CN110444406A - A kind of preparation method of fast activating three-dimensional Ni-C nano material as energy storage electrode material - Google Patents
A kind of preparation method of fast activating three-dimensional Ni-C nano material as energy storage electrode material Download PDFInfo
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- CN110444406A CN110444406A CN201910685819.9A CN201910685819A CN110444406A CN 110444406 A CN110444406 A CN 110444406A CN 201910685819 A CN201910685819 A CN 201910685819A CN 110444406 A CN110444406 A CN 110444406A
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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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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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
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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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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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
- H01G11/44—Raw materials therefor, e.g. resins or coal
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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 present invention relates to energy storage material technical fields, preparation method of specially a kind of fast activating three-dimensional Ni-C nano material as energy storage electrode material, this method is using organic acid, nickel source as presoma, N-N- dimethylformamide (DMF) is solvent, nickel foam is substrate, nickel metal organic frame, distilled water flushing, drying are synthesized by hydro-thermal reaction；The light green sample that will be obtained, sample is placed in the CVD tube furnace for being connected with inert gas, and carbonization obtains Ni-C material；Then Ni-C material is soaked in hydrogenperoxide steam generator, is then rinsed, dries the three-dimensional Ni-C nano material that activation can be obtained；The method of the present invention is simple, and raw material simplicity easily takes, and has high security and a feature of environmental protection, and can fast activating Ni-C material, the application easy to accomplish in industrialization, with great stored energy application prospect.
Description
Technical field
The present invention relates to energy storage material technical field, especially a kind of fast activating three-dimensional Ni-C nano material is as energy storage
The preparation method of electrode material.
Background technique
Energy shortage and environmental degradation are two significant problems that human social development can not be ignored in the process.With fossil
The consumption of the energy and the mankind are continuously increased demand for energy, and since the limitation of technology cannot get fossil energy
Make full use of, tap a new source of energy and novel energy storage and conversion equipment it is increasingly important.
In recent years, many researchers put into a large amount of time and efforts green regenerative energy sources research and development it
In, including wind energy, geothermal energy, solar energy etc..In numerous energy storage devices, electrochemical energy storing device is due to cost
It is low, energy density is high, high recycling rate and the advantages that have extended cycle life, be widely used.At this stage for society
Existing energy problem, the electrochemical storage device of development of new efficient stable, the utilization rate for improving the energy is 21 century emphasis
One of solve the problems, such as.
Supercapacitor, also known as electrochemical capacitor are a kind of equipments and devices that can store electric energy.Supercapacitor
It is the energy density having higher than 3~4 orders of magnitude of traditional capacitor, and has and be higher than 1~2 order of magnitude of lithium ion battery
Power density excellent energy storage device, for comprehensive performance between traditional capacitor and battery, the excellent characteristics having can
To meet the high request that the instrument and equipments such as electric system, backup power source and aerospace system proposes chemical energy source.However, losing
Regret, compared to battery, the low energy densities of supercapacitor are still very important short slab.Therefore, in order to make super electricity
Container is further developed, and finds the electrode material of high capacity to improve the energy density of supercapacitor, while keeping high
Power density properties are one of the emphasis of numerous scientists studies.
Metal organic frame (MOF) is a kind of emerging crystalline material, be by organic linker and metal ion/cluster it
Between coordinate bond constitute.Design and different method for pyrolysis by MOF presoma, adjust the composition and shape of its derived material
Looks can easily be translated into porous metal oxide, porous metals sulfide, porous carbon and its hybrid etc.
Micro/nano structure material.Importantly, having the MOF precursor construction of periodically assembling metal cluster can effectively keep away
The negative effect for exempting from aggregation, has a good application prospect.The working principle and electricity of MOF derivative (such as three-dimensional Ni-C material)
Pond/supercapacitor is similar, also can be used as ideal energy storage electrode material.However, the cyclical stability difference of MOF derivative is it
A very important short slab.Therefore, the stability for improving MOF derivative is the key that it is promoted further to develop.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of fast activating three-dimensional Ni-C nano material as energy storage electrode
The preparation method of material, preparation method of the present invention is simple, and material prepared by the present invention can be used in supercapacitor.
