CN106024424A - Nickel hydroxide/graphene roll-carbon nano-tube composite carbon aerogel, preparation thereof and application thereof - Google Patents
Nickel hydroxide/graphene roll-carbon nano-tube composite carbon aerogel, preparation thereof and application thereof Download PDFInfo
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- CN106024424A CN106024424A CN201610514756.7A CN201610514756A CN106024424A CN 106024424 A CN106024424 A CN 106024424A CN 201610514756 A CN201610514756 A CN 201610514756A CN 106024424 A CN106024424 A CN 106024424A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01M4/366—Composites as layered products
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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
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to a nickel hydroxide/graphene roll-carbon nano-tube composite carbon aerogel, a preparation thereof and an application thereof. The composite carbon aerogel is composed of a composite carbon aerogel skeleton and a nickel hydroxide nano sheet formed on the surface of the composite carbon aerogel skeleton through the in-situ growth process. The preparation of the composite carbon aerogel comprises the steps of adding a graphene roll-carbon nano-tube composite carbon aerogel into a nickel nitrate solution, subjecting the above materials to deposition reaction in a chemical bath, washing and drying to obtain the composite carbon aerogel. According to the technical scheme of the invention, in the simple chemical and deposition means, the nickel hydroxide having pseudo-capacitive properties is compounded with the graphene roll-carbon nano-tube aerogel having double-electrode-layer capacitance properties, so that the advantages of the nickel hydroxide and the graphene roll-carbon nano-tube aerogel are given full play to. Therefore, the obtained material is excellent in electrochemical performance and high in capacitive character.
Description
Technical field
The invention belongs to composite aerogel and preparation thereof and application, particularly to a kind of nickel hydroxide/graphene roll-CNT
Composite carbon aeroge and preparation thereof and application.
Background technology
Graphene has the monolithic layer two-dimensional structure of uniqueness, and it is by sp2Carbon atom Hexagonal array forms.Meanwhile, Graphene has
Higher inside carrier mobility (200000cm2V-1s-1), good thermal conductivity (～5000W m-1K-1), high printing opacity
Rate (～97.7%) and theoretical specific surface area (2630m2g-1), and the mechanical strength of excellence.CNT has higher load
Stream transport factor, good electric conductivity, high-specific surface area, the performance of the uniquenesses such as big L/D ratio, it is widely used in sensing, storage
The fields such as energy device.Itself and Graphene are mixed aeroge, and carbon nanotube portion is attached on graphene sheet layer, and part is then
It is involved in graphene roll, provides more effective transmission channel for electronics, improve the electric conductivity of material.By simply
Technological design, allow the two prepare that a kind of novel pore size is homogeneous by self assembly, hole is evenly distributed, have simultaneously
There is the carbon aerogels of the high-specific surface area of one-dimensional tubular morphology graphene roll.
Nickel hydroxide nano material has nontoxic, environmental friendliness, easily prepared and catalytic performance good, theoretical specific capacity (2082F g-1)
The fields such as advantages of higher, is widely used in ultracapacitor, lithium ion battery electrode material and become study hotspot.But, hydrogen
Nickel oxide nano material is prone to reunite and limit the performance of its performance.
Summary of the invention
The technical problem to be solved be to provide a kind of nickel hydroxide/graphene roll-carbon nano tube composite carbon aeroge and
Preparation and application, the present invention passes through one-step method growth in situ hydrogen on nickel hydroxide/graphene roll-CNT composite aerogel skeleton
Nickel oxide lamella, prepares nickel hydroxide equally loaded graphene roll-CNT composite aerogel；Preparation process of the present invention
Simple and environmentally-friendly, easily operated, it is a kind of Green Chemistry preparation method.
A kind of nickel hydroxide/graphene roll-carbon nano tube composite carbon aeroge of the present invention, described composite carbon aeroge is composite carbon gas
The skeleton surface growth in situ nickel hydroxide nano sheet of gel；Wherein skeleton is that graphene roll, CNT build up three-dimensional jointly
The framing structure of network.
