CN104599863B - A kind of method for preparing composite, composite and its application - Google Patents
A kind of method for preparing composite, composite and its application Download PDFInfo
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- CN104599863B CN104599863B CN201510021386.9A CN201510021386A CN104599863B CN 104599863 B CN104599863 B CN 104599863B CN 201510021386 A CN201510021386 A CN 201510021386A CN 104599863 B CN104599863 B CN 104599863B
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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 provides a kind of method for preparing composite, comprises the following steps：There is provided the foamy graphite with three-dimensional porous structure by S1；S2, the foamy graphite is added in potassium hydroxide solution and activated, and washing obtains activating foamy graphite after drying；S3, the activation foamy graphite is added in nitration mixture and is acidified under ultrasound, washing obtains being acidified foamy graphite after drying；And S4, the acidifying foamy graphite is added in nickel sulfate solution and is mixed to form unit for uniform suspension, precipitating reagent is slowly dropped in the suspension, washing is dried to obtain the composite of foamy graphite and nickel hydroxide nano line after hydro-thermal process.The present invention also provides a kind of thus obtained composite and the composite on the capacitor as the application of electrode material.In a word, the method route for preparing composite of the invention is simple, easily controllable, is conducive to large-scale production, and the composite provided has larger specific capacitance and excellent cyclical stability as electrode material.
Description
Technical field
The present invention relates to a kind of material, relate more specifically to a kind of method for preparing composite, composite and its answer
With.
Background technology
As climate warming and environmental pollution increasingly sharpen, people are gradually sought for reproducible outside fossil energy
New energy, such as solar energy, wind energy and biological energy source, this also just turns into global study hotspot.High performance energy storage device is then
It is that human society effectively utilizes the premise of these reproducible new energy, thus receives much concern.
Ultracapacitor has higher energy density as a kind of new energy-storage travelling wave tube compared with traditional capacitor,
There is higher power density compared with conventional batteries, while also having short charging interval, long service life and maintenance cost low
The advantages of, application prospect is very wide.
It is different according to the principle that ultracapacitor stores energy, it can be divided into three classes：Based on porous carbon electrode and electrolyte
The double layer capacitor of interfacial electric double layer energy storage, the redox reaction energy storage based on metal oxide and conductive polymer surfaces
Faradic pseudo-capacitor, and the mixed capacitor that said two devices have concurrently.Being commonly used for the electrode material of ultracapacitor includes
Carbon material and metal oxide.But, carbon material is relatively low as the specific capacitance of electrode material, and metal oxide is used as electrode material
The less stable of material.
The content of the invention
The present invention is intended to provide a kind of method for preparing composite, the composite obtained by this method is while have
Higher specific capacitance and preferable stability.
The present invention provides a kind of method for preparing composite, comprises the following steps：There is provided with three-dimensional porous structure by S1
Foamy graphite；S2, the foamy graphite is added in potassium hydroxide solution and activated, and washing obtains activation bubble after drying
Foam graphite；S3, the activation foamy graphite is added in nitration mixture and is acidified under ultrasound, washing obtains acidifying bubble after drying
Foam graphite；And S4, the acidifying foamy graphite is added in nickel sulfate solution and is mixed to form unit for uniform suspension, by precipitating reagent
It is slowly dropped in the suspension, washing is dried to obtain the composite wood of foamy graphite and nickel hydroxide nano line after hydro-thermal process
Material.
In the present invention, foamy graphite is a kind of graphited porous carbon materials, with satisfactory electrical conductivity and high-ratio surface
Product, it is applied to ultracapacitor as electrode material to realize energy using the interfacial electric double layer formed between electrode and electrolyte
Storage, does not occur electrochemical reaction, therefore with good cyclical stability.But, foamy graphite is found its single electrode ratio
Electric capacity is relatively low, it is impossible to provide high-energy-density.Nickel hydroxide is a kind of potential electrode material, with cheap, chemistry
Redox characteristic is stable, the advantage such as theoretical specific capacitance height.But, it is poor that nickel hydroxide is found its cycle performance.The present invention
The nano thread structure of the monodimension nanometer material, i.e. nickel hydroxide of nickel hydroxide is selected, it can effectively be prevented in charge and discharge process
The reunion of nickel hydroxide, alleviates the expansion of volume electrode material, maintains the stability of material, in addition, during charge and discharge cycles,
This one-dimensional nano structure make it that in transverse direction (diameter) and longitudinal direction (length) both direction small change occurs for nickel hydroxide, has
The stress produced beneficial to release, makes material obtain more preferable structural stability in cyclic process.The present invention is by with higher
The nickel hydroxide nano line of structural stability, is combined into three-dimensional porous structure with the porous foam graphite of high-specific surface area
Composite, makes full use of both respective advantages and its synergistic function, obtains a kind of with high specific capacitance and excellent
The electrode material for super capacitor of cyclical stability.
