CN108490015A - A kind of determination method of oxygen-containing graphene reducing degree - Google Patents
A kind of determination method of oxygen-containing graphene reducing degree Download PDFInfo
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- CN108490015A CN108490015A CN201810213828.3A CN201810213828A CN108490015A CN 108490015 A CN108490015 A CN 108490015A CN 201810213828 A CN201810213828 A CN 201810213828A CN 108490015 A CN108490015 A CN 108490015A
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- oxygen
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/227—Measuring photoelectric effect, e.g. photoelectron emission microscopy [PEEM]
- G01N23/2273—Measuring photoelectron spectrum, e.g. electron spectroscopy for chemical analysis [ESCA] or X-ray photoelectron spectroscopy [XPS]
Abstract
The invention discloses a kind of determination methods of oxygen-containing graphene reducing degree, including：(1) sample to be tested is measured using x-ray photoelectron spectroscopy, the energy range of scanning is 280eV to 295eV, obtains the xps energy spectrum of sample to be tested C 1s；(2) obtained xps energy spectrum is subjected to swarming fitting, adjustment halfwidth, area, peak shape；(3) by step (2) obtain as a result, judging the reducing degree of oxygen-containing graphene according to the ratio between oxygen-containing functional group total content and C C linkage contents.The present invention can be achieved carbon chemical structure analysis, can by oxygen-containing functional group total content and C C linkage contents work compare, oxygen-containing functional group combine can position compare, realize the judgement of different sample reducing degrees.Invention has the advantages that accurate, quick, undamaged.
Description
Technical field
The invention belongs to test and analysis technology fields, and in particular to a kind of determination method of oxygen-containing graphene reducing degree.
Background technology
Graphene (Graphene) is that one kind can be independently with sp2The standard two of single carbon atom layer thickness existing for hybrid form
(2D) atomic crystal is tieed up, is in planar honeycomb shape, it is current most thin material, and has the peculiar property of tough and tensile densification, again
It is called monoatomic layer graphite.2004, the method for first passage adhesive tape stripping graphite obtained.Currently, preparing for graphene is main
Including：Micromechanics stripping method, chemical vapour deposition technique, epitaxial growth method, graphene oxide reduction method and organic synthesis method etc..
Graphene oxide (Graphene Oxide, abbreviation GO) reduction method is easy to operate, yield is big, while graphene sol
Product Form also allow for the further processing and molding of material.What the graphite after peroxidating intercalation occurred due to its piece interlayer
The oxygen-containing groups such as carbonyl, hydroxyl make graphite layers away from becoming larger.It is strong mutually due to oxygen-containing group and hydrone in aqueous solvent
Effect, can be removed graphene oxide layer using mechanisms such as ultrasonic vibrations, and dispersion in the solution forms GO colloids.With
Afterwards, redox graphene (Reduced Graphene Oxide, letter can be prepared by GO being carried out reduction using some way
Claim RGO).
It, can be by connecing containing being a kind of persursor material of extraordinary functionalization graphene there are many GO of oxygen-containing group
Branch or chemical modification obtain.But the graphene oxidizability that different method for oxidation obtain is different, and then material property is caused to have very
Big difference.In recent years, researcher has found that many active groups, such as carbonyl, carboxyl and epoxy group are contained in graphite oxide surface,
These groups are easily chemically reacted with other substances, and the modification of graphene is made to be provided with feasibility.The modification of graphene with
Carbon nanotube is identical with the mechanism of modification of fullerene, is all that there are a large amount of active groups to lead to inert stone originally for plane of crystal
Black alkene surface also becomes very active.One of the important way that the surface of graphene is modified is introduced on the boundary of chemical constitution
Functional group carries out chemical modification.The type, how many of graphene degree of oxidation, oxygen-containing functional group, can all influence the grafting of graphene
Or chemical modification.Graphene surface can connect a large amount of oxygen-containing group (hydroxyl, aldehyde radical, carboxyl, ehter bond etc.), these groups are with altogether
Valence form is connected on carbon, leverages the electronic property of graphene；Grapheme material is in composite material, surface heavy antisepsis etc.
