CN107644743A - A kind of preparation method of the three-dimensional porous nitrogen-doped graphene of self-supporting-nickel hydroxide electrochemical capacitance electrode material - Google Patents
A kind of preparation method of the three-dimensional porous nitrogen-doped graphene of self-supporting-nickel hydroxide electrochemical capacitance electrode material Download PDFInfo
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- CN107644743A CN107644743A CN201710741976.8A CN201710741976A CN107644743A CN 107644743 A CN107644743 A CN 107644743A CN 201710741976 A CN201710741976 A CN 201710741976A CN 107644743 A CN107644743 A CN 107644743A
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- 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 a kind of three-dimensional porous nitrogen-doped graphene/nickel hydroxide electrode material preparation method, including：Prepare nano porous copper；Prepare three-dimensional porous nitrogen-doped graphene：Under argon gas and hydrogen atmosphere, furnace temperature is risen to 700 1000 DEG C, calcined 13 minutes at this temperature；Calcined again under acetylene, ammonia, hydrogen, argon gas atmosphere 15 minutes；Sample is quickly down to room temperature under the atmosphere of argon gas, then placed a sample into corrosive liquid, removes the copper mold plate of the inside；It is then that obtained sample is clean with deionized water and alcohol washes successively, then dry and can obtain the three-dimensional porous nitrogen-doped graphene film of self-supporting.Prepare three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite.
Description
Technical field
The invention belongs to graphene composite material applied technical field, and in particular to a kind of three-dimensional porous graphene-hydrogen-oxygen
Change the preparation method of nickel composite material.
Background technology
Due to the quick consumption of fossil fuel and the sternness increasingly of problem of environmental pollution, filled as electrochemical energy storage
Star of hope in putting --- ultracapacitor has obtained extensive concern.Ultracapacitor is as a kind of new energy storage
Device, due to its have high power density (>10k W·kg-1), fast charging and discharging process (in several seconds), the stable circulation longevity
Life (>105It is secondary), the advantages that reliability is high, environmentally friendly and low maintenance cost, it is widely used in consumer electronics production
In product, new-energy automobile, Aero-Space, storage and backup system, industrial power and mobile electronic system.Because electrode material is direct
The quality of performance of the supercapacitor is determined, the research for ultracapacitor at present is concentrated mainly on its critical component --- electricity
Pole material；It is most important to develop green, cheap and excellent performance electrode material.
Graphene is by sp2The carbon atom of hydridization is tightly packed into only monoatomic layer and the two dimensional surface of cellular crystal
Structure.Because it has the specific surface area, good chemical stability, excellent mechanical and excellent chemical property of superelevation
The advantages that, become preferable electrode material for super capacitor.But in actual applications, due to depositing for model ylid bloom action power
Graphene frequently suffers from serious reunion or stacking, causes substantially reducing for specific surface area and conductance；And graphene soaks
Lubricant nature is very poor, causes it fully to be contacted with electrolyte.In addition, the energy storage mechnism based on electric double layer, causes graphene super
The specific capacitance of capacitor is relatively low, and these prevent graphene from meeting actual demand, to limit its answering in ultracapacitor
With.
At present, the method for improving graphene capacitor specific capacitance mainly has two kinds.One kind is by carrying out work(to graphene
Energyization is handled to adjust the electronic structure of graphene and chemical property, and wherein N doping is a kind of simple and effective method.
N doping can not only effectively prevent reunion or the stacking of graphene nanometer sheet, improve the electric conductivity of graphene, improve graphene
Hydrophily, moreover it also provides more avtive spot and forming core point, strengthen the phase between graphene and metallic compound
Interaction, so as to be advantageous to pattern, size Control and the raising of chemical property.Another kind is by graphene and metallic compound
It is compound.Metal compound electrode material has higher specific capacitance and energy density, and cheap, has become potential
Electrode material；But their electric conductivity and less stable, cause its short life.Both graphene and metallic compound are entered
Row is effectively compound, and the synergistic function between them can be utilized to realize the optimization of chemical property, both maintained graphene fast
The ability of fast discharge and recharge and good cyclical stability, the fake capacitance of metallic compound is made full use of to provide higher ratio electricity again
Appearance and energy density, so as to realize the Synergistic of chemical property.And the preparation of combination electrode material at present is mainly machinery
The conventional methods such as mixing, this method are difficult to make graphene compound uniformly with metallic compound, this compound advantage is cut significantly
It is weak, turn into the powerful resistance and bottleneck for limiting its development and industrialization.
