CN109342483A - A kind of doping graphene oxide detection method - Google Patents
A kind of doping graphene oxide detection method Download PDFInfo
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- CN109342483A CN109342483A CN201811573879.3A CN201811573879A CN109342483A CN 109342483 A CN109342483 A CN 109342483A CN 201811573879 A CN201811573879 A CN 201811573879A CN 109342483 A CN109342483 A CN 109342483A
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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]
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/071—Investigating materials by wave or particle radiation secondary emission combination of measurements, at least 1 secondary emission
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/084—Investigating materials by wave or particle radiation secondary emission photo-electric effect
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
Abstract
The present invention provides a kind of doping graphene oxide detection methods, it is characterized in that, obtain the x-ray photoelectron spectroscopy figure of doping graphene oxide to be measured, using can determine that doped chemical type except the new peak and the corresponding combination of new peak that occur in addition to the peak C 1S and the peak O lS, and according to the doping way of the corresponding combination energy location determination doping graphene oxide of new peak；The Raman spectrogram for obtaining doping graphene oxide to be measured determines that the doping way of doping graphene oxide is n-type doping in the case where the peak G blue shift and the red shift of the peak G'；In the case where the peak G blue shift and the peak G' blue shift, determine that the doping way of doping graphene oxide is p-type doping.Detection method of the invention can doped chemical type, doping way etc. to graphene oxide detect, can by x-ray photoelectron spectroscopy combined with Raman spectrum in the way of Accurate Analysis is carried out to the doping way of graphene oxide.
Description
Technical field
The present invention relates to graphene oxide detection technique fields, more particularly, are related to a kind of doping graphene oxide inspection
Survey method.
Background technique
Graphene (Graphene) is by sp2Plane hexagonal lattice knot made of the single layer of carbon atom close-packed arrays of hydridization
Structure, 4 electronics of C outermost layer carry out sp with the C atom of surrounding wherein 3 electronics participate in the bonding of graphene2Hydridization forms C-C
Key, remaining one electronically form can in graphene planes the free-moving big pi bond of delocalization.Graphene is logical in 2004 earliest
The lamellar graphite alkene that the method for crossing adhesive tape removing obtains, hereafter causes extensive research interest.Research finds that graphene has
Many excellent performances, as high-termal conductivity (5000W/mK), high carrier migrate (200000cm2V-1s-1), high-specific surface area
(2630m2/g), room-temperature quantum Hall effect etc..
Compared with graphene, the element of graphene oxide is formed and is not fixed, and there are hydroxyls (- OH), ring for graphene oxide
The oxygen-containing functional groups such as oxygroup [- C (O) C-], carbonyl (- C=O), carboxyl (- COOH), ester group (- COO-).Due to these oxygen-containing officials
The thickness of the presence that can be rolled into a ball, graphene oxide is much higher than graphene, makes its Partial Physical Property, such as electric conductivity, mechanical property etc.
It is greatly reduced.But these oxygen-containing functional groups make graphene oxide have good dispersibility and reactivity, graphene oxide
In oxygen-containing functional group etc. be easy to occur with the compound containing amino, carboxyl, isocyanate group etc. with reproducibility group it is anti-
It answers, various doping is carried out to graphene oxide to realize.
The doping for carrying out N, P, S etc. to graphene oxide can effectively adjust its band structure and physical and chemical performance.
Graphene oxide current density, methanol tolerance and good cyclical stability with higher are adulterated, and is mixed containing nitrogen, phosphorus atoms
Miscellaneous graphene oxide can be used as efficient flame-retarding agent, and crucial effect is played to graphene oxide fire-retardant film.It can be seen that
The identification for carrying out graphene oxide doped is very necessary.
Summary of the invention
It is above-mentioned existing in the prior art it is an object of the present invention to solving for the deficiencies in the prior art
One or more problems.For example, one of the objects of the present invention is to provide one kind can to graphene oxide doped element species,
The method that doping content, doping way are detected.