A kind of preparation method of the nickel hydroxide/graphene roll-carbon nano tube composite carbon aeroge of the present invention, including:
(1) by graphene oxide dispersion, acidifying carbon nano tube dispersion liquid, mixing, mixed liquor is obtained, then quenching, freezing
It is dried, carbonization, obtains graphene roll-CNT composite aerogel；
(2) Nickelous nitrate hexahydrate, carbamide are dissolved in organic solvent, obtain nickel nitrate solution；
(3) graphene roll-CNT composite aerogel is added in nickel nitrate solution, carry out chemical bath deposition reaction, washing,
It is dried, obtains sodium hydroxide/graphene roll-carbon nano tube composite carbon aeroge.
In described step (1), graphene oxide dispersion is: graphene oxide disperses in deionized water, ultrasonic, is aoxidized
Graphene dispersing solution；Acidifying carbon nano tube dispersion liquid is: disperseed in deionized water by acidifying CNT, ultrasonic, obtains
Acidifying carbon nano tube dispersion liquid；Wherein graphene oxide is graphene oxide prepared by Hummers method.
The preparation of acidifying CNT: be the mixing that 200mg multi-walled carbon nano-tubes is joined 200mL concentrated sulphuric acid and concentrated nitric acid
Liquid (volume ratio is 3:1) prepares in 60-80 DEG C of reaction 1-3h.
In described step (1), the concentration of graphene oxide dispersion is 4-10mg mL-1；The concentration of acidifying carbon nano tube dispersion liquid
For 1-4mg mL-1。
In described step (1), in mixed liquor, the mass ratio of graphene oxide and acidifying CNT is 8:1～2:1.
In described step (1), lyophilization is: temperature is-30～-50 DEG C, and vacuum is 10-30Pa, and sublimation drying is
20-30h。
Described step is mixed into ultrasonic mixing in (1)；Quenching is quenching in liquid nitrogen；Carbonization is: carbonization in noble gas, carbon
Changing temperature and be 600-900 DEG C, heating rate is 3-7 DEG C of min-1, carbonization constant temperature time is 1-3h.
Described noble gas is argon or nitrogen.
In described step (2) organic solvent be volume ratio be ethanol and the mixing of deionized water of 6:1～1:1, preferably 4:1～2:1
Solution.
In described step (2), consumption of organic solvent is 60～20mL, preferably 50～30mL.
In described step (2), Nickelous nitrate hexahydrate, the mol ratio of carbamide are 1:1～1:5, preferably 1:2～1:4.
In described step (2), Nickelous nitrate hexahydrate is 0.5～8mmol, and preferably scope is 2～6mmol, and carbamide is 1～12mmol,
Preferably scope is 1.5～10mmol.
In described step (3), chemical bath deposition reacts particularly as follows: water-bath temperature is 50-100 DEG C, preferably 60-80 DEG C, instead
It is 5-10h, preferably 6-8h between Ying Shi；Baking temperature is 60-100 DEG C, preferably 70～90 DEG C, and the time is 1-3h, preferably
1.5～2h.
A kind of application of the nickel hydroxide of the present invention/graphene-carbon nano tube composite carbon aeroge, described nickel hydroxide/Graphene-carbon
Nanotube composite carbon aeroge as the new energy devices such as high-performance super capacitor, lithium ion battery ideal electrode material should
With.
Use scanning electron microscope (SEM), X-ray diffractometer (XRD) to characterize nickel hydroxide that the present invention obtained/
Graphene roll-CNT composite aerogel, its result is as follows:
(1) test result of SEM shows: nickel hydroxide/graphene roll prepared by employing chemical bath deposition, Freeze Drying Technique-
CNT composite aerogel pattern is excellent, and graphene roll-CNT aerogel composite has hole structure, Graphene
Jointly be built into the framing structure of three-dimensional network with CNT, its inner void size than more uniform, be evenly distributed.The present invention
Nickel hydroxide nano sheet prepared by is evenly distributed, and a lamella size uniform.This pore size is homogeneous, pore-size distribution phase
To narrower, and the composite carbon aeroge covering with nickel hydroxide nano sheet on skeleton is to prepare high-performance super capacitor, lithium-ion electric
The ideal electrode material of the new energy devices such as pond.See Fig. 1.
