CN108398577A - The test method of the reducing degree of graphene oxide - Google Patents
The test method of the reducing degree of graphene oxide Download PDFInfo
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- CN108398577A CN108398577A CN201810091508.5A CN201810091508A CN108398577A CN 108398577 A CN108398577 A CN 108398577A CN 201810091508 A CN201810091508 A CN 201810091508A CN 108398577 A CN108398577 A CN 108398577A
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- graphene oxide
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- point bias
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
Abstract
The invention discloses a kind of test methods of the reducing degree of graphene oxide comprising step：S1, electrostatic force microscope figure of the reduction-state graphene oxide under different needle point biass is measured using electrostatic force microscope；S2, it is mapped to needle point bias with the phase of reduction-state graphene oxide described in electrostatic force microscope figure, obtains phase needle point bias plot；S3, size of the reduction-state graphene oxide compared with the reducing degree of graphene oxide is determined according to phase needle point bias plot.The present invention is changed by the peak position and peak intensity for comparing phase needle point bias plot, the characterization of nanoscale can be carried out to the reducing degree difference of monolithic layer reduction-state graphene oxide sample after graphene oxide sample is by different restoring method homogeneous reductions；Compared with prior art, the supplement that initial reduction stage of reaction method can be characterized as electrostatic force microscope and scanning polarization force microscope etc., to enrich the characterization approach in graphene oxide research process.
Description
Technical field
The invention belongs to graphene oxide characterization test technical fields, it relates in particular to which a kind of graphene oxide is gone back
The test method of former degree.
Background technology
It is important technology in graphene oxide research field that the reducing degree of graphene oxide, which is characterized and measured,.
In many technologies of current characterization test graphene oxide, traditional spectrum method, the conductance based on microelectrode
Rate test method can only characterize the generation of the reduction reaction of graphene oxide, but provide be test sample average letter
Breath, cannot characterize the reduction reaction of the single-layer oxidized graphite alkene of dispersion in nanoscale；Optical observation and transmission electricity
Sub- microscope can provide the variation of the color change and atomic structure information of the front and back graphene oxide of reduction respectively, however can not
The difference in performance is provided, therefore is difficult to distinguish the reduction-state graphene oxide layer with minor differences on reducing degree.
Currently, the variation based on graphene oxide electrical properties before and after reduction, such as conductive atom of scanning probe microscopy
Force microscope, electrostatic force microscope and scanning polarization force microscope etc. be used to characterize going back for graphene oxide in nanoscale
Original, but electrical return is constituted due to being operated between contact mode and probe and test sample when conducting atomic force microscopy measures,
The electricity for being easy to generate test sample reduction or oxidation induces, and then influences the reducing degree of test sample；Although electrostatic force is aobvious
Micro mirror and scanning polarization force microscope can characterize the process that graphene oxide is gradually reduced, but when reduction reaction is entire
When uniformly occurring on lamella, it is difficult to characterize the reducing degree difference between the graphene oxide layer of distinct methods reduction.
Invention content
To solve the above-mentioned problems of the prior art, the present invention provides a kind of surveys of the reducing degree of graphene oxide
Method for testing, the test method are carried out based on electrostatic force microscope figure, are realized under nanosecond yardstick surface features difference restoring method
The difference of the reducing degree of the reduction-state graphene oxide layer of obtained entire lamella homogeneous reduction.
In order to reach foregoing invention purpose, present invention employs the following technical solutions：
A kind of test method of the reducing degree of graphene oxide, including step：
S1, electrostatic force microscope of the reduction-state graphene oxide under different needle point biass is measured using electrostatic force microscope
Figure；
S2, it is mapped, is obtained to needle point bias with the phase of reduction-state graphene oxide described in the electrostatic force microscope figure
Obtain phase-needle point bias plot；
S3, the reduction-state graphene oxide going back compared with graphene oxide is determined according to the phase-needle point bias plot
The size of former degree；Wherein, in the phase-needle point bias plot, the corresponding specific needle point of peak value or valley of phase is inclined
The absolute value of pressure is smaller, and/or bigger less than the absolute value of the phase under any needle point bias of the specific needle point bias, then
Its corresponding reduction-state graphene oxide is higher compared with the reducing degree of graphene oxide.
