CN109540827A - A kind of graphene oxide method for comprehensive detection - Google Patents
A kind of graphene oxide method for comprehensive detection Download PDFInfo
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- CN109540827A CN109540827A CN201811575202.3A CN201811575202A CN109540827A CN 109540827 A CN109540827 A CN 109540827A CN 201811575202 A CN201811575202 A CN 201811575202A CN 109540827 A CN109540827 A CN 109540827A
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- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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Abstract
The present invention provides a kind of graphene oxide method for comprehensive detection.Described detection method includes the following steps: separating the first sample, the second sample and third sample from graphene oxide, ftir analysis test is carried out to the first sample, obtain the infrared spectrogram of graphene oxide, X-ray photoelectron spectroscopic analysis test is carried out to the second sample, obtain the x-ray photoelectron spectroscopy figure of graphene oxide, Raman spectrum test is carried out to third sample, obtains the Raman spectrogram of graphene oxide；The type and quantity that functional group on graphene oxide is determined according to the infrared spectrogram and the energy spectrum diagram, the number of plies of graphene oxide is determined according to the Raman spectrogram.The beneficial effect comprise that method it is easy, can accurate detection go out the type and quantity of functional group and the specific number of plies of graphene oxide on graphene oxide.
Description
Technical field
The present invention relates to graphene oxide composite material detection fields, particularly, are related to the comprehensive inspection of a kind of pair of graphene oxide
Survey method.
Background technique
Graphene (Graphene) is a kind of new material of individual layer laminated structure being made of carbon atom.It is a kind of by carbon original
Son is with sp2The hexangle type of hydridization composition is in the flat film of honeycomb lattice, the two-dimensional material of only one carbon atom thickness.Although
Graphene has unique texture and many excellent properties, but since single complete six-membered ring structure causes in dispersion process
In it is intermolecular generate very strong active force, as a result allow each lamella to stack；Due to the stabilization inertia on surface, it is dispersed in its indissoluble molten
In agent, it more difficult to which uniformly compound with the material of other organic or inorganics, this is that one during application of graphene makes us
The problem of very perplexing.And graphene oxide (GO) is not only containing there are many functional group, while can also be by small molecule or polymer
Intercalation or removing can effectively improve the performance of composite materials.
Generally, it is considered that the only number of plies in 10 layers of graphite below just can be regarded as two-dimensional structure, titled with the title of graphene
Meaning.According to the difference of the graphene oxide number of plies, significant changes can occur for electronic structure, to influence its electric conductivity, this is in lithium
The application field of ion battery is very crucial.In addition, some researches show that, the thermal conductivity of single-layer graphene oxide, translucency is more preferable,
Multilayer graphene oxide is higher to the disposal efficiency of organic dyestuff.Therefore, to the research of graphene oxide number of plies measurement method
Facilitate the deep relationship understood between graphene oxide performance and microstructure.
In order to which it plays bigger effect in the related art, people go to understand graphene oxide with furtheing investigate in recent years
Structural property (such as number of plies), and the structural property of graphene oxide and the type and quantity of its functional group are closely related, because
This, the identification to graphene oxide, especially the identification of functional group's type and quantity and the number of plies is highly important thereon.
Summary of the invention
For the deficiencies in the prior art, it is an object of the invention to solve above-mentioned one existing in the prior art
Or multiple problems.For example, one of the objects of the present invention is to provide the inspections that one kind can accurately identify graphene oxide information
Survey method.
To achieve the goals above, the present invention provides a kind of graphene oxide method for comprehensive detection.The detection method
It may include dimly by step: separating the first sample, the second sample and third sample from graphene oxide, Fu is carried out to the first sample
In leaf transformation infrared spectrum analysis test, obtain the infrared spectrogram of graphene oxide, to the second sample carry out x-ray photoelectron
Energy spectrum analysis test, obtains the x-ray photoelectron spectroscopy figure of graphene oxide, carries out Raman spectrum test to third sample, obtains
To the Raman spectrogram of graphene oxide；Functional group on graphene oxide is determined according to the infrared spectrogram and the energy spectrum diagram
Type and quantity, the number of plies of graphene oxide is determined according to the Raman spectrogram, wherein on the determining graphene oxide
The step of functional group's type includes: to search middle infrared in the infrared spectrogram, obtains absorption peak on the middle infrared
The wave number is compared with ir data library, determines the type of functional group on graphene oxide by corresponding wave number；Institute
The step of stating number of functional groups on determining graphene oxide includes: to judge each peak in the energy spectrum diagram according to the size in conjunction with energy
Corresponding element is modified by peak intensity of the sensitivity factor to peak corresponding to each element, right by each element institute after amendment
It answers the ratio between peak peak intensity to obtain the relative amount ratio of each element, according to the relative amount ratio, determines on graphene oxide
The quantity of functional group；The step of determining graphene oxide number of plies includes: to calculate I according to the Raman spectrogramG/I2D, when
IG/I2DWhen less than 1.0, tentatively judge graphene oxide for single or double layer structure；Work as IG/I2DWhen being 1.0~1.5, tentatively sentence
Disconnected graphene oxide is 3 layers or 4 layers of structure；Work as IG/I2DWhen greater than 1.5, tentatively judge graphene oxide for 5 layers or more structures,
Wherein, the IGIndicate G peak intensity, the I2DIndicate 2D peak intensity.