The present invention provides a kind of doping graphene oxide detection methods, in doping graphene oxide detection side of the invention
During one of method implements, the detection method be may comprise steps of: obtain the X-ray photoelectricity of doping graphene oxide to be measured
Sub- energy spectrum diagram can determine that doped chemical kind using except the new peak and the corresponding combination of new peak that occur in addition to the peak C lS and the peak O lS
Class, and determine that the doping way of doping graphene oxide is mixed for impurity or absorption according to the corresponding combination energy size of new peak
It is miscellaneous；The Raman spectrogram for obtaining doping graphene oxide to be measured determines doping oxygen in the case where the peak G blue shift and the red shift of the peak G'
The doping way of graphite alkene is n-type doping；In the case where the peak G blue shift and the peak G' blue shift, doping graphene oxide is determined
Doping way is p-type doping.
In the present embodiment, it is described obtain it is to be measured doping graphene oxide Raman spectrogram step may include, with to
It surveys doping graphene oxide Koln anomalous effect to weaken, be displaced at the peak G to high wave number, and the peak G' is to the case where lower wave number displacement
Under, determine that the doping way of doping graphene oxide is n-type doping；It is displaced at the peak G to high wave number, and the peak G' is displaced to high wave number
In the case where, determine that the doping way of doping graphene oxide is p-type doping.
In the present embodiment, the step of x-ray photoelectron spectroscopy figure for obtaining doping graphene oxide to be measured includes
Doped chemical content is determined according to new peak area ratio.
In the present embodiment, the step of x-ray photoelectron spectroscopy figure for obtaining doping graphene oxide to be measured includes
Swarming fitting is carried out to new peak, determines doped chemical chemical bond configuration type.
In the present embodiment, the corresponding area ratio in sub- peak after swarming fitting is carried out to new peak according to described, determination is mixed
Whether the percentage composition of miscellaneous element chemistry key configuration and determining doped chemical exist in the form of compound state.
In the present embodiment, the x-ray photoelectron spectroscopy figure step for obtaining doping graphene oxide to be measured includes root
It whether is absorption doping according to the doping method of doping graphene oxide described in the corresponding location determination in conjunction with energy of the new peak.
In the present embodiment, the doped chemical of the doping graphene oxide includes at least one of nitrogen, p and s.
In another implementation of doping graphene oxide detection method of the invention, the detection method includes following step
It is rapid: the x-ray photoelectron spectroscopy figure of doping graphene oxide to be measured is obtained, it is new using occurring in addition to the peak C lS and the peak O lS
Peak and the corresponding combination of new peak can determine that doped chemical type, and according to the corresponding combination energy location determination doping oxidation stone of new peak
The doping way of black alkene is impurity or absorption doping；The Raman spectrogram for obtaining doping graphene oxide to be measured, with to be measured
Adulterate graphene oxide Koln anomalous effect weaken, the peak G be displaced to high wave number and the peak G' to lower wave number displacement in the case where,
The doping way for determining doping graphene oxide is n-type doping；It is displaced to high wave number at the peak G, and the peak G' is displaced to high wave number
In the case of, determine that the doping way of doping graphene oxide is p-type doping.
In the present embodiment, it is wrapped in the step of x-ray photoelectron spectroscopy figure for obtaining doping graphene oxide to be measured
It includes and doped chemical content is determined according to new peak area ratio.
In the present embodiment, it is described obtain it is to be measured doping graphene oxide x-ray photoelectron spectroscopy figure the step of in
Including carrying out swarming fitting to new peak, doped chemical chemical bond configuration type is determined, and according to the sub- peak after the fitting of new peak swarming
Whether corresponding area ratio determines the percentage composition of doped chemical chemical bond configuration and determines doped chemical with compound state shape
Formula exists.
In the present embodiment, the doped chemical of the doping graphene oxide is at least one of nitrogen, p and s.
Compared with prior art, detection method of the invention can to doping graphene oxide doped chemical type, mix
Miscellaneous constituent content, chemical bond configuration, chemical bond configuration percentage are detected, and x-ray photoelectron spectroscopy and Raman can be utilized
The mode that spectrum combines carries out Accurate Analysis to the doping way of graphene oxide.
Specific embodiment
Hereinafter, doping graphene oxide detection side according to the present invention will be described in detail in conjunction with exemplary embodiment
Method.
