CN106053561A - Nano graphite-carbon nanotube-ionic liquid composite membrane, preparation and applications thereof - Google Patents
Nano graphite-carbon nanotube-ionic liquid composite membrane, preparation and applications thereof Download PDFInfo
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- CN106053561A CN106053561A CN201610307793.0A CN201610307793A CN106053561A CN 106053561 A CN106053561 A CN 106053561A CN 201610307793 A CN201610307793 A CN 201610307793A CN 106053561 A CN106053561 A CN 106053561A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/307—Disposable laminated or multilayered electrodes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a nano graphite-carbon nanotube-ionic liquid composite membrane, preparation and applications thereof. The thickness of the composite membrane is 4000 to 6000 nm. The composite membrane is formed by laminating a plurality of graphene layers. The distance between two neighbored graphene layers is 20 to 50 nm. Carbon nanotubes and ionic liquids are dispersed between two neighbored graphene layers. The specific surface area of the composite membrane is large, moreover, the composite membrane has a good electrochemical activity, and can be widely applied to the fields of nano electro-catalysis and biosensors, and the detection sensitivity is high.
Description
Technical field
The invention belongs to field of nanometer material technology, more particularly, to a kind of nano-graphene-CNT-ionic liquid
Composite membrane and preparation and application thereof, this composite membrane is the composite membrane of nano-graphene-CNT-ionic liquid.
Background technology
Graphene (Graphene) is the Two-dimensional Carbon nano material of a kind of uniqueness, because of its have good electricity, mechanics and
Thermal property (the electron mobility of high 140 times, the hot strength of high 100 times and high leading than same thickness steel alloy than silicon
Hot coefficient etc.), good biocompatibility, cheap synthesis cost and the chemically and thermally mechanical stability of superelevation, exist in recent years
The aspects such as microelectronics, new superconduction material, energy storage, sensor and electro-catalysis have broad application prospects.
Graphene, as two-dimension nano materials, is possible not only to represent self special character, and is expected to be assembled into novel
The thin-film material of macroscopic view.According to current document report, spin coating and dip coating, sucking filtration and evaporation induced self-assembly method can be passed through
Graphene film is become Deng by Graphene NW-TFT.The graphene film obtained is high-sequential from microcosmic and piles up closely
Nanometer laminated structure, the important parameter such as the thickness of film, the Nomenclature Composition and Structure of Complexes can accurately control.But simple graphene film
Stronger pi-pi bond effect is had so that graphene nano lamella is easily heaped, thus reduces graphite between nano-graphene lamella
The specific surface area of alkene film, reduces the mass transfer space of ion, reduces its electrical conductivity, and then the electrochemistry affecting graphene film self is lived
Property.
Summary of the invention
For disadvantages described above or the Improvement requirement of prior art, it is an object of the invention to provide a kind of nano-graphene-
CNT-ionic liquid composite membrane and preparation and application thereof, wherein by the composition crucial to this composite membrane and structure, preparation
In method, the proportioning raw materials of key, processing procedure etc. improve, and compared with prior art can effectively solve the problem that graphene nano
Lamella easily heaps the problem causing graphene film specific surface area low, and this composite membrane has good electro-chemical activity, can be wide
General nano electro-catalytic field and the field of biosensors of being applied to, detection sensitivity is high.
For achieving the above object, according to one aspect of the present invention, it is provided that a kind of nano-graphene-CNT-from
Sub-liquid composite membrane, it is characterised in that the thickness of this nano-graphene-CNT-ionic liquid composite membrane be 4000nm extremely
6000nm, this nano-graphene-CNT-ionic liquid composite membrane is overlapped mutually by multiple graphene sheet layers and is formed, adjacent
Two described graphene sheet layers between spacing be 20nm～50nm；Monodispersed between two adjacent described graphene sheet layers
There are CNT and ionic liquid.
Preferably, described ionic liquid is 1-butyl-3-methyl imidazolium tetrafluoroborate or 1-butyl-3-Methylimidazole. six
Fluorophosphate.