An exemplary embodiment according to the present invention is tentatively judging the graphene oxide for single or double layer structure
In the case where, the 4th sample is separated from the graphene oxide, and the 4th sample is tested using atomic force microscope, with
Determine that the graphene oxide is single or double layer structure.
An exemplary embodiment according to the present invention is tentatively judging the graphene oxide for 3 layers or 4 layers structure
In the case of, the Lorentz force peak number of the peak the 2D fitting of the Raman test result Raman spectrogram is calculated, graphene oxide is differentiated
For 3 layers or 4 layers of structure.
An exemplary embodiment according to the present invention is tentatively judging the graphene oxide for 5 layers or more structures
In the case of, the 5th sample is separated from the graphene oxide, and the electricity of graphene oxide is obtained by high resolution TEM
Sub- micro-image, observation determine the specific number of plies of graphene oxide.
An exemplary embodiment according to the present invention, it is described that the 4th sample is tested using atomic force microscope
Step can include: obtain the three-dimensional image of the 4th sample using atomic force microscope, and by the three-dimensional image
The thickness of display and the graphene oxide thickness of single layer compare, so that it is determined that the graphene oxide number of plies is single or double layer.
An exemplary embodiment according to the present invention, it is described preliminary to judge graphene oxide for single or double layer structure
Step can include: when the halfwidth at the peak 2D is 28cm-1~32cm-1And IG/I2DWhen the intensity ratio at peak is less than 0.7, tentatively
Judge the graphene oxide for single layer structure；When the halfwidth at the peak 2D is 48cm-1~52cm-1And IG/I2DThe intensity at peak
The ratio between for more than or equal to 0.7 less than 1.0 when, tentatively judge the graphene oxide for double-layer structure.
An exemplary embodiment according to the present invention, functional group's type, quantity on the determining graphene oxide
After step, the method also includes: according to the functional group's type and number of functional groups of the determination, obtain the graphite oxide
The quantity of Xi Shangge functional group.
An exemplary embodiment according to the present invention, the wavelength of the middle infrared can be 2.5~25 μm.
An exemplary embodiment according to the present invention, the middle infrared includes characteristic frequency area and fingerprint region, in institute
It states and obtains the corresponding wave number of absorption peak in characteristic frequency area, the corresponding wave number of absorption peak is obtained on the fingerprint region.
An exemplary embodiment according to the present invention, the wavelength in the characteristic frequency area can be 2.5~7.7 μm, described
The wavelength of fingerprint region is greater than 7.7 μm, not larger than 25 μm.
An exemplary embodiment according to the present invention, if element corresponds to multiple peaks in the energy spectrum diagram, with described
The peak intensity of highest peak is as the modified object in multiple peaks.
An exemplary embodiment according to the present invention, the calculating each element relative amount ratio the step of in, it is optional
The area or intensity for taking highest peak are modified intensity as the basis quantitatively calculated, and using sensitivity factor.
An exemplary embodiment according to the present invention, the when carrying out ftir analysis test
A sample be tabletting powder, it is described carry out X-ray photoelectron spectroscopic analysis test when the second sample be tabletting powder.I.e.
Ftir analysis is surveyed and requirement of the X-ray photoelectron spectroscopic analysis test to graphene oxide is: tabletting
Graphene oxide powder is carried out tabletting by powder.
Compared with prior art, beneficial effects of the present invention can include: can accurately and rapidly detect graphene oxide
The type and quantity of upper functional group, while can also detect the number of plies of graphene oxide.
