CN109741959A - A kind of graphene/iron-based MOF super capacitor material and preparation method thereof - Google Patents
A kind of graphene/iron-based MOF super capacitor material and preparation method thereof Download PDFInfo
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- CN109741959A CN109741959A CN201811588291.5A CN201811588291A CN109741959A CN 109741959 A CN109741959 A CN 109741959A CN 201811588291 A CN201811588291 A CN 201811588291A CN 109741959 A CN109741959 A CN 109741959A
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Abstract
The present invention relates to a kind of graphene/iron-based MOF super capacitor materials, which is characterized in that is prepared by the following steps: (1) weighing FeCl according to quality proportioning3·6H2O、Ni(NO3)2·6H2O、H2BDC and DMF is simultaneously mixed uniformly；(2) graphene oxide is added, stirs 1h, ultrasonic 2h, is stirred for 1h, it is to be mixed uniformly after move into reaction kettle；(3) at 110~140 DEG C heat preservation 20~for 24 hours, cooled to room temperature, by centrifuge separation, solid is then cleaned 3 times with DMF and obtains presoma；(4) presoma obtained by step (3) is put into baking oven, in 60~80 DEG C of vacuum drying 12h, obtains graphene/iron-based MOF super capacitor material.During metal-organic framework materials synthesis, using its own condition, " one-step method " has obtained graphene-ferrous metals organic framework composite material；Prepared RGO/MOFs composite material pattern is good, is tightly combined；The introducing of graphene oxide enhances the electric conductivity of material, significantly improves the specific capacitance of material.
Description
Technical field
The invention belongs to field of capacitor material technology, and in particular to a kind of graphene/iron-based MOF super capacitor material
And preparation method thereof.
Background technique
Supercapacitor is a kind of novel energy-storing element between conventional capacitive and battery, has use temperature range
Wide (- 20 DEG C -60 DEG C), the advantages that charging time is short, output power is high, the pollution-free and service life is long.And current supercapacitor
Electrode material mostly uses the composite material of carbon material, metal oxide, or both.
Metal organic framework (Metal Organic Frameworks, MOFs) material is a kind of mainly first by oxygen-containing or nitrogen
The organic ligand of element is connect with transition metal ions and the multidimensional periodicity mesh skeleton material that is formed.MOFs crystal has three-dimensional
Aperture road, higher specific surface area and regular, adjustable pore structure and the features such as hole surface, these features make MOFs
Material obtains very big concern in many research fields such as adsorbing separation, gas storage, shape-selective and chiral catalysis, biological medicine.
MOFs material is as micropore possesses as mesopore molecular sieve regularly arranged cellular structure and special nature, therefore MOFs is in conduct
The numerous areas such as template, catalysis, absorption and light, electricity, magnetic are widely used.
The unique two-dimensional structure of graphene and outstanding intrinsic physical characteristic, such as abnormal high electric conductivity and large surface
Product, application of the graphene-based material in supercapacitor have great potentiality.Graphene-based material and traditional electrode material
Material is compared, during energy storage and release, it is shown that some novel features and mechanism.
Summary of the invention
For the above-mentioned prior art, the technical problem to be solved in the present invention is that it is super to provide a kind of graphene/iron-based MOF
Capacitor material and preparation method thereof, it is good to prepare pattern, compact graphene-ferrous metals organic backbone composite wood
Material, introduces iron-based MOF material for graphene oxide, with the electric conductivity of reinforcing material, improves the specific capacitance of material.
For this purpose, being prepared by the following steps the present invention provides a kind of graphene/iron-based MOF super capacitor material:
(1) FeCl is weighed according to quality proportioning3·6H2O、Ni(NO3)2·6H2O、H2BDC and DMF is simultaneously mixed uniformly；
(2) graphene oxide is added, stirs 1h, ultrasonic 2h, is stirred for 1h, it is to be mixed uniformly after move into reaction kettle；
(3) at 110~140 DEG C heat preservation 20~for 24 hours, cooled to room temperature, by centrifuge separation, then solid is used
DMF is cleaned 3 times and is obtained presoma；
(4) presoma obtained by step (3) is put into baking oven, in 60~80 DEG C of vacuum drying 12h, obtains graphene/iron-based
MOF super capacitor material；
The molar ratio of each raw material in the step (1) are as follows: FeCl3·6H2O:Ni (NO3)2·6H2O:H2BDC:DMF=1~
2:0~2:1:16~282, the additional amount of graphene oxide is 0.5~2mg/ml in the step (2).