(2) XRD test result further demonstrates that pure cerium hydroxide nickel nano film and nickel hydroxide/graphene roll-CNT are combined
On the XRD curve of aeroge, the position of diffraction maximum is identical, all occurs in that relatively at 2 θ=12.8 °, 25.5 °, 34.1 ° and 60.9 °
For sharp-pointed diffraction maximum, correspond respectively to α-Ni (OH)2(003), (006), (101) and (110) crystal face, this
Illustrating, the introducing of graphene roll-CNT composite aerogel does not change Ni (OH)2The crystalline structure of nanometer sheet.See Fig. 2.
Electrochemical results shows: be 1A g in electric current density-1Time, the quality of pure cerium hydroxide nickel nano film only has 610 than electric capacity
F g-1, and the specific discharge capacity of nickel hydroxide/graphene roll-CNT composite aerogel prepared by the present invention can reach 1208F
g-1.See Fig. 3.
Nickel hydroxide/graphene roll of the present invention-CNT composite aerogel uses nickel salt multiple at graphene roll-CNT
Close growth in situ nickel hydroxide lamella on aeroge to prepare.Can be used as a kind of high performance electrode material for super capacitor.This
Invent and will there is the nickel hydroxide of fake capacitance character and the graphene roll of electric double layer capacitance character by simple chemistry with deposition process
-carbon nanotube aerogel is combined mutually so that both are given full play to advantage, obtains having good electrical chemical property and high capacitance
Material.
Beneficial effect
(1) preparation process of the present invention is simple and environmentally-friendly, easily operated, is a kind of Green Chemistry preparation method；
(2) present invention uses on the nickel hydroxide/graphene roll prepared by one-step method chemical bath deposition-CNT composite aerogel skeleton
Nickel hydroxide nano sheet is less and is evenly distributed, and is the reason preparing the new energy devices such as high-performance super capacitor, lithium ion battery
Think electrode material.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the nickel hydroxide/graphene roll-CNT composite aerogel prepared by embodiment 1；
Fig. 2 be the nickel hydroxide/graphene roll-CNT composite aerogel prepared by embodiment 1, nickel hydroxide and pure graphene roll-
The XRD spectra of CNT composite aerogel；
Fig. 3 is that the nickel hydroxide/graphene roll-CNT composite aerogel prepared by embodiment 1, embodiment 2, pure cerium hydroxide nickel exist
2A g-1Constant current charge-discharge curve chart under electric current density.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and not
For limiting the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, those skilled in the art can
To make various changes or modifications the present invention, these equivalent form of values fall within the application appended claims limited range equally.
Embodiment 1
(1) graphite oxide is scattered in deionized water, ultrasonic obtains 8mg mL-1The graphene oxide dispersion of stable dispersion；
(2) acidifying CNT is scattered in deionized water, ultrasonic obtains 4mg mL-1Stable dispersion graphene oxide dispersion
Liquid；
(3) by 10mL 8mg mL-1Graphene oxide dispersion and 10mL 4mg mL-1Acidifying carbon nano tube dispersion liquid mixing,
After ultrasonic, form homogeneous dispersion liquid；
(4) mixed liquor of step (3) gained is placed in mould in liquid nitrogen freezing 20min；
(5) by composite lyophilization in freezer dryer of step (4) gained, lyophilization temperature is-30 DEG C, vacuum
Degree is 10Pa, and sublimation drying is 20h, forms graphene oxide volume-CNT composite aerogel；
(6) step (5) gained aeroge being carried out in nitrogen atmosphere high temperature cabonization, carburizing temperature is 700 DEG C, and heating rate is
5℃min-1, the response time is 3h；
(7) by 0.5g Nickelous nitrate hexahydrate, 320mg carbamide is dissolved in the mixed liquor of 30mL ethanol and water, wherein ethanol and water
Volume ratio be 2:1, stirring make it dissolve；
(8) step (6) gained graphene roll-CNT composite aerogel is put in step (7) gained nickel nitrate saline solution
(9) mixed liquor is put into 70 DEG C of water-baths, constant temperature 8h；
