CN107045949B - A kind of N-Fe2O3/ nitrogen sulphur codope graphene combination electrode material and preparation method - Google Patents
A kind of N-Fe2O3/ nitrogen sulphur codope graphene combination electrode material and preparation method Download PDFInfo
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- CN107045949B CN107045949B CN201710222138.XA CN201710222138A CN107045949B CN 107045949 B CN107045949 B CN 107045949B CN 201710222138 A CN201710222138 A CN 201710222138A CN 107045949 B CN107045949 B CN 107045949B
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- nitrogen sulphur
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- Y02E60/13—Energy storage using capacitors
Abstract
The present invention provides a kind of N-Fe2O3/ nitrogen sulphur codope graphene combination electrode material and preparation method, steps are as follows: graphene oxide is placed in ultrasonic disperse in the mixed solution of ethyl alcohol and ethylene glycol by step 1, obtains the dispersion solution A of stable homogeneous oxidizing graphene；Fe(NO3)39H2O and nitrogen sulphur source are added in the dispersion solution A of step 1 by step 2, are uniformly mixing to obtain mixed solution B；The mixed solution B of step 2 is transferred to progress incubation water heating reaction in polytetrafluoroethylene (PTFE) water heating kettle by step 3, obtains mixed liquor C after completion of the reaction；Step 4 filters the mixed liquor C of step 3, washing, drying, obtains product N-Fe2O3/ nitrogen sulphur codope graphene composite material.The present invention uses one step hydro thermal method synthesizing nano-particle to synthesize N-Fe for the first time2O3Nanometer particle load codope grapheme material, raw material is simple, and environmentally protective, synthesis process is simply pollution-free.
Description
Technical field
The present invention relates to a kind of preparation methods of composite material, more particularly to one kind is using nitrogen sulphur codope graphene as matrix
Localization loads the preparation method of N doping ferric oxide nanoparticles composite material, and prepared composite material can be applied to surpass
Grade capacitor area.
Background technique
As environmental pollution and energy shortage problem are got worse, finds novel fungible energy source and energy storage device has been compeled
In the eyebrows and eyelashes.Supercapacitor is due to specific capacitance height, and good cycling stability, operating temperature range is wide, and environmentally protective, charge efficiency is high
With the charging time it is short the advantages that and attract wide attention.Graphene has single layer two-dimensional structure, due to its biggish specific surface
The performances such as product, the stability of superelevation and excellent conductivity have become the research hotspot of electrochemical field.However document shows stone
The actual capacity of black alkene is less than theoretical capacity, and it is very fast to decay, this needs to carry out the electronics that heteroatomic doping adjusts graphene
Structure.(.Electrochimica such as Chen W, Shi J, Zhu T Acta, 2015,177:327-334；Yi H T, Zhu Y
The Journal of such as Q, Chen X Y Alloys&Compounds, 2015,649:851-858.) it is introduced in graphene film interlayer
N, the hetero atoms such as S can improve the electronic conductivity and high rate performance of graphene, and the doping of N can be in graphene lattice structure
More defects are introduced, and activate the C atom being connected with N, and the introducing of S can be effectively reduced the required activation energy of reaction, mention
The local reactivity of high graphene.Further, since the redistribution of graphene density and spin density, codope can produce
More defective holes generate significant synergistic effect during redox reaction storage charge occurs with metal oxide.
Simple transition metal and transition metal oxide are widely closed because of theoretical capacity with higher
Note, wherein the oxide of iron theoretical specific capacity with higher, cheap and easy to get and advantages of environment protection, receive more grind
Study carefully.But cyclical stability is poor, hinders the further development of actual electrode material.Nitrogen (N) is considered as most possible realization n
Type Fe2O3Doped chemical because its ionic radius and oxygen (O) are close, and N-Fe2O3With more active sites, have
Conducive to the transmission of electrolyte ion, to improve chemical property.By N-Fe2O3With nitrogen sulphur codope grapheme material recombination energy
It effectively avoids stacking between graphene, makes N-Fe2O3High capacitance and the bigger serface advantage of modified graphene material mutually tie
It closes, reaches the perfect combination of electric double layer capacitance and fake capacitance, greatly improve the capacitive property of composite material.Currently, a large amount of
Document to be doped all be first to be respectively synthesized nanoparticle and basis material, then carry out nanometer by two steps or above method
Particle and modified matrix material it is compound.(the .Journal of Alloys& such as Wang M, Huang Y, Chen X
Compounds, 2017,691:407-415.) Chinese patent literature of Publication No. CN105826572A discloses a kind of N, S
Codope carbon nanotube coats FexCatalyst precursor is first made, using high-temperature calcination and acid in the preparation method of C catalyst
Etching obtains catalyst material.