Preferably, in the step (1) each raw material molar ratio are as follows: FeCl3·6H2O:Ni (NO3)2·6H2O:H2BDC:
DMF=1~2:0~2:1:16, the additional amount of graphene oxide is 2mg/ml in the step (2).
Preferably, in the step (1) each raw material molar ratio are as follows: FeCl3·6H2O:Ni (NO3)2·6H2O:H2BDC:
DMF=1~2:0~2:1:282, the additional amount of graphene oxide is 1mg/ml in the step (2).
Preferably, the holding temperature in the step (3) is 110 DEG C, soaking time 20h.
Preferably, the holding temperature in the step (3) is 140 DEG C, and soaking time is for 24 hours.
The present invention also provides a kind of graphene/iron-based MOF super capacitor material preparation methods, including following step
It is rapid:
(1) FeCl is weighed according to quality proportioning3·6H2O、Ni(NO3)2·6H2O、H2BDC and DMF is simultaneously mixed uniformly；
(2) graphene oxide is added, stirs 1h, ultrasonic 2h, is stirred for 1h, it is to be mixed uniformly after move into reaction kettle；
(3) at 110~140 DEG C heat preservation 20~for 24 hours, cooled to room temperature, by centrifuge separation, then solid is used
DMF is cleaned 3 times and is obtained presoma；
(4) presoma obtained by step (3) is put into baking oven, in 60~80 DEG C of vacuum drying 12h, obtains super capacitor equipment
Material；
The molar ratio of each raw material in the step (1) are as follows: FeCl3·6H2O:Ni (NO3)2·6H2O:H2BDC:DMF=1~
2:0~2:1:16~282, the additional amount of graphene oxide is 0.5~2mg/ml in the step (2).
Preferably, the vacuum drying temperature of the step (4) is 70 DEG C.
In conclusion graphene of the present invention/iron-based MOF super capacitor material preparation method is utilized, with six water trichlorines
Change iron (FeCl3·6H2O), ferric nitrate (Ni (NO3)2·6H2O), terephthalic acid (TPA) (H2BDC) and dimethylformamide (DMF) is
Raw material successfully has developed RGO/MIL-88 and RGO/MIL-53 material, and is constructed and carry out electrical property survey for supercapacitor
Examination, test result are excellent.
The beneficial effect that the present invention obtains is: during metal-organic framework materials synthesis, using its own condition,
" one-step method " has obtained graphene-ferrous metals organic framework composite material；Prepared RGO/MOFs composite material pattern
Well, it is tightly combined；The introducing of graphene oxide (grapheneoxide, GO) enhances the electric conductivity of material, significantly improves
The specific capacitance of material.
Detailed description of the invention
Fig. 1 is that the SEM of sample schemes；
Fig. 2 is sample electric performance test figure.
Specific embodiment
A specific embodiment of the invention is described in detail with reference to the accompanying drawing:
Embodiment 1:
According to molar ratio FeCl3·6H2O:Ni (NO3)2·6H2O:H2BDC:DMF=1:1:1:282 weighs each raw material and mixes
It closes uniformly, is then added graphene oxide into mixed liquor according to the amount of 0.5mg/ml, it is small to carry out ultrasound 2 after stirring 1 hour
When, it is stirred for 1 hour, moves into 50ml autoclave, reacted 24 hours at 140 DEG C after mixing, centrifugation obtains solid production
Object is washed 3 times with DMF, and it is 0.5-RGO/MIL-88 that 70 DEG C of vacuum drying, which obtain crocus powder,.