(10), after reaction terminates, obtained nickel hydroxide/graphene roll-CNT composite aerogel deionized water is cleaned 3
After secondary, it be placed in the baking oven of 80 DEG C and be dried 3h, gained composite aerogel is designated as Ni (OH)2@GCA-1。
Embodiment 2
(1) graphite oxide is scattered in deionized water, ultrasonic obtains 8mg mL-1The graphene oxide dispersion of stable dispersion；
(2) acidifying CNT is scattered in deionized water, ultrasonic obtains 4mg mL-1Stable dispersion graphene oxide dispersion
Liquid；
(3) by 10mL 8mg mL-1Graphene oxide dispersion and 10mL 4mg mL-1Acidifying carbon nano tube dispersion liquid mixing,
After ultrasonic, form homogeneous dispersion liquid；
(4) mixed liquor of step (3) gained is placed in mould in liquid nitrogen freezing 20min；
(5) by composite lyophilization in freezer dryer of step (4) gained, lyophilization temperature is-30 DEG C, vacuum
Degree is 10Pa, and sublimation drying is 20h, forms graphene oxide volume-CNT composite aerogel；
(6) step (5) gained aeroge being carried out in nitrogen atmosphere high temperature cabonization, carburizing temperature is 700 DEG C, and heating rate is
5℃min-1, the response time is 3h；
(7) by 1g Nickelous nitrate hexahydrate, 640mg carbamide is dissolved in the mixed liquor of 30mL ethanol and water, wherein ethanol and water
Volume ratio is 2:1, and stirring makes it dissolve；
(8) step (6) gained graphene roll-CNT composite aerogel is put in step (7) gained nickel nitrate saline solution
(9) mixed liquor is put into 70 DEG C of water-baths, constant temperature 8h；
(10), after reaction terminates, obtained nickel hydroxide/graphene roll-CNT composite aerogel deionized water is cleaned 3
After secondary, it be placed in the baking oven of 80 DEG C and be dried 3h, gained composite aerogel is designated as Ni (OH)2@GCA-2。
The capability value of the material as can be seen from Figure 3 prepared by different condition is had than the capability value of pure cerium hydroxide nickel
Raising in various degree.
Claims (10)
1. nickel hydroxide/graphene roll-carbon nano tube composite carbon aeroge, it is characterised in that: described composite carbon aeroge is compound
The skeleton surface growth in situ nickel hydroxide nano sheet of carbon aerogels；Wherein skeleton is that graphene roll, CNT build up jointly
The framing structure of three-dimensional network.
2. a preparation method for nickel hydroxide/graphene roll-carbon nano tube composite carbon aeroge as claimed in claim 1, including:
(1) by graphene oxide dispersion, acidifying carbon nano tube dispersion liquid, mixing, mixed liquor is obtained, then quenching, freezing
It is dried, carbonization, obtains graphene roll-CNT composite aerogel；
(2) Nickelous nitrate hexahydrate, carbamide are dissolved in organic solvent, obtain nickel nitrate solution；
(3) graphene roll-CNT composite aerogel is added in nickel nitrate solution, carry out chemical bath deposition reaction, washing,
It is dried, obtains sodium hydroxide/graphene roll-carbon nano tube composite carbon aeroge.
The preparation method of a kind of nickel hydroxide/graphene roll-carbon nano tube composite carbon aeroge the most according to claim 2, it is special
Levy and be: in described step (1), the concentration of graphene oxide dispersion is 4-10mg mL-1；Acidifying CNT dispersion
The concentration of liquid is 1-4mg mL-1。
The preparation method of a kind of nickel hydroxide/graphene roll-carbon nano tube composite carbon aeroge the most according to claim 2, it is special
Levy and be: in described step (1), in mixed liquor, the mass ratio of graphene oxide and acidifying CNT is 8:1～2:1.
The preparation method of a kind of nickel hydroxide/graphene roll-carbon nano tube composite carbon aeroge the most according to claim 2, it is special
Levy and be: in described step (1), quenching is quenching in liquid nitrogen；Lyophilization is: temperature is-30～-50 DEG C, vacuum
Degree is 10-30Pa, and sublimation drying is 20-30h；Carbonization is: carbonization in noble gas, and carburizing temperature is 600-900 DEG C,
Heating rate is 3-7 DEG C of min-1, carbonization constant temperature time is 1-3h.