The present invention uses one step hydro thermal method to synthesize the oxide carried codope graphene composite material of N- for the first time, and by nitrogen
Doping oxide is applied to for the first time on the electrode material of supercapacitor, with common Fe(NO3)39H2O, graphene oxide, second
Alcohol, ethylene glycol and ammonium thiocyanate are raw material, synthesize N-Fe by easy one step hydro thermal method2O3/ nitrogen sulphur codope graphene is compound
Material, experimental implementation is simple, low in cost, prepared N-Fe2O3Charge can be largely stored, codope graphene can then mention
The channel of supplied for electronic transmission and stable structure skeleton, are conducive to the free migration of electrolyte ion, to give full play to N-Fe2O3
Synergistic effect between nanoparticle and graphene makes the perfect combination of electric double layer capacitance and fake capacitance, obtains having both high power
The super capacitor material of density and high-energy density.
Summary of the invention
It is an object of the invention to: a kind of N-Fe is prepared using easy one step hydro thermal method2O3/ nitrogen sulphur codope graphite
Alkene combination electrode material.
The present invention is achieved through the following technical solutions:
A kind of N-Fe2O3/ nitrogen sulphur codope graphene combination electrode material, the electrode material is by N-Fe2O3With nitrogen sulphur
Codope graphene is combined, the N-Fe2O3It is carried on the nitrogen sulphur codope graphene surface；The N-Fe2O3
In, N element doping is in Fe2O3Crystalline surface；In the nitrogen sulphur codope graphene, N, S element are entrained in graphene；?
The N-Fe2O3In/nitrogen sulphur codope graphene combination electrode material, the doping of N is 2.30wt%~2.39wt%, and S's mixes
Miscellaneous amount is 0.70%~0.90wt%.
A kind of N-Fe2O3The preparation method of/nitrogen sulphur codope graphene combination electrode material, steps are as follows:
Graphene oxide is placed in ultrasonic disperse in the mixed solution of ethyl alcohol and ethylene glycol by step 1, is obtained stable homogeneous
The dispersion solution A of graphene oxide；
Fe(NO3)39H2O and nitrogen sulphur source are added in the dispersion solution A of step 1 by step 2, are uniformly mixing to obtain mixing
Solution B；
The mixed solution B of step 2 is transferred to progress incubation water heating reaction in polytetrafluoroethylene (PTFE) water heating kettle, reaction by step 3
After obtain mixed liquor C；
Step 4 filters the mixed liquor C of step 3, washing, drying, obtains product N-Fe2O3/ nitrogen sulphur codope graphene
Composite material.
In step 1, in the dispersion solution A, the dosage of the graphene oxide and ethyl alcohol and the mixed solution of ethylene glycol
Than for 9mg:7mL, in the mixed solution of the ethyl alcohol and ethylene glycol, the volume of ethyl alcohol and the volume ratio of ethylene glycol be (0.5~
2):1。
Further, the volume ratio of ethyl alcohol and ethylene glycol is 2:1.
In step 2, in the mixed solution B, used Fe(NO3)39H2O and nitrogen sulphur source and the dispersion solution A
Amount ratio is 0.004mol:0.012~0.028mol:70mL.
Further, the nitrogen sulphur source is ammonium thiocyanate or ammonium persulfate.
Further, the nitrogen sulphur source is ammonium thiocyanate, and the molar ratio of the Fe(NO3)39H2O and ammonium thiocyanate is 1:6.
In step 3, the temperature of the incubation water heating reaction is 160~200 DEG C, and the reaction time is 18~30h.
