CN106571245A - Method for producing expanded graphite carbon nanotube composite material and supercapacitor produced from expanded graphite carbon nanotube composite material - Google Patents
Method for producing expanded graphite carbon nanotube composite material and supercapacitor produced from expanded graphite carbon nanotube composite material Download PDFInfo
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- CN106571245A CN106571245A CN201510651429.1A CN201510651429A CN106571245A CN 106571245 A CN106571245 A CN 106571245A CN 201510651429 A CN201510651429 A CN 201510651429A CN 106571245 A CN106571245 A CN 106571245A
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- expanded graphite
- graphite carbon
- nano tube
- carbon nano
- compound material
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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 invention discloses a method for producing an expanded graphite carbon nanotube composite material. The method comprises: 1) heating expandable graphite in an inert gas to obtain expanded graphite; 2) immersing the expanded graphite in a nickel chloride solution; 3) thoroughly removing water from the expanded graphite subjected to the step 2) in a vacuum environment and then transferring the expanded graphite to a vacuum tubular furnace, and exhausting air; 4) inputting the reduction nickel catalyst while heating the tubular furnace, and after the temperature of the tubular furnace reaches the preset temperature, inputting carbon growth source and maintaining the state for a growth period; 5) closing the reduction nickel catalyst and the inputting of the carbon growth source, and obtaining the expanded graphite carbon nanotube composite material through cooling. The present invention also provides a supercapacitor made of the expanded graphite carbon nanotube composite material. The expanded graphite carbon nanotube composite material obtained by the manufacturing method of the invention is effectively increased in specific surface area and charge storage space and low in production cost. The method is simple and adapts to large-scale production and market application.
Description
Technical field
The present invention relates to a kind of manufacture method of expanded graphite carbon nano tube compound material, further relates to a kind of expanded graphite carbon
The automobile-used super capacitor of nanometer tube composite materials manufacture.
Background technology
Hybrid vehicle due to waste gas discharge is few, the low advantage of use cost, in environmental protection and energy scarcity
Increasingly rise under background.One of key technology of hybrid vehicle is its energy storage device.Ultracapacitor is used as between biography
Novel energy storage apparatus between system capacitor and traditional storage battery, its Capacity Ratio traditional capacitor is big 20～200 times, power
Density ratio traditional storage battery battery is big 10～100 times, with excellent charge-discharge performance and the circulation of up to more than 1000 times
Service life, can be applicable to the aspects such as Brake energy recovery, electric motor starting and the accessory power supply of hybrid vehicle, have
Vast potential for future development.
The performance of ultracapacitor is relevant with electrode material, electrolyte and its barrier film for using, and electrode material is wherein most
Main factor, because it is the important base of ultracapacitor.Ultracapacitor is using high-specific surface area material with carbon element or gold
The materials such as category oxide do electrode.It is based on carbon electrode/electricity using the ultracapacitor of material with carbon element according to its Storage mechanism
Solution liquid interface charge separates produced electric double layer storing charge.Thus, electrode material for electric double layer capacitor should have profit
In the high-ratio surface and the pore structure for being easy to electrolyte wetting and ion quickly to move of charge accumulated.CNT is used as new
Nano material, by unique conjugated structure, possesses the performances such as the electron transport property and excellent thermal conductivity, optics of uniqueness,
There is huge application potential in fields such as the energy, electronic device, batteries.
At present preparation method of carbon nano-tube is more ripe, is realized based on the electronic device of CNT, composite etc.
Industrialization.Research shows that the porosity of CNT is up to 99.6%, and its density is 0.01～0.02g/cm3, far below can
The same Graphene frequently as energy storage device electrode.The correlative study work of Graphene is very popular at present, at present success
Prepare Graphene/carbon nanotube composite material to make electrode and measure its specific capacitance for 112F/g, using PEI redox systems
Standby Graphene/carbon nanotube composite material makees electrode and measures its specific capacitance for 120F/g, and with CNT 40% mass is accounted for
Ratio composite graphite alkene simultaneously measures its specific capacitance for 87F/g.But at present Graphene preparation process it is unstable, it is easy reunite,
Still it is unsuitable for industrialized production, and price is of a relatively high, limits its market application foreground.
Expanded graphite, with huge specific surface area and excellent face internal conductance rate, is prepared as three-dimensional porous material with carbon element
Method is ripe, has a wide range of applications in fields such as battery filler, heat conduction, lubrications.Answering for expanded graphite is based in recent years
Condensation material causes people more and more to pay close attention to.Expanded graphite composite carbon nanometer tube be it is a kind of raising material overall performance can
Row method.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of expanded graphite CNT with three-dimensional porous composite construction
Method for composite material.Present invention also offers a kind of car manufactured using the expanded graphite carbon nano tube compound material
Use super capacitor.