The technical solution of the present invention is as follows: a kind of preparation of fast activating three-dimensional Ni-C nano material as energy storage electrode material
Method, this method is using organic acid, nickel source as presoma, and N-N- dimethylformamide (DMF) is solvent, and nickel foam is substrate, leads to
Cross hydro-thermal reaction synthesis nickel metal organic frame, distilled water flushing, drying；The light green sample that will be obtained, sample is placed in logical
Have in the CVD tube furnace of inert gas, carbonization obtains Ni-C material；Then Ni-C material is soaked in hydrogenperoxide steam generator, so
The three-dimensional Ni-C nano material of activation can be obtained by flushing, drying；
Specifically includes the following steps:
S1), by base foam nickel successively acetone, 3mol L-1Be cleaned by ultrasonic respectively in hydrochloric acid, ethyl alcohol 10min, 5min,
After 5min in placement and hydrothermal reaction kettle；
S2), certain density organic acid and nickel source are dissolved in DMF solvent, after stirring is until be completely dissolved, pour into this water
In thermal response kettle, 8h is reacted in 100 DEG C of baking oven, is taken out, and through distilled water flushing, 60 DEG C of drying synthesize the nickel gold of green
Belong to organic frame sample；
S3), sample obtained in S2) is placed in the CVD tube furnace for being connected with inert gas, is carried out at 400~800 DEG C
Be carbonized 30~180min, obtains Ni-C material；
S4), Ni-C material obtained in step S3) is completely soaked to the hydrogenperoxide steam generator for being 10~30% in concentration
In, after activating 10~180min at 100~200 DEG C, through distilled water flushing 2 times, 60 DEG C of drying are to get the three-dimensional to after activating
Ni-C nano material.
Preferably, in the above method, the organic acid is terephthalic acid (TPA), in trimesic acid, phthalic acid
The mixing of any one or more.
It is furthermore preferred that the organic acid is terephthalic acid (TPA) in the above method.
Preferably, in the above method, the concentration of the organic acid is 0.01~0.1mol L-1。
It is furthermore preferred that the organic acid concentration is 0.05mol L in the above method-1。
Preferably, in the above method, the nickel source is nickel nitrate, nickel chloride, any one or more in nickel sulfate
Mixing.
It is furthermore preferred that the nickel source is nickel nitrate in the above method.
It is furthermore preferred that the nickel source concentration is 0.01~0.2mol L in the above method-1。
It is furthermore preferred that the nickel source concentration is 0.05mol L in the above method-1。
Preferably, in the above method, the inert gas is N2, in Ar any one or both mixed gas,
The flow velocity of the gas is 50~400sccm.
It is furthermore preferred that the inert gas is N in the above method2, the flow velocity of the gas is 200sccm.
It is furthermore preferred that the carburizing temperature is 500 DEG C in the above method, the carbonization time is 1h.
It is furthermore preferred that the hydrogenperoxide steam generator concentration is 15% in the above method.
It is furthermore preferred that the activation temperature is 180 DEG C in the above method, the activation time is 30min.
The invention has the benefit that the method for the present invention is simple, raw material simplicity is easily taken, and has high security and the feature of environmental protection,
And can fast activating Ni-C material, the application easy to accomplish in industrialization, have great stored energy application prospect.
Detailed description of the invention
Fig. 1 is scanning (SEM) figure of sample prepared by the embodiment of the present invention 1 and 2, wherein a is before activating in embodiment 2
High and low multiplying power scanning electron microscope (SEM) figure of Ni-C material；B is that the high and low multiplying power of Ni-C material after activating in embodiment 1 is swept
Electronic Speculum (SEM) figure is retouched, is (c) X-ray energy spectrum (EDS) figure of dashed rectangle part in (b)；
What Fig. 2 was that the embodiment of the present invention 1 and 2 prepares sample is 6mol L in electrolyte-1In KOH solution, sweeping speed is 10mV
s-1Under cyclic voltammetry curve；
Fig. 3 is that prepare sample in current density be 30mA cm to the embodiment of the present invention 1 and 2-2Under constant current charge-discharge curve
Figure；
Fig. 4 is that the embodiment of the present invention 1 and 2 prepares the electrochemical impedance figure of sample under the same conditions；
Fig. 5 is that prepare sample in current density be 30mA cm to the embodiment of the present invention 1 and 2-2Under the constant current charge-discharge service life
Performance.
