CN115524356A - Method for verifying modification effect of carbon material - Google Patents
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Abstract
The invention relates to the technical field of detection, in particular to a method for verifying a modification effect of a carbon material.
Description
Technical Field
The invention relates to the technical field of detection, in particular to a method for verifying a modification effect of a carbon material.
Background
Since the discovery and synthesis of fullerene, carbon nanotube, graphene and the like, the preparation and performance research of various novel carbon materials with novel morphology and excellent performance become the research hotspots of the current materials and chemical subjects. The research depth and the application breadth of the novel carbon material become one of the important marks for measuring the advanced level of the national science and technology, wherein the composition structure and the performance regulation and control are the key problems of the carbon material science.
In the related art, after the carbon material is modified, the carbon content of the carbon material needs to be detected, and then the modification effect of the carbon material is evaluated according to the carbon content of the carbon material, however, in the evaluation process, since the carbon content of the carbon material is mainly calculated by evaluation, the test effect is inaccurate, and the effect of the modification treatment cannot be accurately tested or verified.
Disclosure of Invention
The invention mainly aims to provide a method for verifying the modification effect of a carbon material, and aims to solve the technical problem that the effect of modification treatment cannot be accurately tested or verified after the carbon material is modified in the related technology.
In order to achieve the above object, in a first aspect, the present invention provides a method for verifying a modification effect of a carbon material, comprising the steps of:
obtaining initial parameters of the carbon material; the initial parameters comprise an initial element group of the carbon material and initial contents corresponding to elements in the initial element group;
according to preset modification parameters, carrying out modification treatment on the carbon material and obtaining current parameters of the modified carbon material; the current parameters comprise a current element group of the carbon material and current contents corresponding to elements in the current element group;
analyzing and comparing the current parameters with the initial parameters to obtain the current modification effect of the carbon material;
judging whether the current modification effect meets the preset modification requirement or not;
and when the preset modification requirement is met, judging that the carbon material modification effect is qualified.
Optionally, the step of obtaining initial parameters of the carbon material comprises:
scanning the carbon material before modification by using XPS (X-ray diffraction) to obtain a full-scanning spectrum of the carbon material before modification;
determining the initial element group of the carbon material according to the full-scanning spectrogram;
and acquiring an initial high-resolution narrow-scan spectrogram of the initial element group to obtain the initial parameters.
Optionally, the initial element group comprises an initial carbon element and a first element group other than the initial carbon element;
the step of obtaining the initial high-resolution narrow-scan spectrogram of the initial element group to obtain the initial parameters comprises:
respectively acquiring an initial C1s spectrogram of the initial carbon element and an initial element spectrogram corresponding to each element in the first element group;
and acquiring the initial content corresponding to the initial carbon element and each element in the first element group according to the initial C1s spectrogram and the initial element spectrogram to obtain the initial parameter.
Optionally, the step of obtaining the initial content of the initial carbon element and the initial content of each element in the first element group according to the initial C1s spectrogram and the initial element spectrogram to obtain the initial parameter includes:
acquiring an initial functional group in the carbon material according to the initial C1s spectrogram and the initial element spectrogram;
obtaining the initial element chemical state corresponding to each functional group from the initial functional group;
and acquiring the initial carbon element and the initial content corresponding to each element in the first element group according to the chemical state of the initial element to obtain the initial parameter.
Optionally, the step of performing modification treatment on the carbon material according to preset modification parameters and obtaining modified current parameters of the carbon material includes:
performing hybridization treatment on the carbon material according to the preset modification parameters;
collecting and acquiring the current parameters of the carbon material after hybridization treatment.
Optionally, the step of acquiring and obtaining the current parameters of the carbon material after hybridization processing comprises:
scanning the modified carbon material by using XPS (X-ray diffraction) to obtain a current full-scanning spectrum of the modified carbon material;
determining the current element group of the carbon material according to the current full-scanning spectrogram;
and acquiring and obtaining a current high-resolution narrow-scan spectrogram corresponding to each element in the current element group to obtain the current parameters.
Optionally, the current element group includes a current carbon element and a second element group other than the current carbon element;
the step of acquiring and obtaining the current high-resolution narrow-scan spectrogram corresponding to each element in the current element group to obtain the current parameter includes:
respectively acquiring a current C1s spectrogram of the current carbon element and a current element spectrogram corresponding to each element in the second element group;
and acquiring the current content corresponding to each element in the current carbon element and the second element group according to the current C1s spectrogram and the current element spectrogram to obtain the current parameter.