The step S1 includes：The sucrose and ammonium chloride mixed in tubular type kiln roasting, so as to provide the foamy graphite.
It should be understood that preparing foamy graphite by other means is used in the present invention be also feasible, as long as the foamy graphite provided
With three-dimensional porous structure.
The mol ratio of the sucrose and ammonium chloride is 0.5-2.5, and sintering temperature is 1000-1500 DEG C.In this step, sugarcane
Sugar is carbonized to form foamy graphite by high-temperature roasting.Preferably, the roasting process is carried out 2-5 hours under an argon atmosphere.
In the step S2, the mass ratio of the foamy graphite and the potassium hydroxide is 0.1-1, preferably 0.1-0.5.
It should be understood that in this step, the foamy graphite and potassium hydroxide of other ratios are also feasible, as long as being capable of pore-creating and increase
Specific surface area.The concentration of the potassium hydroxide solution is 5-10mol/L.Preferably, activation process progress 10-30 is small
When.
In the step S3, the nitration mixture is sulfuric acid and nitric acid, wherein, the volume ratio of sulfuric acid and nitric acid is 3:1-1:3.
It should be understood that in this step, other nitration mixture are also feasible, as long as oxygen-containing functional group can be introduced, so as to increase hydrogen-oxygen
Change the attachment position of nickel nano wire.Preferably, the acidization is carried out 2-5 hours.
In the step S4, the precipitating reagent is nickel hydroxide, NaOH or urea.It should be understood that other energy
Precipitating reagent hydroxy is enough provided to can be also used in the present invention.
In the step S4, precipitating reagent is slowly dropped in the suspension with vigorous stirring.It is violent by this
Stirring so that precipitating reagent is uniformly mixed with nickel sulfate and reacted.
In the step S4, the mass ratio of the acidifying foamy graphite and the nickel sulfate is 0.02-0.1.Preferably,
The mass ratio of the acidifying foamy graphite and the nickel sulfate is 0.03-0.82.
The mol ratio of the nickel sulfate and the precipitating reagent is 1-3.It should be understood that in this step, the sulphur of other ratios
Sour nickel and precipitating reagent are also feasible, as long as ensuring the hydroxyl reaction of nickel sulfate and precipitating reagent release, so that in acidifying foam
The Surface Creation nickel hydroxide of graphite.Preferably, the mass ratio of nickel sulfate and NaOH is 1.By substantial amounts of experiment,
It has been found that selection NaOH is precipitated more preferable than the effect that selection urea is precipitated, although urea is at high temperature
Decomposition can produce hydroxyl, but application can not be met by precipitating obtained composite by urea progress in certain embodiments
It is required that.It should be understood that it is appropriate preferred by being carried out to urea as the technological parameter of precipitating reagent, the work of optimization can be still provided
For the composite of electrode material.
The hydrothermal temperature is 100-180 DEG C.It should be understood that it is also feasible that other temperature, which carry out hydro-thermal reaction, as long as
Nickel hydroxide is enabled to form nano thread structure in water heating kettle.More specifically, by control the hydrothermal temperature and
Compactedness can adjust the diameter of formed nano wire.Preferably, the diameter of the nano wire formed is between 20-40nm.
The present invention also provides a kind of composite prepared according to the above method, and the composite is foamy graphite
With the composite of nickel hydroxide nano line.In the composite, nickel hydroxide is attached to foam stone in the form of nano wire
The surface of ink.
The present invention also provides above-mentioned composite on the capacitor as the application of electrode material.Pass through experiment, applicant
It was found that, the composite has higher specific capacitance and preferable stability simultaneously.
The mass percent of nickel hydroxide in the composite is 30-85%.