Further, in the step S1, ranging from -12V~12V of needle point bias.
Further, in the step S1, it is divided into 1V between needle point bias.
Further, the reduction-state graphene oxide to graphene oxide by carrying out thermal reduction and/or electronation
It obtains.
Further, electronation is that the graphene oxide is placed in saturation hydrazine hydrate steam to restore.
The present invention by using electrostatic force microscope figure method, by compare phase-needle point bias plot peak position and
Peak intensity changes, can be after graphene oxide sample is by different restoring method homogeneous reductions, to monolithic layer reduction-state graphite oxide
The reducing degree difference of alkene sample carries out the characterization of nanoscale；Compared with prior art, can be used as electrostatic force microscope and
Scanning polarization force microscope etc. characterizes the supplement of initial reduction stage of reaction method, in abundant graphene oxide research process
Characterization approach.
Description of the drawings
What is carried out in conjunction with the accompanying drawings is described below, above and other aspect, features and advantages of the embodiment of the present invention
It will become clearer, in attached drawing：
Fig. 1 is the step flow chart of the test method of the reducing degree of graphene oxide according to the present invention；
Fig. 2 is according to an embodiment of the invention 0 in 1#~5#The phase of sample-needle point bias plot；
Fig. 3 is according to an embodiment of the invention 0 in 1#The atomic force microscope shape appearance figure of sample；Wherein white scale indicates
1000nm；
Fig. 4 is according to an embodiment of the invention 0 in 1#Electrostatic force when sample and the needle point bias of the original positions Fig. 3 are 0V is micro-
Mirror figure；
Fig. 5 is according to an embodiment of the invention 0 in 1#Electrostatic force when sample and the needle point bias of the original positions Fig. 3 are 5V is micro-
Mirror figure；
Fig. 6 is according to an embodiment of the invention 0 in 1#Electrostatic force when sample and the needle point bias of the original positions Fig. 3 are -5V is aobvious
Micro mirror figure；
Fig. 7 is according to an embodiment of the invention 1 in 1#Electrostatic force microscope figure when the needle point bias of sample is 5V；Wherein
White scale indicates 1000nm；
Fig. 8 is according to an embodiment of the invention 1 in 1#Electrostatic force when sample and the needle point bias of the original positions Fig. 7 are -5V is aobvious
Micro mirror figure；
Fig. 9 is according to an embodiment of the invention 2 in 1#Electrostatic force microscope figure when the needle point bias of sample is 5V；Wherein
White scale indicates 1000nm；
Figure 10 is according to an embodiment of the invention 2 in 1#Electrostatic force when sample and the needle point bias of the original positions Fig. 9 are -5V is aobvious
Micro mirror figure；
Figure 11 is according to an embodiment of the invention 3 in 1#Electrostatic force microscope figure when the needle point bias of sample is 5V；Its
Middle white scale indicates 1000nm；
Figure 12 is according to an embodiment of the invention 3 in 1#Electrostatic force when sample and the needle point bias of the original positions Figure 11 are -5V
Microscope figure；
Figure 13 is according to an embodiment of the invention 4 in 1#Electrostatic force microscope figure when the needle point bias of sample is 5V；Its
Middle white scale indicates 1000nm；
Figure 14 is according to an embodiment of the invention 4 in 1#Electrostatic force when sample and the needle point bias of the original positions Figure 13 are -5V
Microscope figure；
Figure 15 is according to an embodiment of the invention 5 in 1#Electrostatic force microscope figure when the needle point bias of sample is 5V；Its
Middle white scale indicates 1000nm；
Figure 16 is according to an embodiment of the invention 5 in 1#Electrostatic force when sample and the needle point bias of the original positions Figure 15 are -5V
Microscope figure；
Figure 17 is 0 in comparative example 1 according to the present invention#Sample and 5#The parsing x-ray photoelectron spectroscopy test spectrum of sample
Figure；
Figure 18 is 0 in comparative example 1 according to the present invention#~5#The x-ray photoelectron spectroscopy of sample tests spectrogram；
Figure 19 is 0 in comparative example 2 according to the present invention#~5#The normalization ultraviolet-visible absorption spectroscopy spectrogram of sample；
Figure 20 is 0 in comparative example 3 according to the present invention#The scanning polarization force microscope figure of sample；
Figure 21 is 0 with the original positions Figure 20 in comparative example 3 according to the present invention#Sample restores sweeping after 15min at 150 DEG C