Detailed description of the invention
By the description carried out with reference to the accompanying drawing, above and other purpose of the invention and feature will become more clear
Chu, in which:
Fig. 1 shows a FTIR spectrum figure of graphene oxide in example of the present invention；
Fig. 2 shows an xps energy spectrum figures of graphene oxide in example of the present invention；
Fig. 3 shows the Raman spectrogram of crystalline flake graphite in example；
Fig. 4 shows the Raman spectrogram of carbon material in example；
Fig. 5 shows the high resolution TEM figure of carbon material in example.
Specific embodiment
Hereinafter, graphene oxide comprehensive detection of the invention will be described in detail in conjunction with attached drawing and exemplary embodiment
Method.
When Infrared irradiation of the sample by frequency consecutive variations, molecule can absorb the radiation of certain frequencies, and by
It is vibrated or rotational motion causes the net change of dipole moment, generates the jump of molecular vibration and rotational energy level from ground state to excitation state
It moves, weakens the transmitted intensity corresponding to these absorption regions.The percentage transmittance and wave number or wavelength for recording infrared light are closed
It is curve, just obtains infrared spectroscopy.It is abscissa that infrared spectrogram, which leads to common wavelengths (λ) or wave number (σ), indicates the position of absorption peak
It sets, is ordinate with light transmittance (T%) or absorbance (A), indicates absorption intensity.In organic molecule, constitutional chemistry key
Or the atom of functional group is in the state constantly vibrated, vibration frequency is suitable with the vibration frequency of infrared light.Therefore, use is infrared
When light irradiates organic molecule, absorption of vibrations, different chemical bonds or official can occur for chemical bond or functional group in molecule
Absorption frequency difference can be rolled into a ball, different location will be on infrared spectroscopy, thus can get in molecule containing which kind of chemical bond or
The information of functional group.
X-ray photoelectron spectroscopic analysis (X-ray photoelectron spectroscopy, XPS) is gone with X-ray
Radiation sample comes out the inner electron of atom or molecule or valence electron stimulated emission.It is known as by the electronics that photon excitation comes out
Photoelectron can measure photoelectronic energy, and using photoelectronic kinetic energy as abscissa, relative intensity (pulse/s) is that ordinate can
Make photoelectron spectroscopy figure.It can analyze reaction of atomic according to photoelectron the intensity of spectral line in energy spectrum diagram (area of Photoelectron peak)
Content or relative concentration.
Raman spectrum is the effective tool for characterizing carbon nanomaterial structure feature and performance.It is imitated using Raman scattering
It answers, the scattering spectrum different from incident light frequency is analyzed to obtain molecular vibration, rotation aspect information, and be applied to divide
A kind of analysis method of minor structure research.So-called Raman scattering is a kind of inelastic scattering effect of the molecule to photon, when with
The exciting light sub-irradiation period of the day from 11 p.m. to 1 a.m of certain frequency, the frequency of a part scattering light and the frequency of incident light are equal.This scattering is point
A kind of elastic scattering of the son to photon.Collision only between molecule and photon is elastic collision, when not having energy exchange, can just be gone out
Existing this scattering, the scattering are known as Rayleigh scattering.The frequency of some scattering light and the frequency of exciting light differ, this to dissipate
Penetrating becomes Raman scattering (and being divided into stockes line and anti-stockes line).And the Raman scattering signal is received and drawn
The method of spectrum analysis can be described as Raman spectrum analysis, and common scattered signal is stockes line.To graphene oxide into
When row characterization, the features such as shape, position and intensity of wave crest formed in Raman map all can be with graphene oxide layer
Several increases and corresponding change occurs.
Atomic force microscope (AFM) is observed and is analyzed using interaction force generally existing between sample and scanning needle point
Object surface appearance feature.It has a nanoscale probe, and being fixed on can be on the micron order elastic cantilever of sensitive manipulation.When
When probe is very close to sample, the atom and the interatomic active force of sample surfaces on top can make cantilever bending, deviate original flat
Weighing apparatus position.3-D image is rebuild according to the spatial offset amount or vibration frequency of probe, pattern, the atom of sample surfaces can be obtained
Ingredient, mechanical property or other properties.
Transmission electron microscope (TEM) can directly observe sample structure feature, such as the number of plies by the full resolution pricture of sample
And size.
Therefore, each peak in the infrared spectroscopy of ftir analysis (FTIR) is able to reflect graphene oxide
The vibration of middle chemical bond and functional group；Each peak of xps energy spectrum is able to reflect the relative amount of element in graphene oxide.High-resolution
Transmission electron microscope (HRTEM), Raman spectrum (Raman), atomic force microscope (AFM) combines can be right
The number of plies of graphene oxide is identified.Above-mentioned test analysis is applied in combination the invention proposes one kind as a result, to come to oxidation stone
The method that black alkene carries out comprehensive detection.