As present invention further optimization, in described nano-graphene-CNT-ionic liquid composite membrane, described
Graphene is 2～4 with the mass ratio of described CNT.
It is another aspect of this invention to provide that provide the system of a kind of nano-graphene-CNT-ionic liquid composite membrane
Preparation Method, it is characterised in that comprise the following steps:
(1) it is ground obtaining mixture after graphene oxide, CNT and ionic liquid being mixed, then, then will
This mixture is dispersed in water, and forms graphene oxide and oxidation that CNT concentration sum is 4mg/ml～6mg/ml
Graphene-carbon nano tube-ionic liquid mixed liquor；
(2) take described graphene oxide-CNT-ionic liquid that step described in 100ml～200ml (1) obtains to mix
Closing liquid, carry out solid-liquid separation by the vacuum filtration instrument with filter membrane, the solid drying of isolated is also divided with described filter membrane
Nano graphene oxide-CNT-ionic liquid composite membrane is i.e. obtained from rear；
(3) described nano graphene oxide-CNT-ionic liquid composite membrane hydrogen that described step (2) is obtained
Iodic acid reduction i.e. obtains nano-graphene-CNT-ionic liquid composite membrane.
As present invention further optimization, the graphene oxide in described step (1) is to use Hummers method to prepare oxygen
The aqueous solution of functionalized graphene, then, obtains graphene oxide after the aqueous solution of this graphene oxide of lyophilization.
As present invention further optimization, graphene oxide described in described step (1), described CNT and described
The proportioning of ionic liquid three is 1mg:(0.25mg～0.5mg): (5 μ l～10 μ l).
As present invention further optimization, the ionic liquid in described step (1) is 1-butyl-3-Methylimidazole. tetrafluoro
Borate.
As present invention further optimization, the described water in described step (1) is ultra-pure water.
As present invention further optimization, the described graphene oxide-CNT-ionic liquid in described step (1)
Body mixed liquor also processes through ultrasonic disperse.
According to another aspect of the present invention, it is provided that utilize above-mentioned nano-graphene-CNT-ionic liquid composite membrane
Nano-graphene-CNT-ionic liquid composite membrane of preparing of preparation method in the application of detection heavy metal ion.
As present invention further optimization, described heavy metal ion is cadmium ion or lead ion.
Above-mentioned nano-graphene-CNT-ionic liquid composite membrane is utilized it is another aspect of this invention to provide that provide
Nano-graphene-CNT-ionic liquid composite membrane of preparing of preparation method without enzyme type hydrogen peroxide electrochemistry
The application of sensor.
By the above technical scheme that the present invention is contemplated, compared with prior art, due to the raw material in preparation method
Proportioning, process technical process etc. improve, and the inside composition of the composite membrane prepared and structure the most also change,
Form the structure of composite membrane with high-specific surface area, high electrochemical activity.
Nano-graphene-CNT-ionic liquid the composite membrane obtained by preparation method of the present invention, its integral thickness
For 4000nm to 6000nm, it is to be overlapped mutually by multi-layer graphene lamella to be formed, it is possible in minimizing composite membrane, Graphene is unordered
Pile up, improve the specific surface area of whole film.This nano-graphene-CNT-ionic liquid composite membrane, macroscopically ties in paper-like
Structure, nano-lamellar structure in high-sequential on microcosmic；This nano-graphene-CNT-ionic liquid composite membrane is by graphite
Alkene lamella is overlapped mutually formation, and the adjacent spacing between graphene sheet layer is 20nm～50nm, CNT and ionic liquid
It is dispersed between adjacent graphene sheet layer.The thickness of each graphene sheet layer can be several nanometer (that is, nano-graphite
Alkene lamella, such as 1nm～10nm etc.), can be connected with each other by π key by the Graphene of multiple monoatomic layers forms that (list is former
The thickness of the Graphene of sublayer is about 0.335nm).