The initial feed for preparing composite of the present invention is the foamy graphite with three-dimensional porous structure, is particularly passed through
The activation foamy graphite obtained after activation step, it has larger specific surface area and more pore structure, wherein, this compares surface
Product is conducive to the attachment of nickel hydroxide nano line, so that the utilization rate of electrode material is improved, and the pore structure is conducive to electrolyte
Transmission.In addition, the method for preparing composite of the present invention includes in the solution mixing acidifying foamy graphite and nickel sulfate
Suspension is formed, then precipitating reagent is slowly dropped to the step of producing precipitation in the mixed solution under agitation so that hydrogen-oxygen
Change nickel homogeneous nucleation on foamy graphite, so that finally ensure that the nano wire of hydro-thermal formation is evenly distributed in foamy graphite, shape
Into complex three-dimensional structures.In a word, the method route for preparing composite of the invention is simple, easily controllable, is conducive to extensive
Production, and the composite provided has larger specific capacitance and excellent cyclical stability.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of the composite according to the present invention；
Fig. 2 a are the scanning electron microscopies of the activation foamy graphite according to the present invention；
Fig. 2 b are the scanning electron microscopies of the composite according to the present invention；
Fig. 2 c are the scanning electron microscopies of the amplification of the nickel hydroxide nano line in composite of the invention；
Fig. 3 a are compared according to the single electrode specific capacitance of the composite, single nickel hydroxide, foamy graphite of the present invention
Figure；And
Fig. 3 b are the cycle performance figure as the single electrode of electrode material according to composite of the invention.
Embodiment
Below in conjunction with the accompanying drawings, presently preferred embodiments of the present invention is provided, and is described in detail.
The mass percent of the nickel hydroxide nano line of embodiment 1 is the preparation of 85% composite
(1) with sucrose and ammonium chloride with mol ratio 1:2 ratio is calcined 2 hours under 1000 DEG C, argon gas atmosphere, is had
There is the foamy graphite of three-dimensional porous structure.
(2) foamy graphite is added in 7mol/L potassium hydroxide solution (in mass ratio 0.1, i.e. potassium hydroxide solution
The quality of potassium hydroxide is 10 times of the quality of foamy graphite) in stirring 4 hours, stand and 20 as a child filtered afterwards, 60 DEG C of dryings
Obtain activating foamy graphite after 24 hours.
(3) (volume ratio is sulfuric acid for activation foamy graphite and nitration mixture:Nitric acid=1:1) 2 hours are acidified under ultrasound, are passed through
Washing obtains being acidified foamy graphite after drying.
(4) acidifying foamy graphite is added in nickel sulfate solution (mass ratio 0.06) and is mixed to form unit for uniform suspension, will
NaOH (nickel sulfate and NaOH mol ratio are 1) solution is slowly dropped in the suspension under agitation, wherein, sulphur
The concentration of sour nickel is 0.06g/mL.Hydro-thermal process 24 hours in water heating kettle are put at 100 DEG C.Finally washing is dried to obtain foam
The composite of graphite and nickel hydroxide nano line.
The X-ray result of the composite is as shown in figure 1, all peak distributions and standard card chip value (JCPDS No.41-
1424) fit like a glove, it was demonstrated that obtained nickel hydroxide nano line is α-(NiOH)2,Its cell parameter is calculated for a=
0.81067nm, b=0.29520nm c=1.37165nm.
The preparation of the composite of embodiment 2
(1) with sucrose and ammonium chloride with mol ratio 2.5:1 ratio is calcined 5 hours under 1500 DEG C, argon gas atmosphere, obtains
To the foamy graphite with three-dimensional porous structure.
(2) foamy graphite is added in potassium hydroxide solution stirring 4 hours in (mass ratio 1), stands 20 as a child mistakes afterwards
Filter, 60 DEG C of drying obtain activation foamy graphite after 24 hours.
(3) activation foamy graphite and nitration mixture (sulfuric acid:Nitric acid=3:1) 5 hours are acidified under ultrasound, by washing drying
After obtain be acidified foamy graphite.
(4) the acidifying foamy graphite is added in nickel sulfate solution (mass ratio 0.03) and is mixed to form even suspension
Liquid, maintenance is stirred vigorously is slowly dropped to the suspension by NaOH (nickel sulfate and NaOH mol ratio are 3) solution
In.Hydro-thermal process 24 hours at 180 DEG C.Finally wash dry (drying temperature is 80 DEG C) and obtain foamy graphite and nickel hydroxide
The composite of nano wire.
Stereoscan photograph is as shown in Fig. 2 wherein, and Fig. 2 a, which can be seen that activation foamy graphite, has three-dimensional porous structure,
Fig. 2 b can be seen that foamy graphite and nickel hydroxide weave in, form the structure that loose structure and nano wire run through mutually,
Wherein, some nanowire growths are on the surface of foamy graphite, some nano wire and foamy graphite weave ins, both it is overall and
Speech is uniformly compounded to form composite.Fig. 2 c are the nickel hydroxide nano lines individually amplified, the diameter of nano wire 20-40nm it
Between.
