CN106784729A - Carbide-derived carbon/charcoal composite energy-storage material and preparation method and application - Google Patents
Carbide-derived carbon/charcoal composite energy-storage material and preparation method and application Download PDFInfo
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- CN106784729A CN106784729A CN201710041691.3A CN201710041691A CN106784729A CN 106784729 A CN106784729 A CN 106784729A CN 201710041691 A CN201710041691 A CN 201710041691A CN 106784729 A CN106784729 A CN 106784729A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The present invention provides carbide-derived carbon/charcoal composite energy-storage material and preparation method and application.The preparation method is comprised the following steps：It is 8 by mol ratio:1~1:1 carbon source and metal powder mixing, is put into 3~72h of ball milling in high energy ball mill；Above-mentioned compound is reacted in high temperature process furnances, reaction temperature is 1000~1500 DEG C, and the reaction time is 0.5~6h, is cooled to room temperature, prepares metal carbides/charcoal；Above-mentioned metal carbides/charcoal is placed in tube furnace, 300~900 DEG C are warming up under inert gas shielding, then change the gaseous mixture for being passed through high-purity chlorine or chlorine and hydrogen, 0.5~6h of reaction time；Reaction is passed through inert gas again after terminating, be cooled to room temperature after the chloride remained in removal sample surfaces and space, you can obtain carbide-derived carbon/charcoal composite energy-storage material.The material that the present invention is obtained has that structure-controllable, carbide-derived carbon/charcoal two-phase carbon ratio example is adjustable, specific surface area is big and the features such as interior adjustable, micropore is evenly distributed in a big way.
Description
Technical field
The invention belongs to novel charcoal material field, and in particular to one kind can be used as lithium ion battery negative and ultracapacitor
The carbide-derived carbon of electrode material/charcoal composite energy-storage material and preparation method and application.
Background technology
With the development of society, the strategic core of energy crisis and environmental protection as human kind sustainable development, research is opened
The novel energy material and raising energy conversion and service efficiency of sending out environment-friendly have turned into the hot issue of global concern.Its
In, development high-performance energy storage device and associated materials are to efficiently using the regenerative resources such as wind energy and solar energy, fast-developing electricity
Electrical automobile and intelligent grid have very important effect.Carbon-based material has good structure designability, specific surface high
Long-pending, excellent conductive capability, unique chemical stability, good mouldability, at the same relative low price, raw material sources it is abundant,
Production technology also comparative maturity, is still lithium ion battery and the widest electrode material of supercapacitor applications so far.
Carbide-derived carbon (CDCs) be with carbide lattice as template, by selective etch by metal in carbide or
Nonmetalloid is removed, and by the intact reservation of carbon skeleton, and nano-pore Carbon Materials are obtained.Pore-size distribution is narrow, pore structure is adjustable
It is outstanding advantage that CDCs is different from normal activated carbon, and the focus of structure regulating also exactly CDCs researchs.With pore-size distribution compared with
Activated carbon wide is compared, and on the one hand CDCs avoids makes electrolyte ion be difficult to enter because aperture is too small, on the other hand avoids
Aperture is excessive to cause the decline of density.CDCs materials can fast charging and discharging, its rated capacity was just can reach within several seconds
More than 95%.Density CDCs higher makes electrode have volume and capacity ratio higher.But compared with general lithium ion battery
(120~170Wh/kg), its energy density is still relatively low.Merely using carbide-derived carbon as the super electricity of electrode active material
Although container shows specific volume flow characteristic higher, but similar with traditional activated carbon resistance rod, still relies primarily on derived carbon big
Specific surface area and special pore structure occur physical adsorption process in electrode surface carries out energy storage, and energy density is not high.Simple carbon
Compound derived carbon there is also that coulombic efficiency first is relatively low and the not good problem of cyclical stability as lithium ion battery negative material.
At present the different carbide presoma of selection and reaction bar are concentrated mainly on for the research of carbide-derived carbon
Part, using CO2Activated with KOH etc., introduce the methods such as other templates, surface be modified, specific surface area to carbide-derived carbon and
The structure in hole is regulated and controled.Research is modified mainly for simple derived carbon, it is difficult to fundamentally solve the energy of derived carbon
The low problem of metric density.
The content of the invention
The present invention provides a kind of carbide-derived carbon/charcoal composite energy-storage material and its preparation side to solve above-mentioned technical problem
Method and application, the energy storage material structure-controllable, charcoal/carbide two-phase carbon ratio example is adjustable, specific surface area is greatly and interior in a big way
Adjustable, micropore is evenly distributed.