Optionally, the step of obtaining the current content corresponding to the current carbon element and each element in the second element group according to the current C1s spectrogram and the current element spectrogram to obtain the current parameter includes:
acquiring a current functional group in the carbon material according to the current C1s spectrogram and the current element spectrogram;
obtaining the current element chemical state corresponding to each functional group from the current functional group;
and obtaining the current carbon element and the current content corresponding to each element in the second element group according to the chemical state of the current element to obtain the current parameter.
Optionally, the step of comparing the current parameter with the initial parameter to obtain the current modification effect of the carbon material includes:
taking the initial C1s spectrogram as a reference spectrogram, and respectively carrying out corresponding peak-splitting fitting on the current C1s spectrogram and the current high-resolution narrow-scan spectrogram according to preset fitting indexes to obtain corresponding fitting data;
comparing the fitting data to obtain a corresponding change value of the current parameter relative to the initial parameter; the preset fitting index comprises a half-peak width A corresponding to the modified carbon element, wherein A is more than or equal to 0.5eV and less than or equal to 2 eV;
and acquiring the current modification effect of the carbon material according to the corresponding change value.
Optionally, after the step of determining whether the current modification effect meets a preset modification requirement, the method further includes:
when the preset modification requirement is not met, judging that the carbon material modification effect is unqualified;
and obtaining a first modification parameter, taking the first modification parameter as the preset modification parameter, and returning to the step of executing the step of modifying the carbon material according to the preset modification parameter and obtaining the modified corresponding current parameter of the carbon material until the modification effect of the carbon material is judged to be qualified.
According to the technical scheme, the initial parameters of the carbon material are obtained, then the carbon material is modified according to the preset improved parameters, the current parameters after the carbon material is modified are obtained, the current parameters are analyzed and compared with the initial parameters, then the current modification effect is obtained, whether the current modification effect meets the preset modification requirement or not is judged, and when the preset modification requirement is met, the carbon material modification effect is judged to be qualified. In the specific implementation process, the initial parameters before modification and the current parameters after modification are obtained, the initial parameters and the current parameters are analyzed and compared to obtain the corresponding current modification effect after modification by adopting the preset modification parameters, and the carbon material meeting the preset modification requirement is defined as a qualified material by analyzing and comparing the current modification effect, so that the modification effect of the carbon material can be accurately verified, and the technical defect that the effect of modification treatment cannot be accurately tested or verified after modification treatment is carried out on the carbon material in the related technology is overcome.
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In order to more clearly illustrate the embodiments or technical solutions of the present invention, the drawings used in the embodiments or technical solutions of the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a flow chart of an exemplary method of verifying the effect of modification of a carbon material in accordance with the present invention;
FIG. 2 is a flowchart of step S100 illustrated in FIG. 1;
FIG. 3 is a flowchart of step S130 illustrated in FIG. 2;
FIG. 4 is a flowchart of the refinement step of step S132 illustrated in FIG. 3;
FIG. 5 is a flowchart of step S200 illustrated in FIG. 1;
FIG. 6 is a flowchart of the refinement step of step S220 illustrated in FIG. 5;
FIG. 7 is a flowchart of the refinement step of step S223 illustrated in FIG. 6;
FIG. 8 is a flowchart of the refinement step of step S223b illustrated in FIG. 7;
FIG. 9 is a flowchart of step S300 illustrated in FIG. 1;
FIG. 10 is a flow chart of another result of an exemplary method of the present invention;
FIG. 11 is a full-scan spectrum of some embodiments of the present invention before acidification;
fig. 12 (a) is a C1s spectrum of the exemplary embodiment of fig. 11 before the acidification treatment, and fig. 12 (b) is a C1s spectrum of the exemplary embodiment of fig. 10 after the acidification treatment;
fig. 13 (a) is a graph of O1s before acidification in the exemplary embodiment of fig. 11, and fig. 13 (b) is a graph of O1s after acidification in the exemplary embodiment of fig. 11;
FIG. 14 is a full scan spectrum of a further embodiment of the invention before alkylation;
fig. 15 (a) is a C1s spectrum after the alkylation treatment of the exemplary embodiment in fig. 14, fig. 15 (b) is an O1s spectrum after the alkylation treatment of the exemplary embodiment in fig. 14, and fig. 15 (C) is an O1s spectrum after the alkylation treatment of the exemplary embodiment in fig. 14.