The present invention provides a kind of doping graphene oxide detection methods, in doping graphene oxide detection side of the invention
In one exemplary embodiment of method, the detection method may include:
Step S01 obtains and analyzes the x-ray photoelectron spectroscopy figure of doping graphene oxide to be measured.
In the present embodiment, the XPS Momentum profiles figure of doping graphene oxide to be measured, x-ray photoelectron spectroscopy figure are analyzed
The number at (XPS map) peak and position can accurately provide the chemical bond present in doping graphene oxide, it is possible thereby to point
The element species of graphene oxide doped and the type of doping is precipitated.Specifically, graphene oxide only in 284.6eV and
Occur the peak C lS and O lS at 531.8eV, and in doping graphene oxide, removing in combination can be 284.6eV and 531.8eV
Locate to there is also new peak except corresponding peak.It can be determined that doping oxidation according to the new peak of appearance and the corresponding combination of new peak
Doped chemical type in graphene.Also, according to new peak to combination energy size (in conjunction with can size indicate to combine can be
Position is different in XPS map, i.e., different in conjunction with the positions at the different corresponding peaks of energy) it can also determine to adulterate the doping of graphene oxide
Mode is that impurity still adsorbs doping.For example, can intuitively can be determined according to the position of the corresponding combination energy of new peak
Whether doping graphene oxide is absorption doping.
Step S02 obtains and analyzes the Raman spectrogram of doping graphene oxide to be measured.
In the present embodiment, p-type or n-type doping will affect the Electron-phonon coupling of graphene, so as to cause Raman position
It moves.In Raman spectrogram (Raman spectrogram), in the case where the peak G blue shift and the red shift of the peak G', it is possible to determine that doping oxidation
The doping way of graphene is n-type doping.In the case where the peak G blue shift and the peak G' blue shift, it is possible to determine that doping graphene oxide
Doping way be p-type doping.
In the present embodiment, in described the step of obtaining the x-ray photoelectron spectroscopy figure to be measured for adulterating graphene oxide
Doped chemical content can also be determined according to the new peak area ratio of appearance.
It in the present embodiment, can in the step of x-ray photoelectron spectroscopy figure for obtaining doping graphene oxide to be measured
To carry out swarming fitting to new peak, doped chemical chemical bond configuration type is determined.And the son after being fitted according to new peak swarming
Whether the corresponding area ratio in peak determines the percentage composition of doped chemical chemical bond configuration and determines doped chemical with compound state
Form exists.Gauss swarming method can be used in the method for the swarming fitting.
In the present embodiment, the x-ray photoelectron spectroscopy figure step for obtaining doping graphene oxide to be measured can be with
It whether is absorption doping according to the doping method of doping graphene oxide described in the corresponding location determination in conjunction with energy of the new peak.
In the present embodiment, the doped chemical for including in the doping graphene oxide can be one in nitrogen phosphate and sulfur etc.
Kind is a variety of.
Specifically, for example, for phosphorus doping graphene oxide, phosphorus doping graphene oxide can except 284.6eV and
There are two peaks new peak P2p and P2s in position at 531.8eV.The ratio between peak area by calculating new peak can obtain doping oxidation stone
Black alkene doping content.The peak P2p occurs widthization and is in mal-distribution in two new peaks occurred, shows at least two kinds of chemical bond structures
Type exists.The peak P2p can be divided by two different sub- peak positions using Gauss swarming method, eachization can be calculated by each sub- peak area ratio
The percentage composition for learning key configuration, is obtained doped chemical and is present in graphite linings grid in the form of compound state, thus can also identified
For impurity.Also, it can also identify whether doping graphene oxide belongs to suction according to the binding site of doped chemical
Attached doping.
In another exemplary embodiment of doping graphene oxide detection method of the invention, the detection method can
To include:
Step S100 obtains and analyzes the x-ray photoelectron spectroscopy figure of graphene oxide to be measured.
In this implementation implementation, correlation analysis idea in this step S100 is related in step S01 described above to divide
Analysis method is consistent.
Step S200 obtains and analyzes the Raman spectrogram of doping graphene oxide to be measured.