In an exemplary embodiment of the present invention, graphene oxide functional group detection method may include following step
It is rapid:
(1) the graphene oxide functional group that the present invention is analyzed by the way that FTIR and XPS test is applied in combination.Specifically, inspection
The step of surveying functional group's type and quantity on graphene oxide can include:
The first sample and the second sample are separated from graphene oxide, Fourier transform infrared spectroscopy point is carried out to the first sample
Analysis test, obtains the infrared spectrogram of graphene oxide, carries out X-ray photoelectron spectroscopic analysis test to the second sample, obtains
The x-ray photoelectron spectroscopy figure of graphene oxide.
The type and quantity of functional group on graphene oxide are determined according to the infrared spectrogram and the energy spectrum diagram.Its
In,
On the determining graphene oxide the step of functional group's type can include: red in being searched in the infrared spectrogram
Outskirt obtains the corresponding wave number of absorption peak on the middle infrared, the wave number is compared with ir data library, really
Determine the type of functional group on graphene oxide；
On the determining graphene oxide the step of number of functional groups can include: judge the energy according to the size in conjunction with energy
The corresponding element in each peak, is modified by peak intensity of the sensitivity factor to peak corresponding to each element, passes through amendment on spectrogram
The ratio between peak peak intensity corresponding to each element obtains the relative amount ratio of each element afterwards, according to the relative amount ratio, determines
The quantity of functional group on graphene oxide.
(2) of the invention by high resolution transmission electron microscope (HRTEM), Raman spectrum (Raman), atomic force microscope
(AFM) it combines to determine the specific number of plies of graphene oxide, i.e., first primarily determines oxidation stone with Raman spectrum
The number of plies of black alkene, if the number of plies at 1~2 layer, further determines its number of plies using atomic force microscope；If the number of plies at 3~4 layers,
Then determined by the Lorentz force peak number that the peak Raman spectrum 2D fits；It is saturating using high-resolution if 5 layers or more if the number of plies
Radio mirror intuitively obtains its number of plies, is capable of the number of plies of the determination graphene oxide of system perfecting.
Determine the specific steps of the number of plies can include:
1) the graphene oxide number of plies is primarily determined by Raman spectrum.The present invention mainly utilizes Raman scattering i.e. Stokes
Scattering primarily determines the graphene oxide number of plies.When inelastic scattering has energy exchange, wavelength shift is changed, and most of frequency is not
It changes, only fraction shifts, and this scattering is known as Raman scattering.When energy is reduced, wave number displacement becomes smaller, and generates
Stockes line；When energy increases, wave number displacement becomes larger, and generates anti-stockes line, they are symmetrically dispersed in Rayleigh scattering
The two sides of line are respectively corresponding to obtain or lose the energy of 1 vibration quantum.When being characterized to graphene oxide,
The features such as shape, position and the intensity of wave crest formed in Raman map can all occur with the increase of the graphene oxide number of plies
Corresponding change.According to these variations, then preliminary judgement can be carried out to the graphene oxide number of plies.
Firstly, separating the sample of test from carbon material, Raman spectrum test is carried out to the sample, obtains graphite oxide
The Raman spectrogram of alkene (i.e. carbon material).It generally will form 3 main peak types on the Raman spectrogram of graphene oxide, be respectively
The peak D, the peak G and the peak 2D (frequency multiplication peak).Wherein, the peak D represents the sp of aromatic rings in graphene oxide structure2The symmetrical of carbon atom stretches
Vibration (radial breathing), is generally used to measure the order degree of sample structure.The peak G is normally at 1580cm-1Position, peak shape is very
Sharply.That the peak G represents is sp in graphene oxide2The in plane vibration mode of hydbridized carbon atoms.The position at the peak G is to graphene oxide
The number of plies is very sensitive, through the position at the peak G, it can be determined that the number of plies of specific graphene oxide sample.With the increase of the number of plies, G
Peak is mobile towards lower wave number direction, that is, mobile towards low energy direction, shows the weakening of the bond energy between graphene oxide layer.Due to
The peak position of graphene oxide will receive temperature, doping and very faint stress influence, so, when need using Raman into
When the row graphene oxide number of plies calculates, extreme care is answered in operation.The peak 2D represents the vibration mode of two photonic crystal lattices, is the peak D
Frequency multiplication peak.In graphene oxide raman spectrum, even if the peak D is not present, the peak 2D is also always very strong, nor represents defect.