Specific embodiment
Specific embodiments of the present invention will be further explained with reference to the accompanying drawing:
Embodiment 1
A kind of preparation method of fast activating three-dimensional Ni-C nano material as energy storage electrode material, comprising the following steps:
S1), by the base foam nickel of 2cm × 3cm successively acetone, 3mol L-1It is cleaned by ultrasonic respectively in hydrochloric acid, ethyl alcohol
After 10min, 5min, 5min in placement and hydrothermal reaction kettle；
S2), by 0.05mol L-1Terephthalic acid (TPA) and 0.05mol L-1Nickel nitrate is dissolved in DMF solvent, and stirring is until complete
It after fully dissolved, pours into this hydrothermal reaction kettle, 8h is reacted in 100 DEG C of baking oven, take out, through distilled water flushing, 60 DEG C are dried,
Synthesize the nickel metal organic frame sample of green；
S3), sample obtained in S2) is placed in and is connected with N2CVD tube furnace in, carbonization 1h is carried out at 500 DEG C, is obtained
Ni-C material；
S4), Ni-C material obtained in step S3) is completely soaked in the hydrogenperoxide steam generator that concentration is 15%, In
After activating 30min at 180 DEG C, through distilled water flushing 2 times, 60 DEG C of drying are remembered to get to the three-dimensional Ni-C nano material after activation
For ANC.
Embodiment 2
S1), by the base foam nickel of 2cm × 3cm successively acetone, 3mol L-1It is cleaned by ultrasonic respectively in hydrochloric acid, ethyl alcohol
After 10min, 5min, 5min in placement and hydrothermal reaction kettle；
S2), by 0.05mol L-1Terephthalic acid (TPA) and 0.05mol L-1Nickel nitrate is dissolved in DMF solvent, and stirring is until complete
It after fully dissolved, pours into this hydrothermal reaction kettle, 8h is reacted in 100 DEG C of baking oven, take out, through distilled water flushing, 60 DEG C are dried,
Synthesize the nickel metal organic frame sample of green；
S3), sample obtained in S2) is placed in and is connected with N2CVD tube furnace in, carbonization 1h is carried out at 500 DEG C, is obtained
Ni-C material, is denoted as NC.
Embodiment 3-12
The method that embodiment 3-12 is used is same as Example 1, by regulating and controlling different Carbonization Conditions and activation condition, shadow
The chemical property for ringing three-dimensional Ni-C nano material, referring specifically to table 1.
1 embodiment 3-12 of table carbonization adjusting, activation condition and Comparative result
Embodiment 13
Performance test
The test of Flied emission scanning electron microscopy Electronic Speculum is carried out to the sample of Examples 1 and 2 preparation, as a result such as Fig. 1 (a), (b)
Shown, wherein Fig. 1 (a) is the high and low multiplying power scanning electron microscope (SEM) of Ni-C material before activating in embodiment 2；Fig. 1 (b) is to implement
High and low multiplying power scanning electron microscope (SEM) figure of Ni-C material after example 1 activates, Fig. 1 (c) are the X-ray energy spectrum of Blocked portion in (b)
(EDS) figure, the pattern after scanning electron microscopy electron microscope shows Ni-C material before activation do not change significantly, while right
Ni-C material after activation is analyzed using X-ray energy spectrum (EDS), and as a result as shown in (c) of Fig. 1, X-ray energy spectrogram is shown
In Ni-C material after activation there are oxygen elements, it was demonstrated that the introducing of oxygen-containing functional group.
Cyclic voltammetry and the constant current charge-discharge test that Fig. 2 and Fig. 3 is respectively adopted in electrochemical method activate to study
The capacitive property of the Ni-C material (NC and ANC) of front and back, by calculating, ANC sample is 30mA cm in current density-2When ratio
Area capacitance value is 4430mF cm-2, it is NC sample specific area capacitance (782mF cm under same current density-2) 5.6 times.
Fig. 4 uses electrochemical impedance spectral method (EIS) and is studied the electric conductivity of the Ni-C material of activation front and back,
Schemed by EIS it is found that compared to untreated Ni-C material, the electric conductivity of the Ni-C material after hydrogen peroxide activates obtains
Certain raising.Fig. 5 uses the constant current charge-discharge test in electrochemical method to study the stability of NC and ANC, leads to
Calculating is crossed it is found that being 30mA cm in current density-2Under, the stability (appearance after circulation 500 times of the Ni-C sample after activation
Amount conservation rate is (capacity retention ratio after circulation 500 times is only 48.5%) for 78.0%) being substantially better than unactivated sample.Thus
As it can be seen that carrying out activation to Ni-C nano material using hydrogen peroxide can be improved its capacitive property and cyclical stability, this is in energy
Source storage aspect has great application prospect.
Examples 1 and 2 illustrate it is activated after the chemical property of Ni-C nano material significantly improve；Embodiment 1,3
~6 illustrate that Carbonization Conditions influence the chemical property of three-dimensional Ni-C nano material, and embodiment 1,7~12 illustrates to activate
Influence of the condition to Ni-C nano material.The chemical property of Ni-C nano material is not as good as embodiment 1 in the embodiment 3~12
's.