In, needs to introduce effective functional group by the methods of graphene oxide reduction or plasma treatment, control going back for graphene
Former and functionalization degree, reaches different application requirements.The redox of Accurate Determining grapheme material and functionalization degree, are commented
Valence material quality, especially thin-film material surface are particularly important.
Currently, graphene oxide reducing degree is mostly weighed with O/C ratios in the prior art, but x-ray photoelectron spectroscopy is table
The easy surface contamination of sample of surface analysis and air contact, it is higher that oxygen adsorbs content.The present invention utilizes x-ray photoelectron spectroscopy solution
Spectrum analysis, oxygen-containing functional group and C-C keys make ratio in being composed by carbon, and oxygen-containing functional group C=O, C-O ,-COOH are combined can position change
Change, realizes graphene oxide, the evaluation of reduced graphene reducing degree.
Invention content
It is an object of the present invention to provide it is a kind of have quickly, accurately analyze graphene oxide, reduced graphene reducing degree
Determination method, realize it is not damaged, conveniently, simple reducing degree evaluation.
The technical solution adopted by the present invention is as follows：
A kind of determination method of oxygen-containing graphene reducing degree, including：
(1) sample to be tested is measured using x-ray photoelectron spectroscopy, the energy range of scanning be 280eV extremely
295eV obtains the xps energy spectrum of sample to be tested C 1s；
(2) obtained xps energy spectrum is subjected to swarming fitting, adjustment halfwidth, area, peak shape；
(3) by step (2) obtain as a result, being judged according to the ratio between oxygen-containing functional group total content and C-C linkage contents oxygen-containing
The reducing degree of graphene.
The present invention is with x-ray photoelectron spectroscopy (XPS) for main detection means, and Spectrum stripping techniques in analysis is analysis means, to obtaining
Graphene oxide, reduced graphene carbon spectrum parsed.Since graphene reducing degree is higher, oxygen content is smaller, spectrogram solution
Oxygen-containing functional group content is fewer after analysis, and the content ratio of oxygen-containing functional group and C-C keys reduces, and oxygen content is fewer, oxygen-containing function
Group combines energy position lower, according to such relationship, conveniently accurately can judge oxygen-containing graphene reducing degree size.
Preferably, the size that reducing degree between sample to be tested is compared by comparing the combination energy position of oxygen-containing functional group, contains
Oxygen functional groups can be smaller, and reducing degree is bigger.
Preferably, in step (1), measuring condition includes：Step-length is 0.05eV or 0.1eV, open score it is logical can for 20eV or
40eV, neutralization rifle electric current are 1.5~1.8A, and neutralization rifle voltage is 2.0~3.6V, and X-ray electric current is 8~10A, X-ray voltage
For 10~15V.
The oxygen-containing graphene refers to the graphene containing oxygen-containing group, including graphene oxide (GO) and reduction-oxidation graphite
Alkene (RGO).
The present invention is suitable for all oxygen-containing graphenes, hinders to sample nondestructive, when carrying out xps energy spectrum acquisition, phase can be used
Same test condition.When being fitted swarming, adjustment halfwidth, area, peak shape, according to oxygen-containing functional group total content and C-C linkage contents
The ratio between and oxygen-containing functional group the oxygen-containing graphene of combination energy location estimating reducing degree.
Compared with prior art, the present invention has the advantages that：
(1) present invention quickly, accurately, hinders sample nondestructive, convenient to device without stripping if it is substrate deposition sample
Part is processed and performance test.
(2) the content ratio of oxygen-containing functional group and C-C keys is obtained by analysis spectrogram and each oxygen-containing functional group combines energy position
It sets variation tendency and can determine whether reducing degree, while the existence of C can also be analyzed, applied convenient for follow-up grafting.