For single-layer graphene oxide sample, the peak 2D is an individual symmetrical peak, halfwidth about 30cm-1.It is right with the increase of the number of plies
Title property reduces, and the peak 2D splits into the peak of multiple overlappings.This apparent peak shape change can effectively distinguish graphene oxide layer number.
Due to the limitation of itself Raman figure, it is only applicable to graphene oxide measurement of the number of plies less than 5 layers.To sum up, it can use IG/I2DPeak
Intensity ratio can primarily determine the number of plies of graphene oxide.IGIndicate G peak intensity, the I2DIndicate 2D peak intensity.
As I in graphene oxide spectrogramG/I2DWhen the intensity ratio at peak is less than 1.0, can tentatively it judge in graphene oxide
There are single layer structure or double-layer structure, if need to determine in graphene oxide is single layer or double-layer structure, needs aobvious with atomic force
Micro mirror does further measurement；Work as IG/I2DIntensity ratio be 1.0~1.5 when, then judge graphene oxide be 3 layers or 4 layers knot
Structure, wherein the peak 2D of 3 layers of graphene oxide can be judged with six Lorentz peaks to be fitted.Work as IG/I2DIntensity > 1.5
When, the Raman spectrum of graphene oxide and the Raman spectrum of graphite are similar, it is difficult to measure the graphene oxide number of plies, need to use at this time
High resolution TEM does further measurement.
2) the system measurement graphene oxide number of plies.
It can use atomic force microscope for the graphene oxide that Preliminary Determination is single or double layer to carry out its number of plies
It is further to determine.After Raman spectrum primarily determines in sample and has single or double layer graphene oxide, atomic force microscope energy
The three-dimensional image for directly obtaining graphene oxide is single layer or the double-deck graphite oxide by the measurement determination to thickness
Alkene.It is described to determine that graphene oxide is single layer or double-layer structure includes the graphene oxide thickness and list that measured by thickness
The graphene oxide thickness of layer compares, and determines the graphene oxide number of plies.For example, for the oxygen being attached in the substrates such as mica sheet
Graphite alkene overburden will increase the about extra play of 0.35nm, so observing the thickness one of single-layer graphene oxide at AFM
As about 0.7~1.2nm.This thickness can be identified into single-layer graphene oxide compared with thickness of sample in afm image, utilize height
Line of writing music, which carries out statistical disposition, can identify the double-deck graphene oxide.
For Preliminary Determination is 3 layers or 4 layers of graphene oxide, it can be fitted by the peak Raman spectrum 2D
Lorentz force peak number determines.For example, can be judged by six Lorentz peaks to be fitted.
The graphene oxide for being 5 layers or more for Preliminary Determination, can use high resolution TEM and does to its number of plies
It is further to determine.It can be by the full resolution pricture at graphene oxide edge or fold come straight using transmission electron microscope (TEM)
The number of plies and size for connecing observation graphene oxide, can directly read the number of plies of graphene oxide directly from image.But
In the less apparent situation of contrast, especially for single layer and the double-deck graphene oxide, high resolution transmission electron microscope
It can not accurately judge the number of plies of graphene oxide.
In the present embodiment, the detection of functional group's type and quantity, the detection of the graphene oxide number of plies on graphene oxide
It can in no particular order sequentially.
In the present embodiment, the method may further comprise the step of: the functional group's type and functional group number according to the determination
Amount, obtains the quantity of graphene oxide Shang Ge functional group.The differentiation for needing that FTIR is combined to carry out functional group's type.
In the present embodiment, when carrying out FTIR and XPS test, for graphene oxide, it is desirable that be that will aoxidize stone
Black alkene powder tabletting.
In the present embodiment, during determining the carbon material number of plies, can use the peak 2D in Raman spectrogram half is high
Wide and IG/I2DThe intensity ratio at peak primarily determines that graphene oxide is single or double layer structure.When the halfwidth at the peak 2D is 28cm-1
~32cm-1And IG/I2DWhen the intensity ratio at peak is less than 0.7, tentatively judge graphene oxide for single layer structure；Half when the peak 2D is high
Width is 48cm-1~52cm-1And IG/I2DWhen the intensity ratio at peak is more than or equal to 0.7 less than 1.0, tentatively judge that graphene oxide is
Double-layer structure.