The object of the invention is realized using following proposal：
The preparation method of carbide-derived carbon/charcoal composite energy-storage material, comprises the following steps：
It is 8 by mol ratio:1~1:1 carbon source and metal powder mixing, is put into 3~72h of ball milling in high energy ball mill；
Above-mentioned compound is reacted in high temperature process furnances, reaction temperature be 1000~1500 DEG C, the reaction time be 0.5~
6h, is cooled to room temperature, prepares metal carbides/charcoal；
Above-mentioned metal carbides/charcoal is placed in tube furnace, 300~900 DEG C is warming up under inert gas shielding, then
Change the gaseous mixture for being passed through high-purity chlorine or chlorine and hydrogen, 0.5~6h of reaction time；
Reaction is passed through inert gas again after terminating, room is cooled to after the chloride remained in removal sample surfaces and space
Temperature, you can obtain carbide-derived carbon/charcoal composite energy-storage material.
In such scheme, described carbon source is appointing in graphite, MCMB, carbon black, CNT or Carbon fibe
Meaning is a kind of.
In such scheme, described metal powder is any one in titanium, zirconium, hafnium, niobium, tantalum, vanadium or molybdenum powder.
In such scheme, the inert gas is nitrogen or argon gas.
In such scheme, it is 10~50mL/min to be passed through high-purity chlorine or chlorine with the flow velocity of the gaseous mixture of hydrogen.
Carbide-derived carbon/carbon composite that described preparation method is prepared is in energy storage lithium ion battery negative
With the application in electrode material for super capacitor.
The application is comprised the following steps：
With above-mentioned carbide-derived carbon/carbon composite as active material, with acetylene black as conductive agent, Kynoar is
Binding agent, wherein active material, conductive agent and binding agent are (70~90) in mass ratio:(5~15):(5~15)；
1-METHYLPYRROLIDONE will be added in the active material, conductive agent and binding agent, on magnetic force heating stirrer
It is well mixed, dried into being coated on Copper Foil after pasty state after slurry；
Punching after compacting, i.e., as the working electrode of lithium ion battery.
Carbide-derived carbon/carbon composite that described preparation method is prepared is in electrode material for super capacitor
Application.
The application is comprised the following steps：
Using above-mentioned carbide-derived carbon/carbon composite as negative electrode active material, with conductive black and polytetrafluoroethylene (PTFE)
By (70~90):(5~15):The mass ratio mixing of (5~15), is placed in agate mortar and grinds, and N- methyl pyrroles are added dropwise thereto
Pyrrolidone, continues to grind；
Slurry is pressed into film-form on twin rollers, drying taking-up is washed into pole piece, weighs the equal pole piece of two tablet qualities,
Pole piece is pressed on shape identical circular shaped foam nickel under 5~10MPa pressure；
Electrolyte is added, simulation ultracapacitor is assembled into.
Beneficial effects of the present invention are：Preparation-obtained carbide-derived carbon/the carbon composite of the present invention has carbon source concurrently
With the carbon structure feature of porous carbide derived carbon, with structure-controllable, carbide-derived carbon/charcoal two-phase carbon ratio example is adjustable, ratio
Surface area is big and the features such as interior adjustable, micropore is evenly distributed in a big way.In the energy storage such as lithium ion battery and ultracapacitor
Wide application prospect is respectively provided with field.
Brief description of the drawings
Fig. 1 is prepared niobium carbide/graphite under the different MCMBs/niobium powder molar ratio in embodiment 1
Change the XRD of MCMB (NbC/GMCMB) presoma.
Fig. 2 is that graphitized intermediate-phase carbon microballoon/niobium powder mol ratio is 2 in embodiment 1:Prepared niobium carbide under the conditions of 1/
The XRD of niobium carbide derived carbon/MCMB (NbC-CDCs/GMCMB) of the MCMB after 800 DEG C of chlorine etchings
Figure.
Fig. 3 is that graphitized intermediate-phase carbon microballoon/niobium powder mol ratio is 2 in embodiment 1:1st, under 800 DEG C of chlorine etching conditions
(a) nitrogen suction/desorption curve and (b) graph of pore diameter distribution of prepared NbC-CDCs/GMCMB.
Fig. 4 is cycle performance figures of the prepared NbC-CDCs/GMCMB in embodiment 1 as lithium ion battery negative.
Fig. 5 is high rate performance figures of the prepared NbC-CDCs/GMCMB in embodiment 1 as lithium ion battery negative.
Fig. 6 is prepared NbC-CDCs/GMCMB in embodiment 1 bent as the constant current charge-discharge of simulation ultracapacitor
Line (current density 0.1A ﹒ g-1)。
Fig. 7 is the XRD of the TiC/CF prepared by embodiment 2.