The objects, features and advantages of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
It should be noted that all the directional indicators (such as up, down, left, right, front, and back … …) in the embodiment of the present invention are only used to explain the relative position relationship, motion situation, etc. between the mechanisms in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indicator is changed accordingly.
In the present invention, unless otherwise expressly stated or limited, the terms "connected," "secured," and the like are to be construed broadly, and for example, "secured" may be a fixed connection, a removable connection, or an integral part; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In addition, if there is a description relating to "first", "second", etc. in the embodiments of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying relative importance or to implicitly indicate the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of the feature. In addition, the meaning of "and/or" appearing throughout includes three juxtapositions, exemplified by "A and/or B" including either A or B or both A and B. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
The inventive concept of the present invention will be further elucidated below in connection with some specific embodiments.
The invention provides a method for verifying a carbon material modification effect.
As shown in fig. 1 to 15 (c), an embodiment of the method for verifying the modification effect of the carbon material according to the present invention is provided.
In this embodiment, referring to fig. 1-15 (c), the method for verifying the modification effect of the carbon material includes the following steps:
s100, obtaining initial parameters of the carbon material; the initial parameters comprise an initial element group of the carbon material and initial contents corresponding to elements in the initial element group;
in the present embodiment, in acquiring the initial parameters, the carbon material is first scanned by XPS to acquire a full scan spectrum thereof; and then observing a full-scanning spectrogram to obtain elements of the carbon material, after determining the element composition, scanning the carbon material by using XPS to obtain a high-resolution narrow-scanning spectrogram corresponding to each element, and then observing the high-resolution narrow-scanning spectrogram to obtain initial contents corresponding to each element so as to form initial parameters.
S200, modifying the carbon material according to preset modification parameters and obtaining current parameters of the modified carbon material; the current parameters comprise a current element group of the carbon material and current contents corresponding to elements in the current element group;
in this embodiment, when modifying the carbon material, the modification requirement is determined according to the specific use of the carbon material, taking the acidification modification treatment of the carbon nanotube as an example:
in specific implementation, according to modification requirements, full-scanning spectrograms before and after acidification (hydrophilic property modification) treatment of the carbon nano tube are confirmed, wherein elements contained in a sample before and after modification and corresponding content change are confirmed, the content change of O elements before and after acidification can be found out obviously through comparison, and the relative atomic percentage content of the O elements can be found to be increased from 1.7% to 37.31% through a high-resolution narrow-scanning spectrogram. Confirming the chemical state and corresponding content change of C1 s:
fig. 12 (a) shows an asymmetric structure of a carbon nanotube C1s, and in order to further accurately describe the chemical state and the corresponding content of the C element after the acidification modification, a C1s spectrogram before the modification is used as a C = C chemical state corresponding C1s reference spectrogram after the acidification modification, and in addition, the half-peak width ratio of the C element corresponding to the C element in the chemical state of C-C, C-O, C = O is controlled within a range of 1 to 1.5 for free fitting, so that it can be seen that the content of the C element in the chemical state of the sample C-C, C-O, C = O after the acidification modification is significantly increased, and the final obtained result is shown in fig. 12 (b). Note: the peak shape structure of the C1s spectrogram in an sp2 hybridization state is asymmetric, and when the C1s spectrogram before modification is taken as a reference spectrogram, the peak shape needs to be completely copied (such as asymmetric tailing and half peak width), and on the basis, the addition of symmetric spectral peaks corresponding to other chemical states is carried out.
It is specifically and explicitly stated that in this example, the preset modification parameters require specific modification schemes to be determined according to the specific use of the carbon material. XPS, also known as X-ray photoelectron spectroscopy, is an example of the present invention.
S300, analyzing and comparing the current parameters with the initial parameters to obtain the current modification effect of the carbon material;
in this embodiment, during analysis and comparison, firstly, the initial C1s spectrogram before modification corresponding to the initial parameter is used as a reference spectrogram, then the current full-scan spectrogram and the current high-resolution narrow-scan spectrogram corresponding to the current parameter are implanted into the reference spectrogram, then the current full-scan spectrogram and the current high-resolution narrow-scan spectrogram are subjected to half-peak width limitation and then subjected to free fitting, finally, corresponding change conditions of the element chemical state, the functional group, the element content and the like of the modified carbon material are obtained, and then, the current modification effect of the carbon material is obtained according to the specific change conditions.