The present invention is (such as 1-butyl-3-Methylimidazole. Tetrafluoroboric acid by graphene oxide, CNT and ionic liquid
Salt) three mixes and formed graphene oxide and graphite oxide that CNT concentration sum is 4mg/ml～6mg/ml
Alkene-CNT-ionic liquid mixed liquor, graphene oxide, CNT and ionic liquid three preferably press 1mg:(0.25mg
～0.5mg): the ratio of (5 μ l～10 μ l) carries out proportioning, it can be ensured that the nano-graphene-CNT-ionic liquid of generation
Composite membrane is to be overlapped mutually by multi-layer graphene, and nano-lamellar structure in high-sequential on microcosmic, by nano-graphene lamella
Being overlapped mutually formation, the adjacent spacing between nano-graphene lamella is that 20nm～50nm, CNT and ionic liquid are equal
Even it is dispersed between described graphene nano lamella.The graphene oxide raw material that preparation method of the present invention uses is nanoscale oxygen
Functionalized graphene (size of graphene oxide in several nanometers to hundreds of nanometer, it is preferred to use Hummers method prepares graphene oxide
Aqueous solution, then by obtaining graphene oxide after the aqueous solution of this graphene oxide of lyophilization).
Preparation method provided by the present invention is simple to operate and friendly to environment, the composite film surface flat-satin of formation, machinery
Intensity is good, and the specific surface area of film is big, and electro-chemical activity is high.When the laminated film that the present invention provides is applied to nano electro-catalytic field
Can effectively detect heavy metal ion, and detection limits low, detection range width.Additionally, the laminated film application that the present invention is provided
When field of biosensors carries out detecting hydrogen peroxide little molecule, having higher detection sensitivity, application prospect is the widest
Wealthy.
Accompanying drawing explanation
Fig. 1 is the macrograph of graphene-carbon nano tube-ionic liquid composite membrane that the present invention provides；
Fig. 2 A and Fig. 2 B is profile scanning Electronic Speculum (SEM) figure of graphene-carbon nano tube-ionic liquid composite membrane, figure
2C and Fig. 2 D is flat scanning Electronic Speculum (SEM) figure of graphene-carbon nano tube-ionic liquid composite membrane；
Fig. 3 A, Fig. 3 B and Fig. 3 C are all the x-ray photoelectron spectroscopies (XPS) of graphene-carbon nano tube-ionic liquid composite membrane
Figure, vertical coordinate is photoelectron intensity, and abscissa is electron binding energy；Wherein, Fig. 3 A is graphene-carbon nano tube-ionic liquid
The full spectrogram of composite membrane, Fig. 3 B is the C1s spectrogram in graphene-carbon nano tube-ionic liquid composite membrane. Fig. 3 C be Graphene-
N1s spectrogram in CNT-ionic liquid composite membrane；
Fig. 4 is the Raman energy spectrum figure of the graphene-carbon nano tube-ionic liquid composite membrane of embodiment 1 preparation, and vertical coordinate is
Photoelectron relative intensity, abscissa is wave number；
Fig. 5 is that the graphene-carbon nano tube-ionic liquid laminated film of embodiment 1 preparation is at HAc-NaAC (pH=4.6)
Buffer solution uses the ion concentration spectrogram of Pb and Cd in differential pulse voltammetry detection solution；
Fig. 6 is that the graphene-carbon nano tube-ionic liquid laminated film of embodiment 1 preparation buffers at PBS (pH=7.4)
Cyclic voltammetric comparison diagram to the hydrogen peroxide of variable concentrations in solution.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, right
The present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, and
It is not used in the restriction present invention.If additionally, technical characteristic involved in each embodiment of invention described below
The conflict of not constituting each other just can be mutually combined.
The preparation of embodiment 1 graphene oxide
By 3g graphite powder, 3g sodium nitrate, 6g potassium permanganate and 23ml concentrated sulphuric acid in ice bath after mix homogeneously in normal-temperature water
Bath lower stirring reaction 2h.Temperature is risen to 35 DEG C, middle temperature reaction 3h.Continue at 90 DEG C after being gradually added into 100ml deionized water
Stirring continues reaction 30min, and mixture is become glassy yellow by sepia.Use dilute hydrochloric acid solution and deionized water abundant after cooling
Washing to filtrate is pH=6.Graphene oxide filter cake is fully saved backup in 60 DEG C of vacuum drying ovens after drying
The preparation of embodiment 2 graphene-carbon nano tubes-ionic liquid laminated film
In the present embodiment 2, the preparation method of graphene-carbon nano tube-ionic liquid laminated film comprises the following steps:
(1) use Hummers method (such as embodiment 1) to prepare the aqueous solution of graphene oxide, aoxidized after lyophilization
Graphene powder.