In the present embodiment, for the graphene oxide after doping, the Raman G summit of the graphene oxide after doping
With its Koln anomalous effect (Kohn anomaly) weaken and to high wave number be displaced, and the peak G' in n-type doping to lower wave number position
It moves, to high wave number position when p-type doping, it is possible thereby to determine the doping graphene oxide for n-type doping or p-type doping.
More than, detection method of the invention is equally applicable to the detection of attribute of doping redox graphene.
In conclusion the detection method of invention can doped chemical type to graphene oxide, doped chemical content, change
Learn key configuration, chemical bond configuration percentage is detected, the side that can be combined using x-ray photoelectron spectroscopy with Raman spectrum
Formula carries out Accurate Analysis to the doping way 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 (5)
1. a kind of doping graphene oxide detection method, which is characterized in that described detection method includes the following steps:
The x-ray photoelectron spectroscopy figure for obtaining doping graphene oxide to be measured, utilizes what is occurred in addition to the peak C 1S and the peak O lS
New peak and the corresponding combination of new peak can determine that doped chemical type, and determine doping oxidation according to the corresponding combination energy size of new peak
The doping way of graphene is impurity or absorption doping；
The Raman spectrogram for obtaining doping graphene oxide to be measured, determines that doping graphene oxide to be measured is mixed for n-type doping or p-type
Miscellaneous, determination method includes:
In the case where the peak G blue shift and the red shift of the peak G', determine that the doping way of doping graphene oxide is n-type doping；At the peak G
Blue shift, and in the case where the peak G' blue shift, determine that the doping way of doping graphene oxide is p-type doping；
Or determination method includes:
Weaken with doping graphene oxide Koln anomalous effect to be measured, be displaced at the peak G to high wave number, and the peak G' is displaced to lower wave number
In the case where, determine that the doping way of doping graphene oxide is n-type doping；It is displaced at the peak G to high wave number, and the peak G' is to Gao Bo
In the case that numerical digit is moved, determine that the doping way of doping graphene oxide is p-type doping.
2. doping graphene oxide detection method according to claim 1, which is characterized in that described to obtain doping oxygen to be measured
The step of x-ray photoelectron spectroscopy figure of graphite alkene includes determining doped chemical content according to the new peak area ratio of appearance.
3. doping graphene oxide detection method according to claim 1, which is characterized in that described to obtain doping oxygen to be measured
The step of x-ray photoelectron spectroscopy figure of graphite alkene includes carrying out swarming fitting to new peak, determines doped chemical chemical bond structure
Type type.
4. doping graphene oxide detection method according to claim 3, which is characterized in that carried out according to described to new peak
The corresponding area ratio in sub- peak after swarming fitting determines the percentage composition of doped chemical chemical bond configuration and determines doping member
Whether element exists in the form of compound state.
5. doping graphene oxide detection method according to claim 1, which is characterized in that the doping graphene oxide
Doped chemical include at least one of nitrogen, p and s.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103407989A (en) * | 2013-06-24 | 2013-11-27 | 温州医学院 | Low-temperature environmentally-friendly preparation method of nitrogen edge doped graphene |
| CN105366662A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Preparing method for sulfur-doped graphene |
| CN108439386A (en) * | 2018-05-23 | 2018-08-24 | 大同新成新材料股份有限公司 | A kind of preparation method of graphene |
-
2018
- 2018-12-21 CN CN201811573879.3A patent/CN109342483A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103407989A (en) * | 2013-06-24 | 2013-11-27 | 温州医学院 | Low-temperature environmentally-friendly preparation method of nitrogen edge doped graphene |
| CN105366662A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Preparing method for sulfur-doped graphene |
| CN108439386A (en) * | 2018-05-23 | 2018-08-24 | 大同新成新材料股份有限公司 | A kind of preparation method of graphene |
Non-Patent Citations (2)
| Title |
|---|
| 吴娟霞 等: "《拉曼光谱在石墨烯表征中的应用》", 《化学学报》 * |
| 田恐虎: "《聚合物基石墨烯复合材料的制备和电磁屏蔽性能研究》", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
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