Further, the temperature of constant temperature thermal response is 180 DEG C, and the reaction time is for 24 hours.
Compared with the prior art, the present invention has the following advantages:
1, the mixed solution of ethyl alcohol and ethylene glycol keeps nano particle diameter smaller, disperses more evenly, sulphur cyanogen under high temperature action
Sour ammonium decomposition releases S2-And NH4 +, N and S are doped in flake graphite alkene structure, double doped structure, NH are formed3It serves not only as
Alkali source, additionally it is possible to N be provided and form N-Fe2O3, graphene and Fe2O3The collective effect of crystalline surface nitrogen makes Fe2O3It can be more evenly
It is stably dispersed in codope graphene surface, reaches the perfect combination of electric double layer capacitance and fake capacitance, it is steady to improve electrochemistry circulation
It is qualitative.
2, XPS shows the N-Fe using the method for the present invention preparation2O3N is successfully in/nitrogen sulphur codope graphene composite material
It is doped to Fe2O3In crystalline surface and graphene, while S is doped in graphene.N is with carbonnitrogen bond, pyridine nitrogen, pyrroles's nitrogen
Exist with N-Fe characteristic peak form, S is with S2p3/2、S2p1/2With-SOnForm exists.Wherein the doping of N be 2.30wt%~
The doping of 2.39wt%, S are 0.70%~0.90wt%.
3, the present invention synthesizes N-Fe with one step hydro thermal method synthesizing nano-particle for the first time2O3Nanometer particle load codope graphite
Alkene material, raw material is simple, environmentally protective, and synthesis process is simply pollution-free.
4, prepared material is applied to the electrode material of supercapacitor for the first time, in the constant current density of 1.0A/g
Under, monopole specific capacitance is up to 1263.7F g-1。
Detailed description of the invention
Fig. 1 is prepared N-Fe2O3/ three-dimensional nitrogen sulphur codope graphene and N-Fe2O3The X-ray diffraction spectrum of independent component
Figure.
Fig. 2 is N-Fe2O3The X-ray photoelectron spectroscopic analysis of/nitrogen sulphur codope graphene, wherein figure A is N1S power spectrum
Peak, figure B are that S2p can spectral peak.
Fig. 3 is N-Fe under different amplification scales2O3The transmission electron microscope photo of/nitrogen sulphur codope graphene.
Fig. 4 is N-Fe2O3, nitrogen sulphur codope graphene, N-Fe2O3/ nitrogen sulphur codope graphene is in 1Ag-1Under the conditions of perseverance
Current charging and discharging curve graph.
Fig. 5 is N-Fe2O3The constant current charge-discharge curve graph of/nitrogen sulphur codope graphene under different current densities.
Specific embodiment
Below with reference to specific implementation example, the present invention will be further described.
Embodiment 1
Weigh 1.6159g Fe (NO3)3·9H2O(0.004mol)、0.9134g NH4SCN (0.012mol) ultrasonic disperse
In the mixed solution (volume ratio 2:1) of 70mL dehydrated alcohol and ethylene glycol, mixed solution is transferred to by ultrasonic disperse 1h
In 100mL water heating kettle, 180 DEG C of reactions are for 24 hours.Cooled to room temperature after the reaction was completed, dehydrated alcohol and deionized water alternately from
The heart washs ten times, and then 12 hours dry in 60 DEG C in a vacuum drying oven, grinding obtains N-Fe2O3Nanoparticle.Sample is in 2 θ
For 24.15 °, 33.16 °, 35.63 °, 40.82 °, 49.46 °, 54.07 °, 57.60 °, 62.44 °, 64.00 °, 71.95 ° and
75.46 ° there is the diffraction maximum of X-ray, and difference can be with Fe2O3(012) of crystal, (104), (110), (113),
(024), (116), (018), (214), (300), (1010) and (220) crystal face are corresponding with standard spectrum, such as Fig. 1, diffraction in figure
Peak is the characteristic diffraction peak of graphene and di-iron trioxide, shows to generate Fe2O3Nanoparticle.By the N- of above-mentioned preparation
Fe2O3Nano material carries out charge-discharge test, and current density is 1A g-1When, specific capacity value has reached 682.4F g-1；By
Specific capacity remains at 78% or more after 2000 charge-discharge tests.