The mass percent of the nickel hydroxide nano line of embodiment 3 is the preparation of 30% composite
(1) with sucrose and ammonium chloride with mol ratio 1:2 ratio is calcined 2 hours under 1500 DEG C, argon gas atmosphere, obtains
Foamy graphite with three-dimensional porous structure.
(2) foamy graphite is added in potassium hydroxide solution stirring 4 hours in (mass ratio 1), stands 20 as a child mistakes afterwards
Filter, 60 DEG C of drying obtain activation foamy graphite after 24 hours.
(3) activation foamy graphite and nitration mixture (sulfuric acid:Nitric acid=3:1) 2 hours are acidified under ultrasound, by washing drying
After obtain be acidified foamy graphite.
(4) the acidifying foamy graphite is added in nickel sulfate solution (mass ratio 0.82) and is mixed to form even suspension
Liquid, NaOH (nickel sulfate and NaOH mol ratio are 1) solution is slowly dropped in the suspension under agitation.
Hydro-thermal process 24 hours at 100 DEG C.Finally washing is dried to obtain the composite of foamy graphite and nickel hydroxide nano line.
The preparation for the composite that embodiment 4 is precipitated using urea
(1) with sucrose and ammonium chloride with mol ratio 2.5:1 ratio is calcined 3 hours under 1300 DEG C, argon gas atmosphere, obtains
To the foamy graphite with three-dimensional porous structure.
(2) foamy graphite is added in potassium hydroxide solution stirring 4 hours in (mass ratio 1), stands 20 as a child mistakes afterwards
Filter, 60 DEG C of drying obtain activation foamy graphite after 24 hours.
(3) activation foamy graphite and nitration mixture (sulfuric acid:Nitric acid=3:1) 5 hours are acidified under ultrasound, by washing drying
After obtain be acidified foamy graphite.
(4) the acidifying foamy graphite is added in nickel sulfate solution (mass ratio 0.06) and is mixed to form even suspension
Liquid, urea (nickel sulfate and urea mol ratio are 1) solution is slowly dropped in the suspension under agitation.At 100 DEG C
Hydro-thermal process 24 hours.Finally washing is dried to obtain the composite of foamy graphite and nickel hydroxide nano line.
Reference examples 1, activation foamy graphite
(1) with sucrose and ammonium chloride with 1:2 ratio is calcined 2 hours under 1000 DEG C, argon gas atmosphere, obtains having three
Tie up the foamy graphite of loose structure.
(2) foamy graphite is added in potassium hydroxide solution stirring 4 hours in (mass ratio 0.1), after standing 20 as a child
Filtering, 60 DEG C of drying obtain activation foamy graphite after 24 hours.
Reference examples 2, nickel hydroxide nano line
Sodium hydroxide solution is slowly dropped in nickel sulfate solution under agitation.Hydro-thermal process 24 hours at 100 DEG C.
Finally washing is dried to obtain nickel hydroxide nano line.
Application examples
By the embodiment 1-4 and reference examples 1-2 products prepared and superconduction carbon, PTFE according to 80：15：5 ratio mixing is equal
It is even, it is coated onto in nickel foam, compressing tablet obtains working electrode after drying.Capacity measurement uses three-electrode system, and active material is work
Electrode, Pt electrodes are as to electrode, Hg-Hg2Cl2Electrode carries out constant current charge-discharge as reference electrode in 6M KOH solutions
Test, arrives electrode specific capacitance after calculating, the results are shown in Table 1.
Table 1
Mass percent of the nickel hydroxide nano line-foamy graphite of the invention in nickel hydroxide as shown in Table 1
(30-85%) has higher specific capacitance and a good cyclical stability when higher, nickel hydroxide nano line and foamy graphite this
Both combinations have given full play to both advantages.In the range of above-mentioned 30-85%, with the foam stone as carbon material
The rise of the mass percent of ink, cyclical stability is increased.And NaOH as precipitating reagent when obtained product
It is more preferable during than urea as precipitating reagent.
In addition, composite of the applicant by the mass percent of substantial amounts of different nickel hydroxides, utilizes different acidifyings
Time is contrasted, and when the mass percent for finding nickel hydroxide is 85%, specific capacitance is higher, and stability is also good.