Description of the drawings
Fig. 1 is that graphite oxide olefinic carbon composes swarming fitted figure；
Fig. 2 is that reduced graphene carbon composes swarming fitted figure.
Specific implementation mode
In order to further appreciate that present disclosure, feature and effect, spy enumerates following embodiment, and attached drawing is coordinated to make
It is described in detail.
Embodiment 1
(1) it selectes graphene oxide respectively first and redox graphene carries out x-ray photoelectron spectroscopy test, scanning
Region：300*700um, the energy range 280eV to 295eV of scanning, step-length 0.05eV, the logical energy 20eV of open score, neutralize rifle electric current
1.8A neutralizes rifle voltage 3.6V, X-ray electric current 8A, X-ray voltage 12V, x-ray power 96W.
(2) swarming Fitting Analysis, adjustment halfwidth, area, peak shape are carried out to carbon spectrum (C 1s).Pass through " Gauss Lorentz lorentz
Linear fit method " is divided according to " GB/T 30704-2014 surface chemist reaction X-ray photoelectron spectroscopic analysis guide "
Analysis.Halfwidth is adjusted according to instrumental resolution between 1 and 3, obtains graphene oxide, reduced graphene carbon composes each combinations of states
Energy position, as shown in table 1.Graphite oxide olefinic carbon composes swarming fitted figure as shown in Figure 1, reduced graphene carbon composes swarming fitted figure such as
Shown in Fig. 2.
Table 1
As known from Table 1, graphene oxide oxygen-containing functional group and sp2+sp3Content ratio be 1.07；The oxygen-containing official of reduced graphene
It can group and sp2+sp3Content ratio be 0.23.Therefore, sample to be tested oxygen-containing functional group is more, the oxygen-containing function obtained after swarming
Group/sp2+sp3Bigger, sample to be tested degree of oxidation is bigger；Otherwise smaller, sample to be tested reducing degree is bigger.
In addition, the sample to be tested of different reducing degrees, oxygen-containing functional group combines energy position also different, and reducing degree is bigger,
In conjunction with can be lower；Conversely, degree of oxidation is higher, oxygen-containing functional group combines energy position higher.Graphene oxide C-O, C=O, COOH
The combination of state can be respectively 287.2eV, 287.9eV and 289.4eV.The combination of reduced graphene C-O, C=O, COOH state
Energy position is respectively 286.2eV, 287.6eV and 289eV；Wherein, graphene oxide C-O is higher by 1eV than reduced graphene.
Therefore, being combined according to the ratio between oxygen-containing functional group total content and C-C linkage contents and oxygen-containing functional group can change in location
It can be determined that oxygen-containing graphene reducing degree.
Embodiment 2
(1) X-ray photoelectricity is carried out to graphene oxide sample A1 and redox graphene sample A2 and A3 respectively first
Sub- power spectrum test, scanning area：110um, the energy range 280eV to 295eV of scanning, step-length 0.1eV, the logical energy 40eV of open score,
Rifle electric current 1.6A is neutralized, rifle voltage 2.6V, X-ray electric current 10A, X-ray voltage 12V, x-ray power 120W are neutralized.
(2) after to carbon spectrum (C 1s) calibration, by " Gauss Lorentz lorentz linear fit method ", according to " GB/T 30704-
2014 surface chemist reaction X-ray photoelectron spectroscopic analysis guides " are analyzed.Halfwidth is adjusted in 1- according to instrumental resolution
Between 3, graphene oxide sample A1, redox graphene sample A2 and A3 carbon spectrum C-C (sp are obtained2、sp3), C-O, C=O,
Each combinations of states energy of COOH, π-π * position.