Embodiment 2
Weigh 90mg graphene oxide, 0.9134g NH4SCN (0.012mol) ultrasonic disperse is in 70mL dehydrated alcohol and second
In the mixed solution (volume ratio 2:1) of glycol, mixed solution is transferred in 100mL water heating kettle by ultrasonic disperse 1h, and 180 DEG C
Reaction is for 24 hours.Cooled to room temperature after the reaction was completed, dehydrated alcohol and deionized water alternating centrifugal wash ten times, then true
12 hours are dried to get nitrogen sulphur codope graphene in 60 DEG C in empty drying box.Nitrogen sulphur codope graphene has biggish ratio
The doping of surface, nitrogen and sulphur has activated carbon atom adjacent thereto, increases the quantity of active site, is conducive to electrolyte ion
It reacts with active material.The nitrogen sulphur codope grapheme material of above-mentioned preparation is subjected to charge-discharge test, current density is
1A g-1When, specific capacity value has reached 643.2F g-1；After 2000 charge-discharge tests specific capacity remain at 93% with
On.
Example 3
Weigh 90mg graphene oxide, 1.6159g Fe (NO3)3·9H2O(0.004mol)、1.8269g NH4SCN
(0.024mol) ultrasonic disperse is in the mixed solution (volume ratio 0.5:1) of 70mL dehydrated alcohol and ethylene glycol, ultrasonic disperse
Mixed solution is transferred in 100mL water heating kettle by 1h, and 180 DEG C of reactions are for 24 hours.Cooled to room temperature after the reaction was completed, anhydrous second
Pure and mild deionized water alternating centrifugal washs ten times, then dries 12 hours in 60 DEG C in a vacuum drying oven to get N-Fe2O3/ tri-
Tie up nitrogen sulphur codope graphene.Product is through X-ray photoelectron spectroscopic analysis (XPS) nitrogen with graphite nitrogen, pyridine nitrogen, pyrroles's nitrogen and N-
Fe form exists, and sulphur is with S 2p3/2, S 2p1/2and-SOnForm exists, and shows that nitrogen-atoms is successfully doped to Fe2O3Crystalline substance
Lattice surface, nitrogen, phosphorus atoms are successfully doped in the lattice structure of graphene, such as Fig. 2.Three-dimensional nitrogen sulphur codope graphene has
The doping of biggish specific surface, nitrogen and sulphur has activated carbon atom adjacent thereto, increases the quantity of active site, forms more
More defective holes is conducive to electrolyte ion and reacts with active material.By the N-Fe of above-mentioned preparation2O3/ nitrogen sulphur codope stone
Black alkene material carries out charge-discharge test, and current density is 1A g-1When, specific capacity value has reached 1263.7F g-1, such as Fig. 4.1
0A g-1Under big current density, capacitor still has in 983F g-1, such as Fig. 5, there are gentle discharge platforms and bright for discharge curve
Aobvious redox reaction fake capacitance discharge process further illustrates that the composite material is used as the electrode material of capacitor in big electricity
The stability having had under current density.Specific capacity remains at 87% or more after 2000 charge-discharge tests.
Embodiment 4
Weigh 90mg graphene oxide, 1.6159g Fe (NO3)3·9H2O(0.004mol)、1.5224g NH4SCN
(0.020mol) ultrasonic disperse is in the mixed solution (volume ratio 2:1) of 70mL dehydrated alcohol and ethylene glycol, ultrasonic disperse
Mixed solution is transferred in 100mL water heating kettle by 1h, 160 DEG C of reaction 30h.Cooled to room temperature after the reaction was completed, anhydrous second
Pure and mild deionized water alternating centrifugal washs ten times, then dries 12 hours in 60 DEG C in a vacuum drying oven to get N-Fe2O3/ nitrogen
Sulphur codope graphene.By the N-Fe of above-mentioned preparation2O3/ nitrogen sulphur codope grapheme material carries out charge-discharge test, current density
For 1A g-1When, specific capacity value has reached 364.8F g-1；Specific capacity remains at 53% after 2000 charge-discharge tests
More than.