The above embodiments and description only illustrate the principle of the present invention and most preferred embodiment, is not departing from this
Under the premise of spirit and range, various changes and improvements may be made to the invention, these changes and improvements both fall within requirement and protect
In the scope of the invention of shield.
Claims (10)
1. a kind of preparation method of fast activating three-dimensional Ni-C nano material as energy storage electrode material, it is characterised in that: the party
Method is using organic acid, nickel source as presoma, and N-N- dimethylformamide (DMF) is solvent, and nickel foam is substrate, passes through hydro-thermal reaction
Synthesize nickel metal organic frame, distilled water flushing, drying；The light green sample that will be obtained, sample is placed in and is connected with inert gas
CVD tube furnace in, carbonization obtain Ni-C material；Then Ni-C material is soaked in hydrogenperoxide steam generator, is then rinsed, is dried
The dry three-dimensional Ni-C nano material that activation can be obtained；
Specifically includes the following steps:
S1), by base foam nickel successively acetone, 3mol L-1After being cleaned by ultrasonic 10min, 5min, 5min respectively in hydrochloric acid, ethyl alcohol
In placement and hydrothermal reaction kettle；
S2), certain density organic acid and nickel source are dissolved in DMF solvent, after stirring is until be completely dissolved, it is anti-pours into this hydro-thermal
It answers in kettle, 8h is reacted in 100 DEG C of baking oven, take out, through distilled water flushing, 60 DEG C of drying, that is, the nickel metal for synthesizing green has
Machine frame sample；
S3), sample obtained in S2) is placed in the CVD tube furnace for being connected with inert gas, is carbonized at 400~800 DEG C
30~180min obtains Ni-C material；
S4), Ni-C material obtained in step S3) is completely soaked in the hydrogenperoxide steam generator that concentration is 10~30%, In
After activating 10~180min at 100~200 DEG C, through distilled water flushing 2 times, 60 DEG C of drying are to get the three-dimensional Ni-C to after activating
Nano material.
2. a kind of preparation side of the fast activating three-dimensional Ni-C nano material according to claim 1 as energy storage electrode material
Method, it is characterised in that: the organic acid be terephthalic acid (TPA), trimesic acid, in phthalic acid any one or it is more
The mixing of kind, the concentration of the organic acid are 0.01~0.1mol L-1。
3. a kind of preparation side of the fast activating three-dimensional Ni-C nano material according to claim 2 as energy storage electrode material
Method, it is characterised in that: the organic acid is terephthalic acid (TPA), and the organic acid concentration is 0.05mol L-1。
4. a kind of preparation side of the fast activating three-dimensional Ni-C nano material according to claim 1 as energy storage electrode material
Method, it is characterised in that: the nickel source is nickel nitrate, nickel chloride, the mixing of any one or more in nickel sulfate, the nickel source
Concentration is 0.01~0.2mol L-1。
5. a kind of preparation side of the fast activating three-dimensional Ni-C nano material according to claim 4 as energy storage electrode material
Method, it is characterised in that: the nickel source is nickel nitrate, and the nickel source concentration is 0.05mol L-1。
6. a kind of preparation side of the fast activating three-dimensional Ni-C nano material according to claim 1 as energy storage electrode material
Method, it is characterised in that: the inert gas is N2, in Ar any one or both mixed gas, the stream of the gas
Speed is 50~400sccm.
7. a kind of preparation side of the fast activating three-dimensional Ni-C nano material according to claim 6 as energy storage electrode material
Method, it is characterised in that: the inert gas is N2, the flow velocity of the gas is 200sccm.
8. a kind of preparation side of the fast activating three-dimensional Ni-C nano material according to claim 1 as energy storage electrode material
Method, it is characterised in that: the carburizing temperature is 500 DEG C, and the carbonization time is 1h.
9. a kind of preparation side of the fast activating three-dimensional Ni-C nano material according to claim 1 as energy storage electrode material
Method, it is characterised in that: the hydrogenperoxide steam generator concentration is 15%.
10. a kind of preparation of the fast activating three-dimensional Ni-C nano material according to claim 1 as energy storage electrode material
Method, it is characterised in that: the activation temperature is 180 DEG C, and the activation time is 30min.
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Cited By (2)
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| CN112473708A (en) * | 2020-11-27 | 2021-03-12 | 中国林业科学研究院林产化学工业研究所 | Catalyst for producing biological aviation fuel oil by catalyzing hydrogenation of grease, and preparation method and application thereof |
| CN112893858A (en) * | 2019-11-19 | 2021-06-04 | 中国科学院大连化学物理研究所 | Preparation method of nickel-carbon-based material |
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Application publication date: 20191112 |