 10-Fe-N-C-400 composite materials under different current densities, with electricity
The continuous increase of current density, the time which completes a charge and discharge constantly shorten, current density 1A/g, 2A/g,
4A/g, 8A/g, 10A/g, 20A/g, 30A/g, 40A/g, 50A/g, corresponding quality specific capacitance is respectively 377F/g,
285.5F/g, 232F/g, 179.3F/g, 166.4F/g, 110.4F/g, 77.1F/g, 55.1F/g and 41.4F/g.This and Wang
Deng[149]The Fe of report3O4/ rGO composite materials are at current density 1A/g, and quality specific capacitance is compared for 186.7F/g, capacitive character
It can be well very much.Constant current charge-discharge curve also shows certain pseudo capacitance characteristic, occurs near redox peaks
Gentle slope illustrates that the material shows certain fake capacitance.
As described above, the present invention provides a kind of preparation sides of nitrogen oxygen codope porous carbon/ferriferrous oxide composite material
Method and its application in electrode of super capacitor, the nitrogen oxygen codope porous carbon/ferriferrous oxide composite material have
Excellent electric property, can be used for making super capacitor electrode, have huge potentiality in electrochemical field.
Claims (5)
1. a kind of preparation method of nitrogen oxygen codope porous carbon/ferriferrous oxide composite material, it is characterised in that：The method packet
Include following steps：
(1) cyclopentadienyl group iron 5-20mmol is weighed, is added in the ptfe autoclave liner of 50mL, adds chlordene
Butadiene and pyridine, the additive amount of hexachlorobutadiene are 1-30mL, and the molar ratio of the hexachlorobutadiene and pyridine is 1:0.03-
30, mixing；
(2) it is put into stainless steel high temperature reaction kettle after sealing, screws reaction kettle cover, place it in 180-220 DEG C in baking oven, instead
It answers 4-20 hours；
(3) cooled to room temperature closes baking oven power supply, opens reaction kettle, the product in kettle is transferred completely into surface plate,
Then drying obtains semi-finished product；
(4) it takes semi-finished product to be placed in porcelain boat, places it in the quartz ampoule middle section of tube furnace, lead to argon gas 30min, empty in pipe
Air；Then temperature and reaction time temperature program are set, heating rate is 10 DEG C/min, and tubular type furnace temperature is made to be slowly increased to
300-500 DEG C, instrument cools down automatically after maintaining 60-120min, closes gas after being cooled to room temperature, it is porous to obtain nitrogen oxygen codope
Carbon/ferriferrous oxide composite material.
2. the preparation method of nitrogen oxygen codope porous carbon/ferriferrous oxide composite material as described in claim 1, feature exist
In：In step (4), the tube furnace temperature rise is 300 DEG C, 400 DEG C or 500 DEG C.
3. the preparation method of nitrogen oxygen codope porous carbon/ferriferrous oxide composite material as described in claim 1, feature exist
In：In step (1), the dosage of the cyclopentadienyl group iron is 5mmol, 10mmol, 15mmol or 20mmol.
4. the nitrogen oxygen codope porous carbon that a kind of preparation method as described in one of claim 1-3 is prepared/tetra- aoxidize three
Iron composite material.
5. a kind of preparation method of electrode of super capacitor, it is characterised in that：Nitrogen oxygen described in one of claim 1-3 is co-doped with
Miscellaneous porous carbon/ferriferrous oxide composite material presses 8 with acetylene black, polytetrafluoroethylene (PTFE):1:1 mass ratio is ground uniformly in mortar；
Ethyl alcohol is added, mixture is tuned into paste, and the paste of gained is coated to the circular shaped foam nickel surface of a diameter of 1.5cm,
And dry 10-15min under infrared lamp；Material after drying carries out tabletting, and pressure 5-6MPa obtains super capacitor electrode.
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