Example 5
Weigh 90mg graphene oxide, 1.6159g Fe (NO3)3·9H2O(0.004mol)、2.1314g NH4SCN
(0.028mol) ultrasonic disperse is in the mixed solution (volume ratio 1:1) of 70mL dehydrated alcohol and ethylene glycol, ultrasonic disperse
Mixed solution is transferred in 100mL water heating kettle by 1h, 160 DEG C of reaction 18h.Cooled to room temperature after the reaction was completed, anhydrous second
Pure and mild deionized water alternating centrifugal washs ten times, then dries 12 hours in 60 DEG C in a vacuum drying oven to get N-Fe2O3/ nitrogen
Sulphur codope graphene.By the N-Fe of above-mentioned preparation2O3/ nitrogen sulphur codope grapheme material carries out charge-discharge test, current density
For 1Ag-1When, specific capacity value has reached 268.6F g-1；Specific capacity remains at 62% after 2000 charge-discharge tests
More than.
Example 6
Weigh 90mg graphene oxide, 1.6159g Fe (NO3)3·9H2O(0.004mol)、2.352g(NH4)2S2O8
(0.012mol) ultrasonic disperse is in the mixed solution (volume ratio 1:1) of 70mL dehydrated alcohol and ethylene glycol, ultrasonic disperse
Mixed solution is transferred in 100mL water heating kettle by 1h, and 180 DEG C of reactions are for 24 hours.Cooled to room temperature after the reaction was completed, anhydrous second
Pure and mild deionized water alternating centrifugal washs ten times, then dries 12 hours in 60 DEG C in a vacuum drying oven to get N-Fe2O3/ nitrogen
Sulphur codope graphene.As shown in figure 3, N-Fe2O3Nanoparticle is dispersed in nitrogen sulphur codope graphene surface, partial size model
It is trapped among 15-25nm.By the N-Fe of above-mentioned preparation2O3/ nitrogen sulphur codope grapheme material carries out charge-discharge test, and current density is
1A g-1When, specific capacity value has reached 968.6F g-1；After 2000 charge-discharge tests specific capacity remain at 78% with
On.
Example 7
Weigh 90mg graphene oxide, 1.6159g Fe (NO3)3·9H2O(0.004mol)、4.704g(NH4)2S2O8
((0.024mol) ultrasonic disperse in the mixed solution (volume ratio 0.5:1) of 70mL dehydrated alcohol and ethylene glycol, divide by ultrasound
1h is dissipated, mixed solution is transferred in 100mL water heating kettle, 200 DEG C of reaction 16h.Cooled to room temperature after the reaction was completed, it is anhydrous
Ethyl alcohol and deionized water alternating centrifugal wash ten times, then dry 12 hours in 60 DEG C in a vacuum drying oven to get N-Fe2O3/
Nitrogen sulphur codope graphene.By the N-Fe of above-mentioned preparation2O3/ nitrogen sulphur codope grapheme material carries out charge-discharge test, and electric current is close
Degree is 1A g-1When, specific capacity value has reached 842.6F g-1；Specific capacity remains at after 2000 charge-discharge tests
72% or more.
Example 8
Weigh 90mg graphene oxide, 1.6159g Fe (NO3)3·9H2O(0.004mol)、2.352g(NH4)2S2O8
(0.012mol) ultrasonic disperse is in the mixed solution (volume ratio 1:2) of 70mL dehydrated alcohol and ethylene glycol, ultrasonic disperse
Mixed solution is transferred in 100mL water heating kettle by 1h, 200 DEG C of reaction 30h.Cooled to room temperature after the reaction was completed, anhydrous second
Pure and mild deionized water alternating centrifugal washs ten times, then dries 12 hours in 60 DEG C in a vacuum drying oven to get N-Fe2O3/ nitrogen
Sulphur codope graphene.By the N-Fe of above-mentioned preparation2O3/ nitrogen sulphur codope grapheme material carries out charge-discharge test, current density
For 1A g-1When, specific capacity value has reached 768.4F g-1；Specific capacity remains at 78% after 2000 charge-discharge tests
More than.