To solve above-mentioned technical problem, the manufacture method of the expanded graphite carbon nano tube compound material that the present invention is provided, its spy
Levying is, comprises the following steps：
1) in an inert atmosphere by expansible graphite heating acquisition expanded graphite；Inert gas is referred in normal temperature and pressure
Under, they are all the monoatomic gases of colorless and odorless, it is difficult to carry out chemical reaction.For example, helium (He), neon (Ne),
Argon (Ar), krypton (Kr), xenon (Xe) and the radioactive radon (Rn) of tool.
2) by step 1) obtain expanded graphite be immersed in nickel chloride solution absorption chlorination nickel particle；
3) by Jing step 2) obtain expanded graphite thoroughly remove moisture removal in vacuum environment after be transferred in vacuum tube furnace
And exclude air；
4) to input reduction Raney nickel while diamond heating, tubular type furnace temperature reaches and be input into again after preset temperature carbon
Growth source is simultaneously kept for the state continued propagation period；
5) reduction Raney nickel and the input of carbon growth source are closed, cooling obtains expanded graphite carbon nano tube compound material.
Wherein, implementation steps 1) when, the inert gas environment flow is 6 × 10-3m3/s-9×10-3m3/ s, heating
Continue more than 20 minutes as 850 DEG C -950 DEG C.
Preferably, the inert gas environment is argon gas, and argon flow amount is 8.33 × 10-3m3/ s, heats as 900 DEG C.
Wherein, implementation steps 2) when, the concentration of nickel chloride solution is 0.01mg/mL-0.03mg/mL, the duration
It is more than or equal to 2 hours.
Preferably, the concentration of nickel chloride solution is 0.02mg/mL.
Wherein, implementation steps 3) when, go moisture removal to be dried more than or equal to 12 using the vacuum environment at 50 DEG C -70 DEG C
Hour, exclusion air is adopted and is passed through flow for 2 × 10-2m3/s-3×10-2m3The inert gas of/s.
Preferably, moisture removal is gone to be dried using the vacuum environment at 60 DEG C, exclusion air is adopted and is passed through flow for 2.67 × 10-2
m3The argon gas of/s.
Wherein, implementation steps 4) when, reduction Raney nickel is hydrogen, and hydrogen flowing quantity is into 5.5 × 10-3m3/s-7.5×10-3
m3/ s, preset temperature is 650 DEG C -750 DEG C, and carbon growth source is acetylene, and acetylene flow is 3 × 10-3m3/s-4×10-3m3/ s,
The growth period is 18-22 minutes.
Preferably, inputting hydrogen flow is 6.67 × 10-3m3/ s, preset temperature is 700 DEG C, and input acetylene flow is
3.33×10-3m3/ s, the growth period is 20 minutes.
A kind of super capacitor that the present invention is provided, makes super using above-mentioned any one expanded graphite carbon nano tube compound material
The electrode of level electric capacity.
What the manufacture method that the present invention is provided solved current hot topic is applied to hybrid vehicle energy storage device super capacitor
Easily there is reunion, the problem of high cost in the Graphene manufacturing process of device.The expansion that manufacture method makes is provided using the present invention
Graphene/carbon nanotube composite makes the ultracapacitor of electrode, and its specific capacitance reaches 150 under 1mV/s sweep speeds
F/g, better than graphene carbon nanotube.When sweep speed reaches 100mV/s, specific capacitance conservation rate reaches and remains to keep
69%, the super capacitor high rate performance of the present invention preferably, is suitably applied high power energy device.Fill for 1000 times simultaneously
After discharge test its specific capacitance conservation rate up to 94% and can keep 96%～99% high charge-discharge efficiencies, with outstanding circulation
Life-span.Compared to CNT and expanded graphite, the expanded graphite carbon nano tube compound material of the present invention is that one kind is combined
The advanced composite material (ACM) of bi-material advantage, contributes to the ultracapacitor developed high-performance, easily manufacture, and by its
It is applied to hybrid vehicle.The expanded graphite carbon nano tube compound material obtained using manufacture method of the present invention is not only effective
The specific surface area and electric charge memory space of ground increase material, and the not defeated outstanding electric property in Graphene is obtained, and
Low manufacture cost, method are simple, it is easy to which large-scale production and market are applied.
Description of the drawings
Below in conjunction with the accompanying drawings the present invention is further detailed explanation with specific embodiment：
Fig. 1 is the schematic flow sheet of manufacture method of the present invention.
Fig. 2 is the effect diagram one that expanded graphite carbon nano tube compound material of the present invention makes super capacitor.
Fig. 3 is the effect diagram two that expanded graphite carbon nano tube compound material of the present invention makes super capacitor.
Fig. 4 is the effect diagram three that expanded graphite carbon nano tube compound material of the present invention makes super capacitor.