(2) after graphene oxide, CNT and ionic liquid being mixed, (milling time can be more than or equal in grinding
Half an hour), graphene oxide quality: carbon nanotube mass: the proportioning of ionic liquid volume three is 1mg:0.5mg:5 μ l, grinds
Mixture after mill is dispersed in water, forms graphene oxide and CNT concentration sum is the oxidation of 5mg/ml
Graphene-carbon nano tube-ionic liquid mixed liquor；
(3) graphene oxide-CNT-ionic liquid mixed liquor obtained in step (2) is taken 150ml, with
Aperture is that the vacuum filtration instrument of the cellulose acetate class filter membrane of 220nm carries out solid-liquid separation, and the solid that solid-liquid separation obtains is dried
After, graphene-carbon nano tube-ionic liquid film layer separates with filter membrane and i.e. can get nano graphene oxide-CNT-ion
Liquid composite membrane；
(4) graphene oxide-CNT-ionic liquid composite membrane hydroiodic acid (hydroiodic acid that will obtain in step (3)
Mass percentage concentration can be such as 45%) reduction, i.e. obtain nano-graphene-CNT-ionic liquid after reduction multiple
Close film.
Nano-graphene-CNT-ionic liquid composite membrane is macroscopically solid film, ionic liquid and Graphene, carbon
The strongest adhesion it is respectively provided with so that this nano-graphene-CNT-ionic liquid composite membrane has good between nanotube
Good entirety combines effect, can combine closely between nano-graphene and CNT.
Embodiment 3 graphene-carbon nano tubes-ionic liquid laminated film detection heavy metal ion
Using graphene-carbon nano tube-ionic liquid laminated film is working electrode, and reference electrode is saturated calomel electricity
Pole, auxiliary electrode is platinum electrode, with 0.2mol/L acetate buffer solution (pH=4.6, such as HAc-NaAc buffer solution) is
Test end liquid.In electrolyzer, add 40mL 0.2mol/L HAc-NaAc buffer solution (pH=4.6), add appropriate Pb
And Cd (II) standard solution (II), inserting three-electrode system, set sedimentation potential as-1.2V, sedimentation time is 300s (stirring),
Preenrichment stops stirring, static 10s after terminating, use differential pulse voltammetry just to be scanned by negative sense, measure and record dissolution bent
Line.Experiment, without letting nitrogen in and deoxidizing, is carried out the most at ambient temperature.Be can be seen that by Fig. 5, this laminated film is dense at wider ion
Can detect in the range of degree, and linear between electric current and concentration, graphene-carbon nano tube prepared by the present invention-from
Sub-liquid laminated film substantially increases the detection limit of Pb and Cd ion, this graphene-carbon nano tube-ionic liquid laminated film
The Pb ion that can detect and the least concentration of Cd ion are respectively 0.2nmol/L and 0.1nmol/L.
Embodiment 4 graphene-carbon nano tubes-ionic liquid laminated film is as without enzyme type hydrogen peroxide sensor
In three-electrode system, working electrode is graphene-carbon nano tube-ionic liquid laminated film, and auxiliary electrode is
Platinum electrode, reference electrode is saturated calomel electrode, and test end liquid is PBS (pH=7.4) buffer solution, is consequently formed hydrogen peroxide
Electrochemical sensor without enzyme.As seen from Figure 6, along with the increase of concentration of hydrogen peroxide, the electric current of cyclic voltammetry curve is gradually
Increase, demonstrate and preferably detect performance.