Embodiment 2:
According to molar ratio FeCl3·6H2O:Ni (NO3)2·6H2O:H2BDC:DMF=1:1:1:282 weighs each raw material and mixes
It closes uniformly, is then added graphene oxide into mixed liquor according to the amount of 1mg/ml, carry out ultrasound 2 hours after stirring 1 hour,
It being stirred for 1 hour, moves into 50ml autoclave, reacted 24 hours at 140 DEG C after mixing, centrifugation obtains solid product,
It is washed 3 times with DMF, it is 1-RGO/MIL-88 that 70 DEG C of vacuum drying, which obtain crocus powder,.
Embodiment 3:
According to molar ratio FeCl3·6H2O:Ni (NO3)2·6H2O:H2BDC:DMF=1:1:1:282 weighs each raw material and mixes
It closes uniformly, is then added graphene oxide into mixed liquor according to the amount of 2mg/ml, carry out ultrasound 2 hours after stirring 1 hour,
It being stirred for 1 hour, moves into 50ml autoclave, reacted 24 hours at 140 DEG C after mixing, centrifugation obtains solid product,
It is washed 3 times with DMF, it is 2-RGO/MIL-88 that 70 DEG C of vacuum drying, which obtain crocus powder,.
Embodiment 4:
According to molar ratio FeCl3·6H2O:Ni (NO3)2·6H2O:H2BDC:DMF=2:1:1:16 weighs each raw material and mixes
It closes uniformly, is then added graphene oxide into mixed liquor according to the amount of 0.5mg/ml, it is small to carry out ultrasound 2 after stirring 1 hour
When, it is stirred for 1 hour, moves into 50ml autoclave, reacted 20 hours at 110 DEG C after mixing, centrifugation obtains solid production
Object is washed 3 times with DMF, and it is 0.5-RGO/MIL-53 that 70 DEG C of vacuum drying, which obtain crocus powder,.
Embodiment 5:
According to molar ratio FeCl3·6H2O:Ni (NO3)2·6H2O:H2BDC:DMF=2:1:1:16 weighs each raw material and mixes
It closes uniformly, is then added graphene oxide into mixed liquor according to the amount of 1mg/ml, carry out ultrasound 2 hours after stirring 1 hour,
It being stirred for 1 hour, moves into 50ml autoclave, reacted 20 hours at 110 DEG C after mixing, centrifugation obtains solid product,
It is washed 3 times with DMF, it is 1-RGO/MIL-53 that 70 DEG C of vacuum drying, which obtain crocus powder,.
Embodiment 6:
According to molar ratio FeCl3·6H2O:Ni (NO3)2·6H2O:H2BDC:DMF=2:1:1:16 weighs each raw material and mixes
It closes uniformly, is then added graphene oxide into mixed liquor according to the amount of 2mg/ml, carry out ultrasound 2 hours after stirring 1 hour,
It being stirred for 1 hour, moves into 50ml autoclave, reacted 20 hours at 110 DEG C after mixing, centrifugation obtains solid product,
It is washed 3 times with DMF, it is 2-RGO/MIL-53 that 70 DEG C of vacuum drying, which obtain crocus powder,.
Fig. 1 is that the SEM of sample schemes, and wherein a, b, c are that MIL-88/RGO composite sample GO concentration is respectively 0.5mg/ml,
Sample drawing when 1mg/ml and 2mg/ml；D, e, f are respectively that MIL-53/RGO composite sample GO concentration is respectively 0.5mg/ml, 1mg/
Sample drawing when ml and 2mg/ml.From figure 1 it appears that gained sample topography is good.Metal organic framework particle equably divides
There is not structure collapse phenomenon, and the two is tightly combined on graphene sheet layer and piece interlayer in cloth.
Fig. 2 is sample electric performance test figure, and wherein a, b are respectively MIL-88 and various concentration composite sample cyclic voltammetric pair
Than scheming and sweeping speed and specific capacitance relationship comparison diagram；C, d are respectively MIL-53 and various concentration composite sample cyclic voltammetric comparison diagram
And sweep speed and specific capacitance relationship comparison diagram.Test condition: the carbon-point collector for coating active material is working electrode, platinum electrode
For auxiliary electrode, saturated calomel electrode is reference electrode, and 1M KOH aqueous solution is electrolyte.From figure 2 it can be seen that GO's adds
Enter and improve to electrical property, with increasing for GO concentration, electrical property is also increased accordingly.When sweeping speed is 10mv/s,
For MIL-88 series when GO additional amount is 1mg/ml, the specific capacitance of material reaches maximum value, is 187.5F/g, and simple MIL-88
Sample specific capacitance is only 40.24F/g；For MIL-53 series when GO additional amount is 2mg/ml, the specific capacitance of material reaches maximum value,
For 156.7F/g, it is higher by by about one time than simple MIL-53 sample specific capacitance.