Retouch polarization force microscope figure；
Figure 22 is 0 with the original positions Figure 20 in comparative example 3 according to the present invention#Sample restores sweeping after 75min at 150 DEG C
Retouch polarization force microscope figure；
Figure 23 is 1 in comparative example 3 according to the present invention#The scanning polarization force microscope figure of sample；Wherein, in white box
It is in situ 1#The atomic force microscope shape appearance figure of sample；White scale indicates 1000nm；
Figure 24 is 0 in comparative example 3 according to the present invention#Sample and 5#The atomic force microscope shape appearance figure of the mixture of sample；
Wherein white scale indicates 1000nm；
Figure 25 is 0 with the original positions Figure 24 in comparative example 3 according to the present invention#Sample and 5#The scanning pole of the mixture of sample
Change force microscope figure；
Figure 26 is 5 in comparative example 3 according to the present invention#The atomic force microscope shape appearance figure of sample；Wherein white scale table
Show 1000nm；
Figure 27 is 5 with the original positions Figure 26 in comparative example 3 according to the present invention#The scanning polarization force microscope figure of sample.
Specific implementation mode
Hereinafter, with reference to the accompanying drawings to detailed description of the present invention embodiment.However, it is possible to come in many different forms real
The present invention is applied, and the present invention should not be construed as limited to the specific embodiment illustrated here.On the contrary, providing these implementations
Example is in order to explain the principle of the present invention and its practical application, to make others skilled in the art it will be appreciated that the present invention
Various embodiments and be suitable for the various modifications of specific intended application.
The invention discloses a kind of test methods of the reducing degree of graphene oxide, as shown in Figure 1 comprising Xia Shubu
Suddenly：
In step sl, electrostatic of the reduction-state graphene oxide under different needle point biass is measured using electrostatic force microscope
Force microscope figure.
Specifically, reduction-state graphene oxide be by graphene oxide carry out thermal reduction and/or electronation obtain
；Wherein, graphene oxide is preferably placed in saturation hydrazine hydrate steam and restores by electronation.
For graphene oxide, the test scope of needle point bias is -12V~12V, is preferably spaced 1V.
In step s 2, it is mapped, is obtained to needle point bias with the phase of reduction-state graphene oxide in electrostatic force microscope figure
Obtain phase-needle point bias plot.
In step s3, reduction-state graphene oxide going back compared with graphene oxide is determined according to phase-needle point bias plot
The size of former degree.
Specifically, in phase-needle point bias plot, the corresponding specific needle point bias of peak value or valley of phase it is exhausted
It is smaller, and/or bigger less than the absolute value of the phase under any needle point bias of the specific needle point bias to being worth, then show that its is right
The reduction-state graphene oxide answered is higher compared with the reducing degree of graphene oxide.
In this way, above-mentioned determination method according to the present invention, you can by relatively being aoxidized to different reduction-state graphene oxides
The reducing degree of graphene is compared.
In order to illustrate the advantageous effect of above-mentioned test method, the reduction that different modes are carried out using graphene oxide is obtained not
Same sample, and accordingly measured, as described in following embodiments 1.
Embodiment 1
Specifically, sample is prepared using following methods：First, by the graphene oxide of 10 a concentration of 0.5mg/mL of μ L
(graphene oxide, GO) suspension drips to the mica surface of new cleavage, is dried up with ear washing bulb after adsorbing 30s, obtains GO samples
Product；Then, GO samples are restored using distinct methods, respectively obtains reduction-state graphene oxide (reduced
Graphene oxide, rGO) sample.
More specifically, above-mentioned GO samples are restored with reference to the method in following table 1.
1 sample number into spectrum of table and acquisition condition
In the range of the needle point bias of -12V~12V, using the interval of 1V, respectively to 0#~5#Sample carries out electrostatic force
Microscopical measurement；It is in each width electrostatic force microscope figure of acquisition, i.e., corresponding to generate a phase value.