Of course, in an exemplary technique of the present invention: the process of obtaining the chemical state and corresponding content change of the C element may also be: the carbon material C1s spectral peak shape before modification is taken as a reference basis, C1s comparison spectrograms before and after modification are observed, and the change of the chemical state and the corresponding content of the C element is confirmed, so that the technical defect that data analysis results are not credible because data analysts do not pay enough attention to the peak shape due to asymmetric SP2 hybrid carbon spectral peaks and the C element data before and after modification in the related technology are subjected to peak fitting is solved, and the technical error is overcome.
Secondly, the method of the present invention further includes: by observing the chemical states and the corresponding content changes of all other elements except carbon element in the carbon material, the overall modification state of the material is further verified by knowing the changes of all the contained elements, so that the data analysis result is further objective, and the reliability is increased.
The data fitting process of the present example was performed by introducing the asymmetric peak shape of C1s directly into the data analysis of the modified carbon material; however, because the peak shape difference of the conventional carbon material doped elements such as O1s, si2p and the like is not obvious in different chemical states, aiming at the defect, the invention can limit the half-peak width when data are fitted during specific treatment, for example, the half-peak width is limited to be between 0.5 and 2eV, and the half-peak width difference is between 1 and 1.5 times in different chemical states, and by adopting the mode, the unification of different carbon material peak splitting methods is ensured, the reliability of a data analysis result is enhanced, and the fitting effect on the numerical value can be met.
S400, judging whether the current modification effect meets the preset modification requirement or not;
in this embodiment, when determining whether the current modification effect meets the preset modification requirement, the current modification effect and the preset modification requirement may be quantized, and then obtained by comparing whether the two data are the same or how much different.
And S500, judging that the carbon material modification effect is qualified when the preset modification requirement is met.
In this embodiment, an initial parameter of the carbon material is obtained, then the carbon material is modified according to a preset modification parameter, a current parameter after the carbon material is modified is obtained, the current parameter is analyzed and compared with the initial parameter, and then a current modification effect is obtained, and then whether the current modification effect meets a preset modification requirement or not is judged, and when the preset modification requirement is met, the carbon material modification effect is judged to be qualified. In the specific implementation process, the initial parameters before modification and the current parameters after modification are obtained, the initial parameters and the current parameters are analyzed and compared to obtain the corresponding current modification effect after modification by adopting the preset modification parameters, and the carbon material meeting the preset modification requirement is defined as a qualified material by analyzing and comparing the current modification effect, so that the modification effect of the carbon material can be accurately verified, and the technical defect that the effect of modification treatment cannot be accurately tested or verified after modification treatment is carried out on the carbon material in the related technology is overcome.
In some embodiments, referring to FIG. 2, the step of obtaining initial parameters of the carbon material comprises:
s110, scanning the carbon material before modification by using XPS to obtain a full scanning spectrum of the carbon material before modification;
it should be specifically and clearly noted that in this embodiment, the step of scanning the carbon material before modification by XPS to obtain the full-scan spectrum of the carbon material is the prior art, and the present invention is only applied to this step, and does not relate to the improvement or design of the structure of the full-scan spectrum obtained by scanning the carbon material by XPS, so that details are not repeated.
S120, determining an initial element group of the carbon material according to the full-scanning spectrogram;
in this embodiment, in specific implementation, the full-scan spectrum is directly observed, and the initial number of elements in the carbon material is obtained according to the peak shape change relationship on the full-scan spectrum, so as to form an initial element group.
S130, obtaining an initial high-resolution narrow-scan spectrogram of the initial element group to obtain initial parameters.
In this embodiment, after obtaining the initial high-resolution narrow-scan spectrogram of the initial element group, the high-resolution narrow-scan spectrogram is directly observed, and then the initial content of the corresponding element is determined according to the element content variation relationship of the high-resolution narrow-scan spectrogram.
In this embodiment, the carbon material before modification is scanned by using XPS to obtain a full scan spectrum of the corresponding carbon material, and then an initial element group of the carbon material is determined according to the full scan spectrum, and then an initial high-resolution narrow scan spectrum of the initial element group of the carbon material is obtained, and initial parameters are obtained, so that the original element composition and element content of the carbon material can be obtained and observed by directly using XPS technology in specific implementation, and the accuracy of determining various element compositions and specific values of various element contents of the carbon material before modification is effectively ensured.