The embodiments of the present invention are described in detail for above-mentioned combination attached drawing, but the present invention is not limited to above-mentioned implementations
Mode can also make many variations to it within the knowledge of one of ordinary skill in the art.
Claims (7)
1. a kind of graphene/iron-based MOF super capacitor material, which is characterized in that be prepared by the following steps:
(1) FeCl is weighed according to quality proportioning3·6H2O、Ni(NO3)2·6H2O、H2BDC and DMF is simultaneously mixed uniformly；
(2) graphene oxide is added, stirs 1h, ultrasonic 2h, is stirred for 1h, it is to be mixed uniformly after move into reaction kettle；
(3) at 110~140 DEG C heat preservation 20~for 24 hours, cooled to room temperature, by centrifuge separation, then by solid DMF
It cleans 3 times and obtains presoma；
(4) presoma obtained by step (3) is put into baking oven, in 60~80 DEG C of vacuum drying 12h, it is super obtains graphene/iron-based MOF
Grade capacitor material；
The molar ratio of each raw material in the step (1) are as follows: FeCl3·6H2O:Ni (NO3)2·6H2O:H2BDC:DMF=1~2:0
~2:1:16~282, the additional amount of graphene oxide is 0.5~2mg/ml in the step (2).
2. graphene according to claim 1/iron-based MOF super capacitor material, which is characterized in that the step (1)
In each raw material molar ratio are as follows: FeCl3·6H2O:Ni (NO3)2·6H2O:H2BDC:DMF=2:1:1:16, in the step (2)
The additional amount of graphene oxide is 2mg/ml.
3. graphene according to claim 1/iron-based MOF super capacitor material, which is characterized in that the step (1)
In each raw material molar ratio are as follows: FeCl3·6H2O:Ni (NO3)2·6H2O:H2BDC:DMF=1:1:1:282, the step (2)
The additional amount of middle graphene oxide is 1mg/ml.
4. graphene according to claim 2/iron-based MOF super capacitor material, which is characterized in that the step (3)
In holding temperature be 110 DEG C, soaking time 20h.
5. graphene according to claim 3/iron-based MOF super capacitor material, which is characterized in that the step (3)
In holding temperature be 140 DEG C, soaking time be for 24 hours.
6. a kind of graphene/iron-based MOF super capacitor material preparation method, which comprises the following steps:
(1) FeCl is weighed according to quality proportioning3·6H2O、Ni(NO3)2·6H2O、H2BDC and DMF is simultaneously mixed uniformly；
(2) graphene oxide is added, stirs 1h, ultrasonic 2h, is stirred for 1h, it is to be mixed uniformly after move into reaction kettle；
(3) at 110~140 DEG C heat preservation 20~for 24 hours, cooled to room temperature, by centrifuge separation, then by solid DMF
It cleans 3 times and obtains presoma；
(4) presoma obtained by step (3) is put into baking oven, in 60~80 DEG C of vacuum drying 12h, obtains super capacitor material；
The molar ratio of each raw material in the step (1) are as follows: FeCl3·6H2O:Ni (NO3)2·6H2O:H2BDC:DMF=1~2:0
~2:1:16~282, the additional amount of graphene oxide is 0.5~2mg/ml in the step (2).
7. graphene according to claim 6/iron-based MOF super capacitor material preparation method, which is characterized in that institute
The vacuum drying temperature for stating step (4) is 70 DEG C.
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| CN111085275A (en) * | 2019-12-31 | 2020-05-01 | 华南理工大学 | Reductive graphene oxide/metal organic framework composite material and preparation method and application thereof |
| CN113840528A (en) * | 2021-09-01 | 2021-12-24 | 浙江工业大学 | MOF-derived composite wave-absorbing material and preparation method and application thereof |
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