Fig. 8 is the XRD of the VC/MWCNT prepared by embodiment 3.
Specific embodiment
To make present disclosure, technical scheme and advantage become more apparent, below in conjunction with specific embodiments and the drawings
The present invention is expanded on further, these embodiments are merely to illustrate the present invention, and the present invention is not limited only to following examples.
Embodiment 1
The present invention provides a kind of preparation method of niobium carbide derived carbon/charcoal composite energy-storage material, and it is comprised the following steps：
1) with MCMB (GMCMB) and niobium (Nb) powder as raw material, by different GMCMB/Nb mol ratio=1:1、
2:1、3:1、4:1 ball milling 12h, makes GMCMB and Nb be sufficiently mixed uniformly；
2) above-mentioned compound is placed in high temperature process furnances and reacts 2h at 1400 DEG C, in preparing niobium carbide/graphitization
Between phase carbon microspheres (NbC/GMCMB) composite；
3) above-mentioned niobium carbide/graphitized intermediate-phase carbon microballoon is placed in tube furnace, is risen under the protection of inert atmosphere argon gas
Then temperature changes and is passed through high-purity chlorine (flow velocity is 10~20mL/min) reaction 1h to 800 DEG C；
4) argon gas is passed through after, room temperature is cooled to after four niobium chlorides remained in removal sample surfaces and space, you can
To niobium carbide derived carbon/graphitized intermediate-phase carbon microballoon composite.
X-ray powder diffraction point is carried out to prepared niobium carbide derived carbon/graphitized intermediate-phase carbon microballoon composite
Analysis, high-resolution-ration transmission electric-lens analysis, the material have the architectural feature of MCMB and niobium carbide derived carbon concurrently.Tied by hole
Structure and specific surface area analysis, near 0.6nm, specific surface area is from before etching for the micropore size integrated distribution of composite
1.1m2/ g increases to 347.1m2/ more than g.
With prepared niobium carbide derived carbon/graphitized intermediate-phase carbon microballoon as active material, with acetylene black as conductive agent,
Kynoar is binding agent, is in mass ratio 85 active material, conductive agent and binding agent:5:10, add a certain amount of N-
, be well mixed for three on magnetic force heating stirrer by methyl pyrrolidone, after slurry into being coated on Copper Foil after pasty state, puts into
In vacuum drying chamber, 12h is dried in 60 DEG C, take out and be compacted backlash into the circular pole piece of a diameter of 12mm through twin rollers, as work
Make electrode, with metal lithium sheet be to electrode, Celgard2325 types polypropylene porous film as barrier film, full of high-purity argon gas
CR2016 type button cells are assembled into glove box.
Using prepared composite as negative electrode active material, 8 are pressed with conductive black and PTFE:1:1 mass ratio is mixed
Close, be placed in and 30min is ground in agate mortar, a small amount of 1-METHYLPYRROLIDONE is added dropwise thereto, continue to grind.By slurry right
Film-form is pressed on roller machine, drying is taken out the circular pole piece for being washed into diameter 12mm, weighs the equal pole piece of two tablet qualities,
Pole piece is pressed on the circular shaped foam nickel for being equally washed into diameter 12mm under 10MPa pressure.With 6mol L-1The KOH aqueous solution for electricity
Solution liquid, is assembled into simulation ultracapacitor.
Constant current charge-discharge test is carried out to experimental cell and simulation ultracapacitor using Neware battery test systems,
Prepared material has specific capacity and more preferable high rate performance higher compared with raw graphite MCMB,
During 0.1C, the specific capacity of 800 DEG C of NbC-CDCs@GMCMB-800 of etching preparation is 402.5mAhg after 50 times circulate-1,
Apparently higher than GMCMB (299.9mAhg-1)；The specific capacity of NbC-CDCs@GMCMB-800 is respectively under conditions of 1C and 2C,
236.1mAh·g-1, and 177.7mAhg-1, the specific capacity (123.7mAhg higher than GMCMB-1, and 81.6mAhg-1)。
Embodiment 2
Roughly the same with embodiment 1, difference is that the carbon source that the present embodiment is used is Carbon fibe, and metal powder is titanium
Powder, reaction temperature is 1200 DEG C, and chlorine etching temperature is 600 DEG C, etch period is 2h, specially：
1) with Carbon fibe (CF) and titanium (Ti) powder as raw material, by CF/Ti mol ratio=3:1 ball milling 72h, makes GMCMB and Ti
It is sufficiently mixed uniform；
2) above-mentioned compound is placed in high temperature process furnances and reacts 4h at 1200 DEG C, prepare titanium carbide/Carbon fibe
(TiC/CF) composite；
3) above-mentioned titanium carbide/Carbon fibe is placed in tube furnace, is warming up to 600 DEG C under the protection of inert atmosphere argon gas, so
After change and be passed through high-purity chlorine (flow velocity be 20~30mL/min) reaction 2h；
4) argon gas is passed through after, room temperature is cooled to after the titanium tetrachloride remained in removal sample surfaces and space, you can
To titanium carbide derived carbon/carbon fiber composite；
X-ray powder diffraction analysis, high-resolution are carried out to prepared titanium carbide derived carbon/carbon fiber composite saturating
Electronic microscope photos is penetrated, by pore structure and specific surface area analysis, the micropore size integrated distribution of composite compares table in below 1nm
Area is significantly increased, and pore-size distribution and specific surface area can be adjusted by the mol ratio of feed change Carbon fibe and titanium valve
Control.