In the present embodiment, when Infrared irradiation when carbon material by frequency consecutive variations, molecule can absorb certain
The radiation of frequency, and the net change of dipole moment is caused by its vibration or rotational motion, molecular vibration and rotational energy level are generated from base
State weakens the transmitted intensity corresponding to these absorption regions to the transition of excitation state.Record the percentage transmittance of infrared light
With wave number or wavelength plot, infrared spectroscopy is just obtained.Infrared spectrogram leads to common wavelengths (λ) or wave number (σ) is abscissa,
The position for indicating absorption peak is ordinate with light transmittance (T%) or absorbance (A), indicates absorption intensity.In organic molecule
In, the atom of constitutional chemistry key or functional group is in the state constantly vibrated, the vibration frequency phase of vibration frequency and infrared light
When.Therefore, when with Infrared irradiation organic molecule, absorption of vibrations can occur for chemical bond or functional group in molecule, no
Same chemical bond or functional group's absorption frequency is different, and different location will be on infrared spectroscopy, be contained in molecule to can get
There is the information of which kind of chemical bond or functional group.
The step of determining functional group's type on graphene oxide is specific can include:
Graphene oxide infrared spectrogram is divided into three regions: near infrared region (0.75~2.5 μm), middle infrared (2.5
~25 μm) and far-infrared band (25~300 μm).It is, in general, that near infrared spectrum is generated by the frequency multiplication of molecule, sum of fundamental frequencies；In
Infrared spectroscopy belongs to the fundamental vibration spectrum of molecule；Far-infrared spectrum then belongs to the rotation spectrum of molecule and the vibration of certain groups
Spectrum.
By the source of absorption peak, mid-infrared light spectrogram (2.5~25 μm) is generally divided into (2.5~7.7 μm of characteristic frequency
That is 4000~1330cm-1) and fingerprint region (7.7~16.7 μm, i.e. 1330~400cm-1) two regions.Wherein characteristic frequency
Absorption peak in area is substantially to be generated by the stretching vibration of group；Fingerprint region is mainly by some singly-bound C-O, C-N and C-X (halogen
Plain atom) etc. stretching vibration and the hydric groups such as C-H, O-H bending vibration and C-C skeletal vibration generate.
Therefore, for the analyzing step of obtained graphene oxide infrared spectrogram can include: the first step finds oxidation stone
The middle infrared (2.5~25 μm) of black alkene.Second step finds characteristic frequency area (2.5~7.7 μm, i.e. 4000-1330cm-1) and
Fingerprint region (7.7~16.7 μm, i.e. 1330~400cm-1).Step 3: according to the corresponding wave number pair of characteristic peak in infrared spectrogram
Determine what functional group the group is than infrared spectrum database.Such as: 1725cm-1It is the flexible vibration of carbonyl C==O on carboxyl
It is dynamic, 1615cm-1It is the stretching vibration of carbon-carbon double bond C==C, 1373cm-1It is the stretching vibration of C-OH, 1078cm-1It is epoxy group
The stretching vibration of C-O-C.
In the present embodiment, since the spectral peak of XPS is often wider, intensity cannot be determined according only to peak heights, generally
Area under using spectral peak is substantially equal to peak height and multiplies half-peak breadth as intensity.The area or intensity for choosing highest peak are as quantitative scoring
The basis of calculation, mostly uses sensitivity factor method, because the intensity and content when each element generation photoelectron are not necessarily directly proportional, from
And intensity is modified using sensitivity factor, way are as follows: be subject to peak side, background point of intersection of tangents background correction, meter
Peak area or peak intensity are calculated, then respectively divided by the sensitivity factor of respective element, so that it may obtain the relative amount of each element, then
Obtain each element relative amount ratio.Or using formula ni/nj=(Ii/Si)/(Ij/Sj) the opposite of two elements is directly asked to contain
Measure ratio, wherein ni、njIt may respectively be the atomic concentration of different elements, Ii、IjIt may respectively be the intensity of spectral line of different elements, Si、Sj
It may respectively be the sensitivity factor of different elements.
It can be according to quantity of the element relative amount than calculating functional group.Such as: when C/O=2:1, graphite oxide can be calculated
In oxygen-containing functional group quantity.Different elements have fixed combination energy numerical value in corresponding functional group, by tabling look-up or
Person and other work compare, or combine FTIR it is determined which kind of functional group, then have stoichiometric relationship, can be from element
Content obtain the content of corresponding functional group.
The above exemplary embodiments for a better understanding of the present invention carry out further it below with reference to specific example
Explanation.