The content of the invention
It is an object of the invention to provide a kind of three-dimensional porous nitrogen-doped graphene/nickel hydroxide electrode material system of Fabrication of High Specific Capacitance
Preparation Method.Three-dimensional porous nitrogen-doped graphene/nickel hydroxide electrode material obtained by the preparation method has the hole of three-dimensional insertion
Structure, increases substantially the chemical property of electrode material, and being capable of self-supporting, it is not necessary to which the slurry of dusty material is coated
Journey, can directly it be applied without any post-processing, can be cost-effective with simplification of flowsheet.The present invention solves the technology
The technical scheme of problem is,
A kind of three-dimensional porous nitrogen-doped graphene/nickel hydroxide electrode material preparation method, step are as follows：
1) nano porous copper is prepared
The alloy foil sheet of 80~120 μ m-thicks is prepared, wherein Cu, Mn atom number percentage is respectively 30% and 70%, room
Alloy foil sheet is placed in 0.01-0.3M hydrochloric acid weak solutions under temperature, 20-120 minutes are handled using the method for the de- alloy of chemistry；Will
Obtained nano porous copper is first cleaned with deionized water, then with washes of absolute alcohol, then by the nanoporous copper foil of cleaning
It is dried in vacuo at room temperature.
2) three-dimensional porous nitrogen-doped graphene is prepared
Nano porous copper made from step 1 is put into quartz boat, the quartz boat equipped with nano porous copper is placed in reaction
Pipe furnace thorax perimeter；Argon gas and hydrogen are first passed through, wherein, argon gas, hydrogen ratio press 500:200 flow configuration, now will
Furnace temperature rises to 700-1000 DEG C, quartz boat is quickly moved into flat-temperature zone in the middle part of reaction tube after furnace temperature rises to assigned temperature, herein
Temperature lower calcination 1-3 minutes；Then 1-50 is pressed again:5-50:500:200 flow proportional is passed through acetylene, ammonia, hydrogen, argon gas,
1-5 minutes are calcined on this condition；Quartz boat is quickly moved to outside burner hearth from flat-temperature zone in the middle part of reaction tube after calcining,
Sample is quickly down to room temperature under the atmosphere of argon gas, then taken out sample from tube furnace；Then it is the nanometer calcined is more
It is 10g that hole copper, which immerses proportioning,：10ml：In the corrosive liquid of 100ml iron chloride, hydrochloric acid and water, etching time is 10~24 hours,
Remove the copper mold plate of the inside；Then that obtained sample is clean with deionized water and alcohol washes successively, then drying can obtain
To the three-dimensional porous nitrogen-doped graphene film of self-supporting.
3) three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite is prepared
By six water nickel chlorides, urea and water according to 0.5-0.7g：1.1-1.3g：Nickel salt and urine is made in 70-90mL proportioning
Plain mixed solution 70~90ml altogether, in the reactor for the polytetrafluoroethyllining lining that mixed solution is transferred to；Then by step
2) the three-dimensional porous nitrogen-doped graphene film obtained by is also placed in reactor, static 1~3 hour, is then placed in vacuum drying
70~120 DEG C are heated in case, is reacted 4~20 hours, question response kettle is cooled to room temperature, and the self-supporting in inner liner of reaction kettle is thin
Film takes out, and produces three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite wood with deionized water and alcohol cleaning drying successively
Material, to prepare electrochemical capacitance electrode.
Compared with prior art, the present invention obtains three-dimensional porous N doping using nano porous metal as matrix using CVD
Graphene, finally by three-dimensional porous nitrogen-doped graphene and certain density nickel salt and urea mixed solution hydro-thermal, obtain self-supporting
Three-dimensional porous nitrogen-doped graphene and nickel hydroxide composite.The inventive method has the advantage that：(1) nitrogen in the present invention
The method that the preparation of doped graphene material uses chemical vapor deposition, this method technique is simple, the reaction time is short, yield is high,
Cost is low, pollution-free, environment-friendly, and a step can synthesize three-D nano-porous nitrogen-doped graphene；(2) the three of this method preparation
Tieing up porous nitrogen-doped graphene-nano whiskers nickel hydroxide composite has the three-dimensional structure continuously penetrated, improves electronics
With the transmission rate of ion；(3) three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite prepared by this method combines nitrogen
The characteristics of high conductivity and nickel hydroxide Fabrication of High Specific Capacitance of doped graphene, the structural behaviour for having given full play to nitrogen-doped graphene is excellent
Synergistic function between gesture and metallic compound, the chemical property of electrode material is greatly improved；(4) our legal system
Standby three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite being capable of self-supporting, it is not necessary to the slurry coating of dusty material
Process, it can directly be applied without any post-processing, simplify technological process, greatly save cost.