With prepared titanium carbide derived carbon/Carbon fibe as active material, with acetylene black as conductive agent, Kynoar is
Binding agent, is 85 active material, conductive agent and binding agent in mass ratio:5:10, a certain amount of 1-METHYLPYRROLIDONE is added,
Three is well mixed on magnetic force heating stirrer, after slurry into being coated on Copper Foil after pasty state, in putting vacuum drying chamber into,
12h is dried in 60 DEG C, is taken out and is compacted backlash into the circular pole piece of a diameter of 12mm through twin rollers, as working electrode, with metal
Lithium piece is that, to electrode, Celgard2325 types polypropylene porous film is assembled into as barrier film in the glove box full of high-purity argon gas
CR2016 type button cells.
Constant current charge-discharge test is carried out to experimental cell using Neware battery test systems, is as a result shown, titanium carbide
Derived carbon/Carbon fibe has more preferably high rate performance compared with raw material Carbon fibe, under higher current density, shows higher
Specific capacity.
Embodiment 3
Roughly the same with embodiment 1, difference is that the carbon source that the present embodiment is used is CNT, and metal powder is
Vanadium powder, reaction temperature is 1300 DEG C, reaction time 5h；The etching gas for using are chlorine and the gaseous mixture of hydrogen, etching temperature
For 700 DEG C, etch period are 1.5h, specially：
1) with CNT (MWCNT) and vanadium (V) powder as raw material, by MWCNT/V mol ratio=5:1 ball milling 72h, makes
MWCNT and V are sufficiently mixed uniformly；
2) above-mentioned compound is placed in high temperature process furnances and reacts 5h at 1300 DEG C, prepare vanadium carbide/CNT
(VC/MWCNT) composite；
3) above-mentioned vanadium carbide/CNT is placed in tube furnace, 700 DEG C is warming up under the protection of inert atmosphere argon gas,
Then gaseous mixture (flow velocity is 30~50mL/min) the reaction 1.5h for being passed through chlorine and hydrogen is changed；
4) argon gas is passed through after, room temperature is cooled to after the vanadium tetrachloride remained in removal sample surfaces and space, you can
To vanadium carbide derived carbon/carbon nano tube compound material；
X-ray powder diffraction analysis, high-resolution are carried out to prepared vanadium carbide derived carbon/carbon nano tube compound material
Transmission electron microscope analysis, by pore structure and specific surface area analysis, the micropore size integrated distribution of composite in below 1nm, than
Surface area is significantly increased, and pore-size distribution and specific surface area can be carried out by the mol ratio of feed change CNT and vanadium powder
Regulation and control.
With prepared vanadium carbide derived carbon/CNT as active material, with acetylene black as conductive agent, Kynoar
It is binding agent, is in mass ratio 85 active material, conductive agent and binding agent:5:10, add a certain amount of N- crassitudes
, be well mixed for three on magnetic force heating stirrer by ketone, after slurry into being coated on Copper Foil after pasty state, puts vacuum drying chamber into
In, 12h is dried in 60 DEG C, take out and be compacted backlash into the circular pole piece of a diameter of 12mm through twin rollers, as working electrode, with gold
Category lithium piece is that, to electrode, Celgard2325 types polypropylene porous film is assembled as barrier film in the glove box full of high-purity argon gas
Into CR2016 type button cells.
Constant current charge-discharge test is carried out to experimental cell using Neware battery test systems, is as a result shown, vanadium carbide
Derived carbon/CNT has more preferably high rate performance compared with raw material CNT, under higher current density, shows more
Specific capacity high.