In this way, i.e. corresponding per a sample generate 25 phase values, using these phase values as ordinate, with its corresponding needle
Sharp bias makes phase-needle point bias plot as abscissa；As shown in Figure 2.
Six phases-needle point bias plot according to fig. 2, determining peak value or valley per a sample and its corresponding needle point
Bias；As shown in table 2.
Table 20#~5#The peak value or valley and its corresponding needle point bias of the phase of sample-needle point bias plot
From figure 2 it can be seen that 0#The phase of sample is positive value, and 1#~5#The phase of sample is negative value, illustrate by
0#Sample is to 1#~5#Reduction reaction has occurred in sample；And from 1#Sample variation is to 5#Sample, phase contrast significantly increase, such as
In Fig. 2 shown in dotted line.In conjunction with table 2 as can be seen that 1#~5#In sample, the absolute value of the corresponding specific needle point bias of valley
It is sequentially reduced, shows the reducing degree of sample according to 1#Sample is to 5#The sequence of sample is deepened, as shown in lateral arrows in Fig. 2；And
1#~5#In sample, it is less than any needle point bias pair of above-mentioned specific needle point bias (peak value or the corresponding needle point bias of valley)
The absolute value for the phase answered successively increases, and also indicates that the reducing degree of sample according to 1#Sample is to 5#The sequence of sample is deepened, and is such as schemed
In 2 shown in longitudinal arrow.It follows that in the present embodiment, 0#~5#The reducing degree of sample is to deep sequence from shallow：0#Sample
Product ＜ 1#Sample ≈ 2#Sample ＜ 3#Sample ≈ 4#Sample ＜ 5#Sample.
That is, in the test method of the present embodiment, according to phase-needle point bias figure, the peak value or valley of phase
Phase under the smaller, and/or any needle point bias less than the specific needle point bias of the absolute value of corresponding specific needle point bias
Absolute value it is bigger, then show that its corresponding reduction-state graphene oxide is higher compared with the reducing degree of graphene oxide.
In addition, from figure 2 it can be seen that phase contrast significantly increases at dotted line, therefore respectively illustrate 0#~5#Sample
Respectively -5V, 5V needle point bias under electrostatic force microscope figure use atom first and in order to compare in-site detecting effect
Force microscope (Atomic Force Microscope, AFM) is to 0#Sample is characterized, as shown in Figure 3；It is quiet in order to show
The raised mode of force microscope imaging has had been removed the influence of topographical information, aobvious using the electrostatic force under the needle point bias of 0V
Micro mirror pair 0#Sample has carried out the characterization with the original positions Fig. 3, as shown in figure 4, not having the influence of any topographical information in entire figure；0#
~5#Sample respectively -5V, 5V needle point bias under electrostatic force microscope figure respectively as shown in Fig. 5~Figure 16, from Fig. 5~figure
It is evident that its corresponding phase in 16.
In order to further verify the advantageous effect of test method shown in above-described embodiment 1, using other characterization methods
To above-mentioned 0#~5#Sample is characterized, as shown in following comparative examples 1~3.
Comparative example 1
In this comparative example, using x-ray photoelectron spectroscopy test (X-ray photoelectronspectroscopy,
XPS 0) is characterized respectively#~5#Sample.
Figure 17 shows 0#Sample and 5#The parsing x-ray photoelectron spectroscopy of sample tests spectrogram, that is, the knot to deconvolute
Close can be 284.5eV, 285.5eV, 286.9eV and 288.5eV peak (being indicated respectively with a, c, b, d), this four classes peak generation respectively
Table C=C/C (aromatic rings), C-O (epoxy group and alkoxy), C=O and COOH group.As can be seen from Figure 17, sample is also
(5 after original#Sample) XPS spectrum in the carbon atom that is combined with oxygen significantly reduced, shown most oxygen-containing functional group
It is removed；And can be obtained from XPS data, for the sample (5 after electronation#Sample), carbon atom in aromatic rings with contain
Carbon atomic ratio in oxygen functional group is from initial 1.1:1 increases to 6.3:1.