In some embodiments, referring to fig. 3, the initial element group includes an initial carbon element and a first element group other than the initial carbon element;
the method comprises the steps of obtaining an initial high-resolution narrow-scan spectrogram of an initial element group to obtain initial parameters, and comprises the following steps:
s131, respectively obtaining an initial C1S spectrogram of an initial carbon element and an initial element spectrogram corresponding to each element in the first element group;
in the present embodiment, the initial C1s spectrum of the initial carbon element and the initial element spectra of the elements in the first element group are obtained by scanning with XPS and obtaining them.
It should be noted that, in the exemplary technique, if the first element group includes hydrogen element (H), oxygen element (O) and silicon element (Si), the initial element spectrum includes an initial H1s spectrum, an initial O1s spectrum and an initial Si1s spectrum.
S132, obtaining initial carbon elements and initial contents corresponding to the elements in the first element group according to the initial C1S spectrogram and the initial element spectrogram to obtain initial parameters.
In this embodiment, in specific implementation, the initial C1s spectrogram of the initial carbon element and the initial element spectrogram of each element in the first element group are respectively obtained, then the corresponding initial content of each element is obtained according to the initial C1s spectrogram and the initial element spectrogram of each element in the first element group, and then the element composition and the initial content corresponding to each element are combined to obtain the initial parameter.
In some embodiments, referring to fig. 4, the step of obtaining the initial content of the initial carbon element and each element in the first element group according to the initial C1s spectrogram and the initial element spectrogram to obtain the initial parameter includes:
s132a, acquiring an initial functional group in the carbon material according to the initial C1S spectrogram and the initial element spectrogram;
in the embodiment, in the specific implementation, the specific manner of obtaining the functional group is to obtain the corresponding functional group by observing an initial C1s spectrogram and an initial element spectrogram.
S132b, acquiring the initial element chemical state corresponding to each functional group from the initial functional group;
in this embodiment, when obtaining the initial elemental chemical states corresponding to each functional group in the initial functional groups, the method may adopt that the initial C1s spectrogram is used as a reference spectrogram, then the obtained initial elemental spectrogram is fitted to the initial C1s spectrogram, and then the corresponding elemental chemical states are finally obtained by observing a change relationship of peak shapes of spectral peaks after fitting.
S132c, obtaining the initial carbon element and the corresponding initial content of each element in the first element group according to the chemical state of the initial element, and obtaining initial parameters.
In this embodiment, the initial functional group in the carbon material is obtained according to the initial C1s spectrogram and the initial element spectrogram, then the initial element chemical state corresponding to each functional group is obtained from the initial functional group, and finally the initial carbon element and the initial content corresponding to each element in the first element group are obtained according to the initial element chemical state, so as to obtain the initial parameter.
In some embodiments, referring to fig. 5, the step of modifying the carbon material according to the preset modification parameters and obtaining the modified current parameters of the carbon material includes:
s210, carrying out hybridization treatment on the carbon material according to preset modification parameters;
in this example, the exemplary hybridization process is sp2 hybridization.
S220, collecting and obtaining the current parameters of the hybridized carbon material.
When the carbon material is subjected to hybridization treatment, the corresponding hybridization treatment requirement is determined according to the specific application of the carbon material, taking the acidification hybridization treatment of the carbon nanotube as an example:
in specific implementation, according to modification requirements, full-scanning spectrograms before and after acidification (hydrophilic property modification) treatment of the carbon nano tube of elements contained in a sample and corresponding content change before and after hybridization treatment are confirmed, the content change of O elements before and after acidification treatment can be found out obviously through comparison, and the relative atomic percentage content of the O elements can be found to be increased from 1.7% to 37.31% through a high-resolution narrow-scanning spectrogram. Confirming the chemical state and corresponding content change of C1 s:
fig. 12 (a) shows an asymmetric structure of a carbon nanotube C1s, and in order to further accurately describe the chemical state and the corresponding content of the C element after the acidification modification, a C1s spectrogram before the modification is used as a C = C chemical state corresponding C1s reference spectrogram after the acidification modification, and in addition, the half-peak width ratio of the C element corresponding to the C element in the chemical state of C-C, C-O, C = O is controlled within a range of 1 to 1.5 for free fitting, so that it can be seen that the content of the C element in the chemical state of the sample C-C, C-O, C = O after the acidification modification is significantly increased, and the final obtained result is shown in fig. 12 (b). Note: the peak shape structure of the C1s spectrogram in an sp2 hybridization state is asymmetric, and when the C1s spectrogram before modification is taken as a reference spectrogram, the peak shape needs to be completely copied (such as asymmetric tailing and half peak width), and on the basis, the addition of symmetric spectral peaks corresponding to other chemical states is carried out.