Fig. 5 is the effect diagram four that expanded graphite carbon nano tube compound material of the present invention makes super capacitor.
Specific embodiment
As shown in figure 1, the present invention provides a kind of manufacture method of expanded graphite carbon nano tube compound material, including following step
Suddenly：
1) in an inert atmosphere by expansible graphite heating acquisition expanded graphite, the present embodiment is using argon gas as lazy
Property gas (other inert gases are equally applicable), the ar gas environment be 6 × 10-3m3/s-9×10-3m3/ s, is heated to
Continue more than 20 minutes in 850 DEG C -950 DEG C.
Preferably, the ar gas environment is 6 × 10-3m3/s、8.33×10-3m3/ s or 9 × 10-3m3/, heat as 850 DEG C,
900 DEG C or 950 DEG C, continue 20 minutes or more than 20 minutes.
2) by step 1) obtain expanded graphite be immersed in nickel chloride solution absorption chlorination nickel particle, nickel chloride solution
Concentration be 0.01mg/mL-0.03mg/mL, the duration is more than or equal to 2 hours.
Preferably, the concentration of nickel chloride solution is 0.01mg/mL, 0.02mg/mL or 0.03mg/mL, continues 2
Hour or more than 2 hours.
3) by Jing step 2) obtain expanded graphite thoroughly remove moisture removal in vacuum environment after be transferred in vacuum tube furnace
And exclude air；Go moisture removal to be dried more than or equal to 12 hours using the vacuum environment at 50-70 DEG C, exclude air and adopt
With being passed through 2 × 10-2m3/s-3×10-2m3The inert gas of/s.
Preferably, moisture removal is gone to be dried 12 hours using the vacuum environment at 50 DEG C, 60 DEG C or 70 DEG C or more than 12
Hour, exclusion air is adopted and is passed through 2 × 10-2m3/s、2.67×10-2m3/ s or 3 × 10-2m3Argon gas (other of/s
Inert gas is equally applicable).
4) to input reduction Raney nickel while diamond heating, tubular type furnace temperature reaches and be input into again after preset temperature carbon
Growth source is simultaneously kept for the state continued propagation period；Reduction Raney nickel is hydrogen, and hydrogen flowing quantity is into 5.5 × 10-3m3/s
-7.5×10-3m3/ s, preset temperature is 650 DEG C -750 DEG C, and carbon growth source input acetylene flow is 3 × 10-3m3/s
-4×10-3m3/ s, the growth period is 18-22 minutes.
Preferably, it is into 5.5 × 10 to reduce Raney nickel inputting hydrogen flow-3m3/s、6.67×10-3m3/ s or
7.5×10-3m3/ s, preset temperature is 650 DEG C, 700 DEG C or 750 DEG C, and carbon growth source input acetylene flow is 3 × 10-3
m3/s、3.33×10-3m3/ s or 4 × 10-3m3/ s, the growth period is 18 minutes, 20 minutes or 22 minutes.
5) reduction Raney nickel hydrogen and the input of carbon growth source acetylene are closed, cooling obtains expanded graphite CNT and is combined
Material.
A kind of super capacitor, using above-mentioned any one expanded graphite carbon nano tube compound material the electricity of super capacitor is made
Pole.
It is bent that Fig. 2 show cyclic voltammetric of the ultracapacitor based on expanded graphite CNT under different scanning rates
Line, sweep interval is -1V～0V.As seen from the figure, with the increase of sweep speed, cyclic voltammetry curve still keeps preferable
Symmetry, reflect typical electric double layer capacitance feature, illustrate filling under the conditions of the heavy-current discharge ultracapacitor
Discharge process is the physical process of absorption and parsing, with preferable invertibity.
It is the high rate performance curve obtained by cyclic voltammetry curve shown in Fig. 3.In 1mV/s sweep speeds, based on swollen
The specific capacitance of the ultracapacitor of swollen graphene/carbon nanotube is 150F/g；When sweep speed increases to 100mV/s, send out
Raw activation polarization phenomenon, specific capacitance drops to 102.4F/g, but specific capacitance conservation rate is still up to 69%, high rate performance
Do well.In sweep interval 1mV/s～100mV/s, the specific capacitance of composite expanded graphite/CNT is bright
Aobvious is higher than CNT and expanded graphite, illustrates that composite greatly improves specific surface area, enabling the more electricity of storage
Lotus, is the advanced composite material (ACM) for combining CNT and expanded graphite bi-material advantage, is more suitable for ultracapacitor.