Figure 18 shows 0#~5#The XPS spectrum figure of sample, it is clear that the 1 of various difference reducing degrees#~5#Between sample
Difference is difficult to find out from the XPS spectrum figure being almost overlapped；That is, be using the XPS means of testing in this comparative example can not
The reduction-state graphene oxide of different reducing degrees is distinguished as shown in above-described embodiment 1.
Comparative example 2
In this comparative example, 0 is characterized respectively using ultravioletvisible absorption#~5#Sample.
Figure 19 shows 0#~5#The spectrogram of the normalization ultraviolet-visible absorption spectroscopy of sample.As can be seen from Figure 19, phase
For 0#Sample, 1#~5#The main absorption peak of sample from 226nm red shifts to 264nm or so, visible light region influx and translocation,
And disappear in the peak shoulder of 300nm or so, these all show pi-conjugated knot in the removal of oxygen-containing functional group and graphene nano lamella
The reparation of structure.However, in addition to air high temperature (450 DEG C) and oxidation are to 2#The apparent destruction for the translucency that sample is brought, 1#~5#
Sample has no other difference.
Therefore, being also using the means of testing of the ultravioletvisible absorption in this comparative example can not be as shown in above-described embodiment 1
The reduction-state graphene oxide of different reducing degrees is distinguished.
Comparative example 3
In this comparative example, using scanning polarization force microscope (scanning polarization force
Microscopy, SPFM) 0 is characterized respectively#~5#Sample.
Figure 20~Figure 27 respectively illustrates the SPFM figures of different samples.It is worth noting that in SPFM figures, with practical shape
Increase of the looks height compared to apparent height may indicate that the reduction of GO samples.
It is known from figures that, reduction reaction is the (figure of (Figure 22,23,25) uniformly occurred or uneven generation
21, position shown in longitudinal arrow in Figure 27)；Obviously, after GO lamellas are by distinct methods homogeneous reduction, 1#~5#Each sample between
The difference of reducing degree be difficult found out by the comparison of apparent height, this is because contained in SPFM figures topographical information (Figure 25,
Position shown in lateral arrows in 27), and SPFM imagings are easy to be influenced at image force size (setting value) by setting.Namely
It says, being also using the SPFM means of testing in this comparative example can not be as shown in above-described embodiment 1 by different reducing degrees and reduction
React what the reduction-state graphene oxide uniformly occurred distinguished.
To sum up, the test method of the reducing degree of graphene oxide according to the present invention compared with the prior art can
After graphene oxide sample is by different restoring method homogeneous reductions, using the method for electrostatic force microscope figure, by comparing phase
The peak position and peak intensity of position-needle point bias plot change, can be to the reducing degree difference of monolithic layer reduction-state graphene oxide sample
Carry out the characterization of nanoscale.
Although the present invention has shown and described with reference to specific embodiment, it should be appreciated by those skilled in the art that：
In the case where not departing from the spirit and scope of the present invention limited by claim and its equivalent, can carry out herein form and
Various change in details.
Claims (5)
1. a kind of test method of the reducing degree of graphene oxide, which is characterized in that including step：
S1, electrostatic force microscope figure of the reduction-state graphene oxide under different needle point biass is measured using electrostatic force microscope；
S2, it is mapped to needle point bias with the phase of reduction-state graphene oxide described in the electrostatic force microscope figure, obtains phase
Position-needle point bias plot；
S3, reduction journey of the reduction-state graphene oxide compared with graphene oxide is determined according to the phase-needle point bias plot
The size of degree；Wherein, in the phase-needle point bias plot, the corresponding specific needle point bias of peak value or valley of phase
Absolute value is smaller, and/or bigger less than the absolute value of the phase under any needle point bias of the specific needle point bias, then its is right
The reduction-state graphene oxide answered is higher compared with the reducing degree of graphene oxide.
2. test method according to claim 1, which is characterized in that in the step S1, needle point bias ranging from-
12V~12V.
3. test method according to claim 2, which is characterized in that in the step S1, be divided between needle point bias
1V。
4. according to any test methods of claim 1-3, which is characterized in that it is right that the reduction-state graphene oxide passes through
Graphene oxide carries out thermal reduction and/or electronation obtains.
5. test method according to claim 4, which is characterized in that electronation is full for the graphene oxide to be placed in
It is restored in hydrazine hydrate steam.
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