Brief description of the drawings
Fig. 1 is Cu used in the present invention30Mn70The photomacrograph of alloy foil sheet；
Fig. 2 is the nano porous copper SEM image prepared by the present invention；
Fig. 3 is the photomacrograph of the three-dimensional porous nitrogen-doped graphene prepared by example 1；
Fig. 4 is the SEM image for the three-dimensional porous nitrogen-doped graphene that example 1 is prepared by matrix of nano porous copper；
Fig. 5 is the TEM image for the three-dimensional porous nitrogen-doped graphene that example 1 is prepared by matrix of nano porous copper；
Fig. 6 is the XRD spectrum of three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite prepared by example 1；
Fig. 7 is the SEM image of three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite prepared by example 1；
Fig. 8 is the TEM image of three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite prepared by example 1；
Fig. 9 is the CV (cyclic voltammetric) of three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite prepared by example 1
Test curve, sweep speed are 2mV s-1；
Figure 10 is the constant current charge and discharge of three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite prepared by example 1
Electrical testing curve, test current density is 1A/g；Three-dimensional porous nitrogen-doped graphene/hydrogen-oxygen prepared by the present invention is calculated
The specific capacitance for changing nickel composite material is 1844F/g (according to the total Mass Calculation of nitrogen-doped graphene and nickel hydroxide).This explanation
Prepared three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite has excellent chemical property；
Figure 11 is three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite difference current density prepared by example 1
Under specific capacitance numerical value.
The present invention does not address part and is applied to prior art.
Embodiment
The specific embodiment of preparation method of the present invention given below.These embodiments are only used for describing preparation of the present invention in detail
Method, it is not intended to limit the application scope of the claims.
Embodiment 1
(1) nano porous copper is prepared.From the Cu of 100 μ m-thicks30Mn70Alloy foil sheet, and it is cut into 1 × 1cm2Greatly
It is small；Then alloy foil sheet is immersed in 0.05M hydrochloric acid solution, carries out removal alloying at room temperature 40 minutes, by paper tinsel after terminating
Piece uses deionized water and alcohol washes successively, is then placed in vacuum drying chamber and dries 2 hours, obtains nano porous copper.
(2) three-dimensional porous nitrogen-doped graphene is prepared.Obtained nano porous copper is put into quartz boat, then equipped with
The quartz boat of nano porous copper is placed in reaction tube burner hearth perimeter, is first passed through argon gas and hydrogen, wherein, argon gas, hydrogen ratio
By 500:200 flow configuration, now rises to 900 DEG C by furnace temperature；Quartz boat is quickly moved to after furnace temperature rises to assigned temperature
Flat-temperature zone in the middle part of reaction tube, calcine at this temperature 2 minutes, then lead to acetylene, ammonia, hydrogen, argon gas again, ratio presses 50:
30:500:200 flow configuration, is calcined 3 minutes on this condition；It is after calcining that quartz boat is quickly permanent from reaction tube middle part
Warm area is moved to outside burner hearth, and sample is quickly down into room temperature under the atmosphere of argon gas, then takes out sample from tube furnace, and
Shut stove and gas circuit；Then it is 10g ferric trichloride+10ml hydrochloric acid+100ml water the nano porous copper of burning-out to be immersed into proportioning
Corrosive liquid in, etching time is 18 hours, removes the copper mold plate of the inside, then by obtained sample successively with deionized water and
Alcohol washes, the then three-dimensional porous nitrogen-doped graphene film of drying to obtain self-supporting.