The preparation method of a kind of nickel hydroxide/graphene roll-carbon nano tube composite carbon aeroge the most according to claim 5, it is special
Levy and be: described noble gas is argon or nitrogen.
The preparation method of a kind of nickel hydroxide/graphene roll-carbon nano tube composite carbon aeroge the most according to claim 2, it is special
Levy and be: in described step (2) organic solvent be volume ratio be ethanol and the mixed solution of deionized water of 6:1～1:1.
The preparation method of a kind of nickel hydroxide/graphene roll-carbon nano tube composite carbon aeroge the most according to claim 2, it is special
Levy and be: in described step (2), Nickelous nitrate hexahydrate, the mol ratio of carbamide are 1:1～1:5.
The preparation method of a kind of nickel hydroxide/graphene roll-carbon nano tube composite carbon aeroge the most according to claim 2, it is special
Levy and be: in described step (3), chemical bath deposition reacts particularly as follows: water-bath temperature is 50-100 DEG C, the response time
For 5-10h；Baking temperature is 60-100 DEG C, and the time is 1-3h.
10. the application of nickel hydroxide/graphene roll-carbon nano tube composite carbon aeroge as claimed in claim 1, it is characterised in that:
Nickel hydroxide/graphene roll-carbon nano tube composite carbon aeroge is as high-performance super capacitor, lithium ion battery electrode material
Application.
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| CN107586442A (en) * | 2017-08-29 | 2018-01-16 | 华南理工大学 | A kind of β nickel hydroxides multi-walled carbon nanotube/unsaturated polyester resin nano composite flame-proof material and preparation method thereof |
| CN108328611A (en) * | 2017-01-20 | 2018-07-27 | 中国科学院物理研究所 | A kind of self-supporting redox graphene volume network material and preparation method thereof |
| CN108328595A (en) * | 2017-01-20 | 2018-07-27 | 中国科学院物理研究所 | A kind of carbon aerogels and preparation method thereof and pressure sensor |
| CN108550824A (en) * | 2018-04-28 | 2018-09-18 | 上海理工大学 | A kind of high-capacity battery cathode material preparation method |
| CN110085434A (en) * | 2019-04-10 | 2019-08-02 | 南京航空航天大学 | Helical form Ni (OH)2Nanometer sheet/nitrogen-doped graphene/carbon pipe composite membrane preparation method and application |
| CN114085154A (en) * | 2021-12-01 | 2022-02-25 | 浙江解氏新材料股份有限公司 | Method for synthesizing para-fluoroaniline based on high-activity skeleton nickel |
| CN114388818A (en) * | 2022-01-17 | 2022-04-22 | 中国人民解放军国防科技大学 | Carbon aerogel supported atomic-level dispersed metal oxygen reduction electrocatalyst and preparation method and application thereof |
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| CN107586442B (en) * | 2017-08-29 | 2020-05-22 | 华南理工大学 | β -nickel hydroxide-multiwalled carbon nanotube/unsaturated polyester resin nanocomposite flame-retardant material and preparation method thereof |
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| CN108550824B (en) * | 2018-04-28 | 2020-08-04 | 上海理工大学 | Preparation method of high-capacity battery negative electrode material |
| CN110085434A (en) * | 2019-04-10 | 2019-08-02 | 南京航空航天大学 | Helical form Ni (OH)2Nanometer sheet/nitrogen-doped graphene/carbon pipe composite membrane preparation method and application |
| CN114085154A (en) * | 2021-12-01 | 2022-02-25 | 浙江解氏新材料股份有限公司 | Method for synthesizing para-fluoroaniline based on high-activity skeleton nickel |
| CN114085154B (en) * | 2021-12-01 | 2024-03-19 | 浙江解氏新材料股份有限公司 | Method for synthesizing p-fluoroaniline based on high-activity framework nickel |
| CN114388818A (en) * | 2022-01-17 | 2022-04-22 | 中国人民解放军国防科技大学 | Carbon aerogel supported atomic-level dispersed metal oxygen reduction electrocatalyst and preparation method and application thereof |
| CN114388818B (en) * | 2022-01-17 | 2024-04-09 | 中国人民解放军国防科技大学 | Oxygen reduction electrocatalyst for carbon aerogel loaded atomic fraction dispersed metal and preparation method and application thereof |
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