It is charging and discharging curve of the ultracapacitor based on expanded graphite CNT under 50mA electric currents shown in Fig. 4.By
Figure is visible, although be not the isosceles triangle of standard, but without obvious voltage jump, illustrates expanded graphite/carbon nanometer
The Ohmic resistance of pipe is relatively low, shows that the material power characteristic is high, and invertibity is preferable, with good capacitance characteristic.In addition
Measure the high level that efficiency for charge-discharge of the expanded graphite/carbon nanotube electrode under different electric currents maintains 96%～99%.As a result
Show, the applicable current range of expanded graphite/CNT extensively, is conducive to being suitable for as the ultracapacitor of electrode
The different loads operating mode of hybrid vehicle.
It is the cyclical stability test chart based on the ultracapacitor of expanded graphite CNT shown in Fig. 5.Fill in 50mA
Under discharge current, composite specific capacitance in front 100 cycle charge discharge electrical testings declines 5.5%, and this is due to discharge and recharge
Irreversible redox reaction in the amount of activated material functional group in process composite so that the knot of material script there is
There is part and change in structure, cause electrolyte to reduce with the effective contact area of electrode material, but this phenomenon can followed necessarily
Tend towards stability after ring number of times.More stable specific capacitance is still kept after 1000 cycle charge-discharges, about 6% is only lost,
Show that expanded graphite/CNT has outstanding stability, there is good cycle life as super capacitor material.
The present invention has been described in detail above by specific embodiment and embodiment, but these are not constituted to this
The restriction of invention.Without departing from the principles of the present invention, those skilled in the art can also make many deformations and change
Enter, these also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of manufacture method of expanded graphite carbon nano tube compound material, is characterized in that, comprise the following steps：
1) in an inert atmosphere by expansible graphite heating acquisition expanded graphite；
2) by step 1) obtain expanded graphite be immersed in nickel chloride solution absorption chlorination nickel particle；
3) by Jing step 2) obtain expanded graphite thoroughly remove moisture removal in vacuum environment after be transferred in vacuum tube furnace
And exclude air；
4) to input reduction Raney nickel while diamond heating, tubular type furnace temperature reaches and be input into again after preset temperature carbon
Growth source is simultaneously kept for the state continued propagation period；
5) reduction Raney nickel and the input of carbon growth source are closed, cooling obtains expanded graphite carbon nano tube compound material.
2. expanded graphite carbon nano tube compound material manufacture method as claimed in claim 1, is characterized in that：Implementation steps
1) when, the inert gas environment flow is 6 × 10-3m3/s-9×10-3m3/ s, heating is held as 850 DEG C -950 DEG C
It is continuous more than 20 minutes.
3. expanded graphite carbon nano tube compound material manufacture method as claimed in claim 2, is characterized in that：Implementation steps
1) when, the inert gas environment is argon gas, and argon flow amount is 8.33 × 10-3m3/ s, heats as 900 DEG C.
4. expanded graphite carbon nano tube compound material manufacture method as claimed in claim 1, is characterized in that：Implementation steps
2) when, the concentration of nickel chloride solution is 0.01mg/mL-0.03mg/mL, and the duration is more than or equal to 2 hours.
5. expanded graphite carbon nano tube compound material manufacture method as claimed in claim 4, is characterized in that：Implementation steps
2) when, the concentration of nickel chloride solution is 0.02mg/mL.
6. expanded graphite carbon nano tube compound material manufacture method as claimed in claim 1, is characterized in that：Implementation steps
3) when, go moisture removal to be dried more than or equal to 12 hours using the vacuum environment at 50 DEG C -70 DEG C, exclude air using logical
Inbound traffics are 2 × 10-2m3/s-3×10-2m3The inert gas of/s.
7. expanded graphite carbon nano tube compound material manufacture method as claimed in claim 6, is characterized in that：Implementation steps
3) when, moisture removal is gone to be dried using the vacuum environment at 60 DEG C, exclusion air is adopted and is passed through flow for 2.67 × 10-2m3/s
Argon gas.
8. expanded graphite carbon nano tube compound material manufacture method as claimed in claim 1, is characterized in that：Implementation steps
4) when, reduction Raney nickel is hydrogen, and hydrogen flowing quantity is into 5.5 × 10-3m3/s-7.5×10-3m3/ s, preset temperature
For 650 DEG C -750 DEG C, carbon growth source is acetylene, and acetylene flow is 3 × 10-3m3/s-4×10-3m3/ s, grows the period
For 18-22 minutes.
9. expanded graphite carbon nano tube compound material manufacture method as claimed in claim 1, is characterized in that：Implementation steps
4) when, inputting hydrogen flow is 6.67 × 10-3m3/ s, preset temperature is 700 DEG C, and input acetylene flow is 3.33 × 10-3
m3/ s, the growth period is 20 minutes.
10. a kind of super capacitor, is characterized in that：Using the expanded graphite carbon nanometer described in claim 1-9 any one
Pipe composite makes the electrode of super capacitor.
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