(1) ftir analysis test is carried out to graphene oxide and X-ray photoelectron spectroscopic analysis is surveyed
Examination, and respectively obtain graphene oxide as shown in Figure 1 FTIR spectrum and xps energy spectrum figure as shown in Figure 2.
It can be observed that the position of the absorption peak of part functional group, thus can determine whether there is carbonyl in graphene oxide from Fig. 1
Base, carboxyl, hydroxyl, epoxy group, the functional groups such as carbon-carbon double bond.Wherein 3397cm-1The wider absorption peak in left and right is stretching for hydroxyl O-H
Contracting vibration；1725cm-1It is the stretching vibration of carbonyl C==O on carboxyl；1615cm-1It is the flexible vibration of carbon-carbon double bond C==C
It is dynamic；1373cm-1It is the stretching vibration of C-OH；And 1078cm-1It is the stretching vibration of epoxy group C-O-C.
The intensity that C1s and O1s corresponds to peak can be observed from Fig. 2, C:O=2:1 is calculated according to sensitivity factor method.Root
The quantity of oxygen-containing functional group can be calculated according to carbon-to-oxygen ratio, other elements all calculate its functional group number using sensitivity factor method
Amount, such as sulfur-bearing or the number of functional groups containing halogen etc..
(2) are carried out by Raman spectrum test, and obtains corresponding Raman spectrogram for crystalline flake graphite, graphene oxide.Wherein,
Fig. 3 shows the Raman spectrogram of crystalline flake graphite, and Fig. 4 shows the Raman spectrogram of graphene oxide.
The present invention is carried out using the comparative analysis of crystalline flake graphite and the Raman map (i.e. Fig. 3 and Fig. 4) of graphene oxide
Further instruction.As shown in figure 3, crystalline flake graphite is in 1360cm-1Place has a faint absorption peak (peak D), in 1580cm-1
Place there are a point and strong absorption peak (peak G) corresponding to the first-order Raman scattering of E2g optical mode illustrates that the structure of graphite is non-
It is conventional whole.After graphite is oxidized, the peak G of graphite oxide has broadened, and moves to 1590cm-1Place, and also in 1360cm-1
There is a stronger peak D, after showing that graphite is oxidized, a part of sp in structure in place2Hydbridized carbon atoms are converted to sp3Hydridization knot
Structure, i.e., the C=C double bond in graphite linings are destroyed.
As shown in figure 4, graphene oxide is in 1590cm-1There is a stronger absorption peak (peak G) in place, compared to scale
The peak G of graphite occurs illustrating that graphene oxide is reduced compared with the crystalline flake graphite number of plies to the movement of high wave number direction.In 2700cm-1Place
There is the wider peak 2D in a peak (frequency multiplication peak), this is by two in the carbon atom phonon double resonance transition with reversed momentum
Caused by, the movement of this characteristic peak and shape then have close be associated with the graphene oxide number of plies.And IG/I2D> 1.5, it says
The multilayered structure that this bright graphene oxide is 5 layers or more, cannot be further analyzed using Raman spectrum, therefore, I
Sample is measured using high magnification transmission electron microscope.
Transmission electron microscope analysis is done to one region of carbon material and obtains high resolution TEM (HRTEM) figure (Fig. 5 a institute
Show), the stacked graph of graphene oxide can be intuitively obtained, the number of plies that this graphene oxide sample can be obtained after statistical counting is 7
Layer.In addition it takes another region of carbon material to do transmission electron microscope analysis and obtains Fig. 5 b, can obviously observe two panels multilayer oxygen fossil in Fig. 5 b
Black alkene lamination is staggered, and the lamination being located above is of five storeys graphene oxide, underlying to have 7 layers.
In conclusion the advantages of graphene oxide method for comprehensive detection of the invention can include: method is easy, efficiently, energy
It is enough that organically various test is applied in combination, the type sum number of functional group on graphene oxide can be measured accurately, rapidly
Amount, while also can detect that the specific number of plies of graphene oxide.
Although those skilled in the art should be clear above by combining exemplary embodiment to describe the present invention
Chu can carry out exemplary embodiment of the present invention each without departing from the spirit and scope defined by the claims
Kind modifications and changes.