In above-described embodiment, CNT is commercial CNT, and such as, the purity of CNT is preferably greater than 95%,
The diameter of CNT is preferably 10nm～20nm, and length is preferably 10 μm～30 μm；Ionic liquid can use 1-butyl-3-
Methyl imidazolium tetrafluoroborate ([bmim] BF4) ionic liquid, naturally it is also possible to use other ionic liquid at room temperature such as 1-butyl-
3-Methylimidazole. hexafluorophosphate.Obtain graphene oxide powder after lyophilization and be generally nanoscale.
As it will be easily appreciated by one skilled in the art that and the foregoing is only presently preferred embodiments of the present invention, not in order to
Limit the present invention, all any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, all should comprise
Within protection scope of the present invention.
Claims (9)
1. nano-graphene-CNT-ionic liquid composite membrane, it is characterised in that this nano-graphene-carbon nanometer
The thickness of pipe-ionic liquid composite membrane is 4000nm to 6000nm, this nano-graphene-CNT-ionic liquid composite membrane
Being overlapped mutually by multiple graphene sheet layers and formed, the adjacent spacing between two described graphene sheet layers is 20nm～50nm；
Between two adjacent described graphene sheet layers, Monodispersed has CNT and ionic liquid；Preferably, described ionic liquid is
1-butyl-3-methyl imidazolium tetrafluoroborate or 1-butyl-3-Methylimidazole. hexafluorophosphate.
2. nano-graphene-CNT-ionic liquid composite membrane as claimed in claim 1, it is characterised in that described Graphene
It is 2～4 with the mass ratio of described CNT.
3. the preparation method of nano-graphene-CNT-ionic liquid composite membrane, it is characterised in that include following step
Rapid:
(1) it is ground obtaining mixture after graphene oxide, CNT and ionic liquid being mixed, then, then this is mixed
Compound is dispersed in water, and forms graphene oxide and graphite oxide that CNT concentration sum is 4mg/ml～6mg/ml
Alkene-CNT-ionic liquid mixed liquor；
(2) described graphene oxide-CNT-ionic liquid mixed liquor that step described in 100ml～200ml (1) obtains is taken,
Solid-liquid separation is carried out, the solid drying of isolated after separating with described filter membrane by the vacuum filtration instrument with filter membrane
I.e. obtain nano graphene oxide-CNT-ionic liquid composite membrane；
(3) described nano graphene oxide-CNT-ionic liquid composite membrane hydroiodic acid that described step (2) is obtained
Reduction i.e. obtains nano-graphene-CNT-ionic liquid composite membrane.
4. the preparation method of nano-graphene-CNT-ionic liquid composite membrane as claimed in claim 3, it is characterised in that
Graphene oxide in described step (1) is the aqueous solution using Hummers method to prepare graphene oxide, then, lyophilization
Graphene oxide is obtained after the aqueous solution of this graphene oxide.
5. the preparation method of nano-graphene-CNT-ionic liquid composite membrane as claimed in claim 3, it is characterised in that
The proportioning of graphene oxide described in described step (1), described CNT and described ionic liquid three is 1mg:(0.25mg
～0.5mg): (5 μ l～10 μ l).
6. the preparation method of nano-graphene-CNT-ionic liquid composite membrane as claimed in claim 3, it is characterised in that
Ionic liquid in described step (1) is 1-butyl-3-methyl imidazolium tetrafluoroborate；Preferably, the institute in described step (1)
Stating water is ultra-pure water.
7. the preparation method of nano-graphene-CNT-ionic liquid composite membrane as claimed in claim 3, it is characterised in that
Described graphene oxide-CNT-ionic liquid mixed liquor in described step (1) also processes through ultrasonic disperse.
8. utilize the preparation method of nano-graphene-CNT-ionic liquid composite membrane described in claim 3-7 any one
Nano-graphene-CNT-ionic liquid the composite membrane prepared is in the application of detection heavy metal ion；Preferably, institute
Stating heavy metal ion is cadmium ion or lead ion.
9. utilize the preparation method of nano-graphene-CNT-ionic liquid composite membrane described in claim 3-7 any one
Nano-graphene-CNT-ionic liquid the composite membrane prepared is answering without enzyme type hydrogen peroxide electrochemical sensor
With.
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