Wherein, graphene oxide sample A1 oxygen-containing functional groups and C-C (sp2+sp3) content ratio be 1.03；Oxygen reduction fossil
Black alkene sample A2 and A3 oxygen-containing functional group and C-C (sp2+sp3) content respectively than being 0.22,0.20.Therefore, sample to be tested contains
Oxygen functional group is more, the oxygen-containing functional group/C-C (sp obtained after swarming2+sp3) bigger, sample to be tested degree of oxidation is bigger；Instead
It is smaller, sample to be tested reducing degree is bigger.
In addition, the sample to be tested of different reducing degrees, oxygen-containing functional group combines energy position also different, and reducing degree is bigger,
In conjunction with can be lower；Conversely, degree of oxidation is higher, oxygen-containing functional group combines energy position higher.Graphene oxide sample A1C-O, C=
O, the combination of COOH states can be respectively 287.1eV, 287.8eV and 289.3eV.Redox graphene sample A2C-O, C=
O, the combination energy position of COOH states is respectively 286.2eV, 287.7eV and 289.1eV, redox graphene sample A3C-O,
The combination energy position of C=O, COOH state is respectively 286.1eV, 287.6eV and 289.0eV.
It integrates the ratio between oxygen-containing functional group total content and C-C linkage contents and oxygen-containing functional group is combined energy position, it is possible to determine that,
In above-mentioned sample, the reducing degree of the reducing degree highest of redox graphene sample A3, graphene oxide sample A1 is minimum.
Claims (6)
1. a kind of determination method of oxygen-containing graphene reducing degree, which is characterized in that including：
(1) sample to be tested is measured using x-ray photoelectron spectroscopy, the energy range of scanning is 280eV to 295eV, is obtained
To the xps energy spectrum of sample to be tested C 1s；
(2) obtained xps energy spectrum is subjected to swarming fitting, adjustment halfwidth, area, peak shape；
(3) by step (2) obtain as a result, judging oxygen-containing graphite according to the ratio between oxygen-containing functional group total content and C-C linkage contents
The reducing degree of alkene.
2. the determination method of oxygen-containing graphene reducing degree according to claim 1, which is characterized in that by comparing oxygen-containing
The size of reducing degree between sample to be tested is compared in the combination energy position of functional group, and oxygen-containing functional group combines can smaller, reducing degree
It is bigger.
3. the determination method of oxygen-containing graphene reducing degree according to claim 1, which is characterized in that in step (1), survey
Amount condition includes：Step-length is 0.05eV or 0.1eV, and it can be 20eV or 40eV that open score is logical.
4. the determination method of oxygen-containing graphene reducing degree according to claim 1, which is characterized in that in step (1), survey
Amount condition includes：Neutralization rifle electric current is 1.5~1.8A, and neutralization rifle voltage is 2.0~3.6V.
5. the determination method of oxygen-containing graphene reducing degree according to claim 1, which is characterized in that in step (1), survey
Amount condition includes：X-ray electric current is 8~10A, and X-ray voltage is 10~15V.
6. the determination method of oxygen-containing graphene reducing degree according to claim 1, which is characterized in that the oxygen-containing graphite
Alkene refers to the graphene containing oxygen-containing group, including graphene oxide and redox graphene.
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Cited By (6)
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| CN109342353A (en) * | 2018-12-21 | 2019-02-15 | 四川聚创石墨烯科技有限公司 | A method of judging carbon material type |
| CN109540826A (en) * | 2018-12-21 | 2019-03-29 | 四川聚创石墨烯科技有限公司 | A kind of detection method of graphene oxide functional group |
| CN109540827A (en) * | 2018-12-21 | 2019-03-29 | 四川聚创石墨烯科技有限公司 | A kind of graphene oxide method for comprehensive detection |
| CN109580676A (en) * | 2018-12-21 | 2019-04-05 | 四川聚创石墨烯科技有限公司 | A method of determining whether carbon material is graphene oxide |
| CN109613030A (en) * | 2018-12-21 | 2019-04-12 | 四川聚创石墨烯科技有限公司 | A method of determining whether carbon material is doping graphene oxide |
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Application publication date: 20180904 |