Claims (10)
1. a kind of graphene oxide method for comprehensive detection, which is characterized in that described detection method includes the following steps:
The first sample, the second sample and third sample are separated from graphene oxide, Fourier transform infrared is carried out to the first sample
Spectrum analysis test, obtains the infrared spectrogram of graphene oxide, carries out X-ray photoelectron spectroscopic analysis survey to the second sample
Examination, obtains the x-ray photoelectron spectroscopy figure of graphene oxide, carries out Raman spectrum test to third sample, obtains graphite oxide
The Raman spectrogram of alkene；
The type and quantity that functional group on graphene oxide is determined according to the infrared spectrogram and the energy spectrum diagram, according to described
Raman spectrogram determines the number of plies of graphene oxide, wherein
The step of functional group's type includes: to search middle infrared in the infrared spectrogram on the determining graphene oxide,
The corresponding wave number of absorption peak on the middle infrared is obtained, the wave number is compared with ir data library, determines oxygen
The type of graphite Xi Shang functional group；
The step of number of functional groups includes: to be judged in the energy spectrum diagram according to the size in conjunction with energy on the determining graphene oxide
The corresponding element in each peak, is modified by peak intensity of the sensitivity factor to peak corresponding to each element, passes through each member after amendment
Ratio between peak peak intensity corresponding to element obtains the relative amount ratio of each element, according to the relative amount ratio, determines oxidation stone
The quantity of Mo Xishang functional group；
The step of determining graphene oxide number of plies includes: to calculate I according to the Raman spectrogramG/I2D, work as IG/I2DIt is less than
When 1.0, tentatively judge graphene oxide for single or double layer structure；Work as IG/I2DWhen being 1.0~1.5, graphite oxide is tentatively judged
Alkene is 3 layers or 4 layers of structure；Work as IG/I2DWhen greater than 1.5, tentatively judge graphene oxide for 5 layers or more structures, wherein the IG
Indicate G peak intensity, the I2DIndicate 2D peak intensity.
2. graphene oxide method for comprehensive detection according to claim 1, which is characterized in that tentatively judging the oxidation
In the case that graphene is single or double layer structure, the 4th sample is separated from the graphene oxide, utilizes atomic force microscopy
Mirror tests the 4th sample, using the determination graphene oxide as single or double layer structure.
3. graphene oxide method for comprehensive detection according to claim 2, which is characterized in that described to utilize atomic force microscopy
The step of mirror tests the 4th sample includes: the 3 dimensional drawing that the 4th sample is obtained using atomic force microscope
Picture, and the graphene oxide thickness of thickness and single layer that the three-dimensional image is shown is compared, so that it is determined that oxidation stone
The black alkene number of plies is single or double layer.
4. graphene oxide method for comprehensive detection according to claim 1, which is characterized in that tentatively judging the oxidation
In the case that graphene is 3 layers or 4 layers of structure, the Lorentz of the peak the 2D fitting of the Raman test result Raman spectrogram is calculated
Power peak number, differentiating graphene oxide is 3 layers or 4 layers of structure.
5. graphene oxide method for comprehensive detection according to claim 1, which is characterized in that tentatively judging the oxidation
In the case that graphene is 5 layers or more structures, the 5th sample is separated from the graphene oxide, and electricity is transmitted by high-resolution
Mirror obtains the electron micrograph image of graphene oxide, and observation determines the specific number of plies of graphene oxide.
6. graphene oxide method for comprehensive detection according to claim 1, which is characterized in that the preliminary judgement aoxidizes stone
The step of black alkene is single or double layer structure includes: when the halfwidth at the peak 2D is 28cm-1~32cm-1And IG/I2DPeak it is strong
When the ratio between degree is less than 0.7, tentatively judge the graphene oxide for single layer structure；When the halfwidth at the peak 2D is 48cm-1~
52cm-1And IG/I2DWhen the intensity ratio at peak is more than or equal to 0.7 less than 1.0, tentatively judge the graphene oxide for bilayer knot
Structure.
7. graphene oxide method for comprehensive detection according to claim 1, which is characterized in that in the determining graphite oxide
After the step of Xi Shang functional group type, quantity, the method also includes: according to functional group's type of the determination and functional group
Quantity obtains the quantity of graphene oxide Shang Ge functional group.
8. the detection method of graphene oxide functional group according to claim 1, which is characterized in that the infrared spectrogram
On middle infrared wavelength be 2.5~25 μm.
9. the detection method of graphene oxide functional group according to claim 1, which is characterized in that
The middle infrared includes characteristic frequency area and fingerprint region, and the wavelength in the characteristic frequency area is 2.5~7.7 μm, described
The wavelength of fingerprint region is greater than 7.7 μm, is less than or equal to 25 μm.
10. graphene oxide method for comprehensive detection according to claim 1, which is characterized in that if element is in the power spectrum
Multiple peaks are corresponded on figure, then using the peak intensity of highest peak in the multiple peak as the modified object.
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