(3) three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite is prepared.The water nickel chlorides of 0.594g six are weighed to be put into
It is sufficiently stirred to obtain nickel chloride aqueous solution in 40mL water, then weighs 1.2g urea and be equally put into 40mL water and be sufficiently stirred to obtain
Aqueous solution of urea, nickel chloride and aqueous solution of urea are then mixed into the simultaneously 30 minutes liquid that is uniformly mixed of magnetic agitation, by gained
Nickel chloride and urea the mixed liquor polytetrafluoroethyllining lining that is transferred to 100ml stainless steel cauldron in；Then by step 2
Obtained three-dimensional porous nitrogen-doped graphene film is also placed in the stainless steel cauldron of above-mentioned polytetrafluoroethyllining lining, static
2 hours；It is then placed in vacuum drying chamber and is heated to 90 DEG C, is incubated 8 hours, question response kettle is cooled to room temperature, by reactor
Self-supporting film in lining takes out and is cleared up and dried with deionized water and alcohol successively, that is, obtains three-dimensional porous N doping graphite
Alkene/nickel hydroxide composite.
(4) the electrochemical capacitance performance of the prepared three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite of test.It is three-dimensional
Three electrode tests of porous nitrogen-doped graphene/nickel hydroxide composite electrochemical capacitance performance are carried out in the 6M KOH aqueous solution,
Wherein platinized platinum and Hg/HgO electrodes is respectively as to electrode and reference electrode.
The pore structure of three-dimensional insertion, its hole be present in prepared three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite
Footpath is in 1-2 μ ms, and the length of nickel hydroxide nano pin is in the range of 100-300nm.
Embodiment 2
As different from Example 1：(2) three-dimensional porous nitrogen-doped graphene is prepared.Obtained nano porous copper is put into
In quartz boat, the quartz boat equipped with nano porous copper is then placed in reaction tube burner hearth perimeter, is passed through acetylene, ammonia, hydrogen
Gas, argon gas, ratio press 50:30:500:200 flow configuration, now rises to 900 DEG C by furnace temperature；Treat that furnace temperature rises to assigned temperature
Quartz boat is quickly moved to flat-temperature zone in the middle part of reaction tube afterwards, calcined 3 minutes at this temperature, it is after calcining that quartz boat is quick
Flat-temperature zone is moved to outside burner hearth in the middle part of the reaction tube, and sample is quickly down into room temperature under the atmosphere of argon gas, then by sample from
Taken out in tube furnace, and shut stove and gas circuit；Then by the nano porous copper of burning-out immerse proportioning for 10g ferric trichlorides+
In the corrosive liquid of 10ml hydrochloric acid+100ml water, etching time is 24 hours, removes the copper mold plate of the inside, the sample that will then obtain
Product use deionized water and alcohol washes successively, then the three-dimensional porous nitrogen-doped graphene film of drying to obtain self-supporting.Remaining
With embodiment 1, repeat no more here.
Prepared three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite is compared with example 1 obtains, three-dimensional insertion
Pore structure it is smaller, its aperture is in the range of 300-600nm.
Embodiment 3
As different from Example 1：(3) three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite is prepared.Weigh
The water nickel chlorides of 0.594g six, which are put into 40mL water, to be sufficiently stirred to obtain nickel chloride aqueous solution, then is weighed 1.2g urea and be equally put into
It is sufficiently stirred to obtain aqueous solution of urea in 40mL water, nickel chloride and aqueous solution of urea is then mixed into simultaneously magnetic agitation 30 minutes
Be uniformly mixed liquid, the mixed liquor of the nickel chloride of gained and urea is transferred to 100ml polytetrafluoroethyllining lining it is stainless
In steel reactor；Then the three-dimensional porous nitrogen-doped graphene film obtained by step 2 is also placed in above-mentioned polytetrafluoroethylene (PTFE)
In the stainless steel cauldron of lining, static 2 hours；It is then placed in vacuum drying chamber and is heated to 90 DEG C, is incubated 12 hours, kettle to be answered
Room temperature is cooled to, the self-supporting film in inner liner of reaction kettle is cleared up and dried with deionized water and alcohol successively, produces three-dimensional
Porous nitrogen-doped graphene/nickel hydroxide composite.Remaining is repeated no more here with embodiment 1.
Compared to example 1, nickel hydroxide institute accounting in prepared three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite
Example is higher, and the length of nickel hydroxide nano pin is longer.