Claims (9)
1. the preparation method of carbide-derived carbon/charcoal composite energy-storage material, it is characterised in that comprise the following steps：
It is 8 by mol ratio:1~1:1 carbon source and metal powder mixing, is put into 3~72h of ball milling in high energy ball mill；
Above-mentioned compound is reacted in high temperature process furnances, reaction temperature is 1000~1500 DEG C, the reaction time is 0.5~6h,
Room temperature is cooled to, metal carbides/charcoal is prepared；
Above-mentioned metal carbides/charcoal is placed in tube furnace, 300~900 DEG C are warming up under inert gas shielding, then change logical
Enter the gaseous mixture of high-purity chlorine or chlorine and hydrogen, 0.5~6h of reaction time；
Reaction is passed through inert gas again after terminating, room temperature is cooled to after the chloride remained in removal sample surfaces and space,
Can obtain carbide-derived carbon/charcoal composite energy-storage material.
2. preparation method as claimed in claim 1, it is characterised in that described carbon source is graphite, MCMB, charcoal
Any one in black, CNT or Carbon fibe.
3. preparation method as claimed in claim 1, it is characterised in that described metal powder be titanium, zirconium, hafnium, niobium, tantalum, vanadium or
Any one in molybdenum powder.
4. preparation method as claimed in claim 1, it is characterised in that the inert gas is nitrogen or argon gas.
5. preparation method as claimed in claim 1, it is characterised in that be passed through high-purity chlorine or chlorine with the gaseous mixture of hydrogen
Flow velocity is 10~50mL/min.
6. carbide-derived carbon/carbon composite that the preparation method as described in any one of claim 1 to 5 is prepared is in storage
Application in energy lithium ion battery negative and electrode material for super capacitor.
7. application as claimed in claim 6, it is characterised in that it is comprised the following steps：
It is active material with the carbide-derived carbon/carbon composite described in claim 6, with acetylene black as conductive agent, gathers inclined
PVF is binding agent, and wherein active material, conductive agent and binding agent are (70~90) in mass ratio:(5~15):(5~15)；
1-METHYLPYRROLIDONE will be added in the active material, conductive agent and binding agent, in mixing on magnetic force heating stirrer
Uniformly, dried into being coated in after pasty state on Copper Foil after slurry；
Punching after compacting, i.e., as the working electrode of lithium ion battery.
8. carbide-derived carbon/carbon composite that the preparation method as described in any one of claim 1 to 5 is prepared is super
Application in level capacitor electrode material.
9. application as claimed in claim 8, it is characterised in that it is comprised the following steps：
Using the carbide-derived carbon/carbon composite described in claim 6 as negative electrode active material, with conductive black and poly- four
PVF presses (70~90):(5~15):The mass ratio mixing of (5~15), is placed in agate mortar and grinds, and N- is added dropwise thereto
Methyl pyrrolidone, continues to grind；
Slurry is pressed into film-form on twin rollers, drying taking-up is washed into pole piece, weighs the equal pole piece of two tablet qualities, 5~
Pole piece is pressed on shape identical circular shaped foam nickel under 10MPa pressure；Electrolyte is added, simulation ultracapacitor is assembled into.
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Cited By (8)
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| CN107128926A (en) * | 2017-06-28 | 2017-09-05 | 湖南大学 | A kind of preparation method of self-supporting Carbide-derived carbons nano wire |
| CN107394219A (en) * | 2017-07-31 | 2017-11-24 | 中南大学 | A kind of VC/ graphene composite materials and preparation method thereof and the application in lithium-air battery |
| CN107731546A (en) * | 2017-09-29 | 2018-02-23 | 程杰 | A kind of activated carbon electrodes and preparation method thereof |
| CN110422914A (en) * | 2019-08-02 | 2019-11-08 | 重庆大学 | A kind of charcoal base capacitance electrode material and the capacitive electrode using its preparation |
| CN111348941A (en) * | 2020-04-29 | 2020-06-30 | 中国人民解放军国防科技大学 | Carbide-derived carbon/rhenium/iridium coating on surface of C/C composite material and preparation method thereof |
| WO2020254294A1 (en) * | 2019-06-18 | 2020-12-24 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Alkaline metal secondary battery and uses thereof |
| CN113045318A (en) * | 2021-05-11 | 2021-06-29 | 西北工业大学 | Submicron carbide ceramic hollow microsphere and preparation method thereof |
| CN114031076A (en) * | 2021-11-09 | 2022-02-11 | 四川金时新能科技有限公司 | Biomass superstructure carbon, and preparation method and application thereof |
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