In one of embodiment, although higher as specific capacity when precipitating reagent with urea, the less stable of circulation should
The composite that embodiment is provided can not be applied effectively.Fig. 3 gives the specific capacitance and cyclical stability of embodiment 1, from figure
As can be seen that the specific capacitance of the composite of the present invention illustrates theirs apparently higher than single nickel hydroxide and foamy graphite
It is compound to improve the performance of material, can also retain 90% after the cyclical stability of material 3000 times in addition, be have it is good
The electrode material of application prospect.
In summary, nickel hydroxide nano of the invention line-foamy graphite composite has higher specific surface area, compared with
Many pore passage structures, and the nano wire pattern of nickel hydroxide can be greatly enhanced the electrical property and stability of material.And
Last handling process is simple, can be with large-scale application in follow-up commercial Application and industrial amplification process.
Above-described, only presently preferred embodiments of the present invention is not limited to the scope of the present invention, of the invention is upper
Stating embodiment can also make a variety of changes.What i.e. every claims and description according to the present patent application were made
Simply, equivalence changes and modification, fall within the claims of patent of the present invention.Of the invention not detailed description is
Routine techniques content.
Claims (9)
1. a kind of method for preparing composite, it is characterised in that the described method comprises the following steps：
S1, there is provided the foamy graphite with three-dimensional porous structure for the sucrose and ammonium chloride mixed in tubular type kiln roasting；
S2, the foamy graphite is added to pore-creating and the activation of increase specific surface area is carried out in potassium hydroxide solution, and washing is dry
Obtain activating foamy graphite after dry；
S3, the activation foamy graphite is added in nitration mixture and is acidified under ultrasound to introduce oxygen-containing functional group, so as to increase
The attachment position of nickel oxide nanowires is hydrogenated with, washing obtains being acidified foamy graphite after drying；And
S4, the acidifying foamy graphite is added in nickel sulfate solution and is mixed to form unit for uniform suspension, it will thus provide be hydroxy
Precipitating reagent is slowly dropped in the suspension so that the hydroxyl reaction of nickel sulfate and precipitating reagent release, so that in acidifying bubble
The Surface Creation nickel hydroxide of foam graphite, 100-180 DEG C of hydro-thermal process causes nickel hydroxide formation nano thread structure, is washed out
It is dried to obtain the composite of foamy graphite and nickel hydroxide nano line.
2. according to the method described in claim 1, it is characterised in that in the step S4, the precipitating reagent be nickel hydroxide,
NaOH or urea.
3. according to the method described in claim 1, it is characterised in that in the step S4, with vigorous stirring by precipitating reagent
It is slowly dropped in the suspension.
4. according to the method described in claim 1, it is characterised in that in the step S4, the acidifying foamy graphite and institute
The mass ratio for stating nickel sulfate is 0.02-0.1.
5. method according to claim 4, it is characterised in that the mass ratio of the acidifying foamy graphite and the nickel sulfate
For 0.03-0.82.
6. method according to claim 4, it is characterised in that the mol ratio of the nickel sulfate and the precipitating reagent is 1-3.
7. a kind of composite that method according to any one of the claims is prepared, it is characterised in that institute
It is foamy graphite and the composite of nickel hydroxide nano line to state composite.
8. a kind of composite according to claim 7 is on the capacitor as the application of electrode material.
9. application according to claim 8, it is characterised in that the mass percent of the nickel hydroxide in the composite
For 30-85%.
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| CN106920962A (en) * | 2017-04-25 | 2017-07-04 | 华南理工大学 | A kind of nickel oxide/graphite composite nano materials for lithium ion battery and preparation method and application |
| CN114875430A (en) * | 2022-04-19 | 2022-08-09 | 中国科学院过程工程研究所 | Graphite-based bifunctional electrosynthesis hydrogen peroxide catalytic material and preparation method thereof |
| CN115974114B (en) * | 2023-03-18 | 2023-07-14 | 河北坤天新能源股份有限公司 | Quick-charging graphite composite material and preparation method thereof |
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| CN101049928B (en) * | 2006-04-04 | 2010-05-12 | 中国矿业大学(北京) | Method for manufacturing high heat conducting foam material of graphite with even apertures |
| CN104098083A (en) * | 2014-07-15 | 2014-10-15 | 黑龙江大学 | Method for preparing porous nano carbon materials with biomass serving as carbon source |
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| CN102142541A (en) * | 2011-02-25 | 2011-08-03 | 浙江大学 | High capacity and stable cyclic performance lithium ion battery electrode and preparation method thereof |
| CN102683040A (en) * | 2012-05-16 | 2012-09-19 | 浙江大学 | Preparation method for graphene/alpha nickel hydroxide nanometer compound material |
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