Embodiment 4
As different from Example 1：(3) three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite is prepared.Weigh
The water nickel chlorides of 0.594g six, which are put into 40mL water, to be sufficiently stirred to obtain nickel chloride aqueous solution, then is weighed 0.6g urea and be equally put into
It is sufficiently stirred to obtain aqueous solution of urea in 40mL water, nickel chloride and aqueous solution of urea is then mixed into simultaneously magnetic agitation 30 minutes
Be uniformly mixed liquid, the liquid that the nickel chloride of gained and urea mix is transferred to 100ml polytetrafluoroethyllining lining it is stainless
In steel reactor；Then the three-dimensional porous nitrogen-doped graphene film obtained by step 2 is also placed in above-mentioned polytetrafluoroethyllining lining
Stainless steel cauldron in, static 2 hours, be then placed in vacuum drying chamber and be heated to 90 DEG C, be incubated 8 hours, kettle to be answered is cold
But to room temperature, the self-supporting film in inner liner of reaction kettle is cleared up and dried with deionized water and alcohol successively, it is more to produce three-dimensional
Hole nitrogen-doped graphene/nickel hydroxide composite.Remaining is repeated no more here with embodiment 1.
Prepared three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite is similar to the appearance structure that example 1 obtains.
Claims (1)
1. a kind of three-dimensional porous nitrogen-doped graphene/nickel hydroxide electrode material preparation method, including the steps：
1) nano porous copper is prepared
The alloy foil sheet of 80~120 μ m-thicks is prepared, wherein Cu, Mn atom number percentage is respectively 30% and 70%, at room temperature
Alloy foil sheet is placed in 0.01-0.3M hydrochloric acid weak solutions, 20-120 minutes are handled using the method for the de- alloy of chemistry；It will be made
Nano porous copper first cleaned with deionized water, then with washes of absolute alcohol, then by the nanoporous copper foil room temperature of cleaning
Under be dried in vacuo.
2) three-dimensional porous nitrogen-doped graphene is prepared
Nano porous copper made from step 1 is put into quartz boat, the quartz boat equipped with nano porous copper is placed in reaction pipe furnace
Thorax perimeter；Argon gas and hydrogen are first passed through, wherein, argon gas, hydrogen ratio press 500:200 flow configuration, now by furnace temperature
700-1000 DEG C is risen to, quartz boat is quickly moved to flat-temperature zone in the middle part of reaction tube after furnace temperature rises to assigned temperature, in this temperature
Lower calcining 1-3 minutes；Then 1-50 is pressed again:5-50:500:200 flow proportional is passed through acetylene, ammonia, hydrogen, argon gas, herein
Under the conditions of calcine 1-5 minutes；Quartz boat is quickly moved to outside burner hearth from flat-temperature zone in the middle part of reaction tube after calcining, in argon gas
Atmosphere under sample is quickly down to room temperature, then sample is taken out from tube furnace；Then the nano porous copper that will have been calcined
It is 10g to immerse proportioning：10ml：In the corrosive liquid of 100ml iron chloride, hydrochloric acid and water, etching time is 10~24 hours, is removed
The copper mold plate of the inside；It is then that obtained sample is clean with deionized water and alcohol washes successively, then dry and can obtain certainly
Support three-dimensional porous nitrogen-doped graphene film.
3) three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite is prepared
By six water nickel chlorides, urea and water according to 0.5-0.7g：1.1-1.3g：Nickel salt is made in 70-90mL proportioning and urea mixes
Solution 70~90ml altogether is closed, in the reactor for the polytetrafluoroethyllining lining that mixed solution is transferred to；Then by step 2) institute
The three-dimensional porous nitrogen-doped graphene film obtained is also placed in reactor, static 1~3 hour, is then placed in vacuum drying chamber
70~120 DEG C are heated to, is reacted 4~20 hours, question response kettle is cooled to room temperature, and the self-supporting film in inner liner of reaction kettle is taken
Go out, and produce three-dimensional porous nitrogen-doped graphene/nickel hydroxide composite with deionized water and alcohol cleaning drying successively,
To prepare electrochemical capacitance electrode.
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| CN108751169A (en) * | 2018-06-08 | 2018-11-06 | 天津大学 | Preparation method for in-situ synthesis of three-dimensional nano-porous graphene-coated metal oxide/hydroxide/sulfide composite material |
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