The above disclosure is only a preferred embodiment of the invention, cannot limit right of the invention certainly with this
Range, therefore, the equivalent variations done in the scope of the invention still falls within the range that the present invention is covered.Skill belonging to the present invention
The technical staff in art field can do various modifications or supplement or is substituted in a similar manner to described specific embodiment,
However, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (8)
1. a kind of N-Fe2O3/ nitrogen sulphur codope graphene combination electrode material, which is characterized in that the electrode material is by N-
Fe2O3It is combined with nitrogen sulphur codope graphene, the N-Fe2O3It is carried on the nitrogen sulphur codope graphene surface；Institute
State N-Fe2O3In, N element is entrained in Fe2O3Crystalline surface；In the nitrogen sulphur codope graphene, N, S element are entrained in stone
In black alkene；In the N-Fe2O3In/nitrogen sulphur codope graphene combination electrode material, the doping of N be 2.30 wt% ~
The doping of 2.39wt%, S are 0.70% ~ 0.90wt%.
2. a kind of N-Fe as described in claim 12O3The preparation method of/nitrogen sulphur codope graphene combination electrode material, it is special
Sign is that steps are as follows:
Graphene oxide is placed in ultrasonic disperse in the mixed solution of ethyl alcohol and ethylene glycol by step 1, obtains stable homogeneous oxidizing
The dispersion solution A of graphene；
Fe(NO3)39H2O and nitrogen sulphur source are added in the dispersion solution A of step 1 by step 2, are uniformly mixing to obtain mixed solution
B；
The mixed solution B of step 2 is transferred to progress incubation water heating reaction, end of reaction in polytetrafluoroethylene (PTFE) water heating kettle by step 3
After obtain mixed liquor C；
Step 4 filters the mixed liquor C of step 3, washing, drying, obtains product N-Fe2O3/ nitrogen sulphur codope graphene is compound
Material；
In step 2, in the mixed solution B, the dosage of used Fe(NO3)39H2O and nitrogen sulphur source and the dispersion solution A
Than for 0.004mol:0.012 ~ 0.028mol:70mL.
3. a kind of N-Fe as claimed in claim 22O3The preparation method of/nitrogen sulphur codope graphene combination electrode material, it is special
Sign is, in step 1, in the dispersion solution A, and the amount ratio of the graphene oxide and ethyl alcohol and the mixed solution of ethylene glycol
For 9mg:7mL, in the mixed solution of the ethyl alcohol and ethylene glycol, the volume of ethyl alcohol and the volume ratio of ethylene glycol are (0.5 ~ 2): 1.
4. a kind of N-Fe as claimed in claim 32O3The preparation method of/nitrogen sulphur codope graphene combination electrode material, it is special
Sign is that further, the volume ratio of ethyl alcohol and ethylene glycol is 2:1.
5. a kind of N-Fe as claimed in claim 22O3The preparation method of/nitrogen sulphur codope graphene combination electrode material, it is special
Sign is that further, the nitrogen sulphur source is ammonium thiocyanate or ammonium persulfate.
6. a kind of N-Fe as claimed in claim 22O3The preparation method of/nitrogen sulphur codope graphene combination electrode material, it is special
Sign is, further, the nitrogen sulphur source is ammonium thiocyanate, and the molar ratio of the Fe(NO3)39H2O and ammonium thiocyanate is 1:6.
7. a kind of N-Fe as claimed in claim 22O3The preparation method of/nitrogen sulphur codope graphene combination electrode material, it is special
Sign is, in step 3, the temperature of the incubation water heating reaction is 160 ~ 200 DEG C, and the reaction time is 18 ~ 30 h.
8. a kind of N-Fe as claimed in claim 72O3The preparation method of/nitrogen sulphur codope graphene combination electrode material, it is special
Sign is that further, the temperature of constant temperature thermal response is 180 DEG C, and the reaction time is 24 h.
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| CN104028222A (en) * | 2014-05-13 | 2014-09-10 | 同济大学 | Composite nano-material, preparation method and application thereof to remove tetrabromobisphenol-A |
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