It is specifically and explicitly stated that in this example, the preset modification parameters require specific modification schemes to be determined according to the specific use of the carbon material.
In some embodiments, referring to fig. 6, the step of collecting and obtaining the current parameters of the carbon material after hybridization comprises:
s221, scanning the modified carbon material by using XPS to obtain a current full-scanning spectrogram of the modified carbon material;
in this embodiment, the process of scanning the modified carbon material to obtain the full-scan spectrum of the modified carbon material is the same as the process of obtaining the full-scan spectrum before modification, and is not described herein again.
S222, determining the current element group of the carbon material according to the current full-scanning spectrogram;
in this embodiment, the process of determining the current element group of the carbon material according to the current full-scan spectrogram is the same as the process of determining the initial element group according to the initial element group, and details thereof are omitted here.
And S223, acquiring and obtaining a current high-resolution narrow-scan spectrogram corresponding to each element in the current element group to obtain current parameters.
In this embodiment, the process of obtaining the current parameter according to the current high-resolution narrow-scan spectrogram is the same as the process of obtaining the initial parameter according to the initial high-resolution narrow-scan spectrogram, and details are not repeated here.
In some embodiments, referring to fig. 7, the current element group includes the current carbon element and a second element group other than the current carbon element;
the method comprises the steps of acquiring and obtaining a current high-resolution narrow-scan spectrogram corresponding to each element in a current element group to obtain current parameters, and comprises the following steps:
s223a, respectively obtaining a current C1S spectrogram of the current carbon element and a current element spectrogram corresponding to each element in a second element group;
and S223b, obtaining the current carbon element and the current content corresponding to each element in the second element group according to the current C1S spectrogram and the current element spectrogram, and obtaining the current parameters.
In some embodiments, referring to fig. 8, the step of obtaining the current content of each element in the current carbon element and the second element group according to the current C1s spectrogram and the current element spectrogram to obtain the current parameter includes:
s223b1, obtaining a current functional group in the carbon material according to the current C1S spectrogram and the current element spectrogram;
s223b2, obtaining the current element chemical state corresponding to each functional group from the current functional group;
and S223b3, obtaining the current carbon element and the corresponding current content of each element in the second element group according to the chemical state of the current element, and obtaining the current parameter.
In some embodiments, referring to fig. 9, the step of comparing the current parameter with the initial parameter to obtain the current modification effect of the carbon material comprises:
s310, taking the initial C1S spectrogram as a reference spectrogram, and respectively carrying out corresponding peak-splitting fitting on the current C1S spectrogram and the current high-resolution narrow-scan spectrogram according to preset fitting indexes to obtain corresponding fitting data;
in this embodiment, in the implementation, since the peak shape, half-peak width, and peak position of the metal element in the metal state and the oxidation state are generally greatly different, the half-peak width needs to be limited in the fitting.
S320, comparing the fitting data to obtain a corresponding change value of the current parameter relative to the initial parameter; the preset fitting index comprises a half-peak width A corresponding to the modified carbon element, wherein A is more than or equal to 0.5eV and less than or equal to 2 eV;
and S330, acquiring the current modification effect of the carbon material according to the corresponding change value.
In some embodiments, referring to fig. 10, after the step of determining whether the current modification effect meets the preset modification requirement, the method further includes:
s600, judging that the modification effect of the carbon material is unqualified when the preset modification requirement is not met;
s700, obtaining a first modification parameter, taking the first modification parameter as a preset modification parameter, and returning to the step of executing modification processing on the carbon material according to the preset modification parameter and obtaining a corresponding modified current parameter of the carbon material until the modification effect of the carbon material is judged to be qualified.
In this embodiment, in specific implementation, when the modification effect of the carbon material is determined to be unqualified, it indicates that the modification effect of the material cannot meet the predetermined modification requirement due to the predetermined modification parameters, and therefore, it is necessary to re-determine the modification parameters and then select an identical carbon material that is not subjected to modification treatment for modification treatment.
Of course, in an exemplary technique, the invention may also be performed as follows: confirming the element and corresponding content change contained in the sample before and after modification: observing full-scanning spectrograms before and after the modification treatment of the carbon nano tube, and roughly and qualitatively judging whether elements exist or not; and collecting high-resolution narrow-scan spectrograms of all elements contained in the sample before and after modification. And obtaining the relative atomic percentage of each element before and after modification through a high-resolution narrow-scan spectrogram of each element.
Confirming the chemical state and corresponding content change of C1 s: taking the C1s spectrogram before modification as a reference spectrogram, properly adding C-C, C-O, C = O chemical state corresponding spectral peak according to the actual situation of the material on the basis, and controlling the width ratio of the lower corresponding half peak within the range of 1-1.5 eV for free fitting; and observing the content change of the C element in each chemical state of the sample after the modification treatment.
The peak shape structure of the C1s spectrogram in an sp2 hybridization state is asymmetric, and when the C1s spectrogram before modification is taken as a reference spectrogram, the peak shape needs to be completely copied (such as asymmetric tailing and half peak width), and on the basis, the addition of symmetric spectral peaks corresponding to other chemical states is carried out.
Confirming the chemical states and corresponding content changes of other elements: and (4) observing the content, peak position and peak shape change of other elements except carbon in the sample before and after modification, and performing peak splitting fitting treatment on the spectrogram by combining the actual condition of the material.
The peak shape, half-peak width and peak position of the metal state and the oxidation state of the metal element generally have great difference, and a complex spectrogram processing method is recommended to be adopted for fitting analysis; the peak shape difference of the doping elements of the conventional carbon material, such as O1s, si2p and the like, in different chemical states is not obvious, and the half-peak width can be limited when data are fitted, wherein the half-peak width is limited to 0.5-2eV, and the half-peak width difference in different chemical states is 1-1.5 times.
Verifying the content variation trend and the chemical state matching condition of each element: and analyzing the chemical states and the contents of the elements corresponding to the elements containing C to ensure that the element content variation trend in each chemical state is consistent with the actual condition of the sample.
In some embodiments, please refer to fig. 11 to fig. 13 (b), which take an example of performing an acidification modification process on a carbon nanotube and obtaining corresponding XPS data, illustrating the process of the test data:
confirming the element and corresponding content change contained in the sample before and after modification: fig. 11 is a full-scan spectrogram before and after carbon nanotube acidification (hydrophilic property modification), and comparison shows that the content of O element changes significantly before and after acidification, and the high-resolution narrow-scan spectrogram shows that the relative atomic percentage content of O element increases from 1.7% to 37.31%.
Confirming the chemical state and corresponding content change of C1 s: fig. 12 (a) shows an asymmetric structure of a carbon nanotube C1s, and in order to further accurately describe the chemical state and the corresponding content of the C element after the acidification modification, a C1s spectrogram before the modification is used as a C = C chemical state corresponding C1s reference spectrogram after the acidification modification, and in addition, the half-peak width ratio of the C element corresponding to the C element in the chemical state of C-C, C-O, C = O is controlled in the range of 1ev to 1.5eV for free fitting, so that the content of the C element in the chemical state of the sample C-C, C-O, C = O after the acidification treatment is obviously increased, and the final obtained result is shown in fig. 12 (b).
In an exemplary technique, the specific process of peak fitting and processing is: fitting the peak of the C1s spectrum of the carbon nano tube before modification, and confirming the specific parameters of the peak shape fitting.
The comparative spectra of C1s before and after modification were observed to confirm the approximate change of the chemical state of the C element (e.g., whether a distinct peak of C-C, C-O, C = O chemical state appears).
Taking the C1s spectrogram before modification as a reference spectrogram (fitting parameters of specific peak shapes of the carbon nanotubes before modification are applied mechanically), properly adding C-C, C-O, C = O chemical state corresponding spectral peaks according to the actual situation of the material, and controlling the width ratio of the lower corresponding half peak within the range of 1-1.5 eV for free fitting; and observing the content change of the C element in each chemical state of the sample after the modification treatment.
The peak shape structure of the C1s spectrogram in an sp2 hybridization state is asymmetric, and when the C1s spectrogram before modification is taken as a reference spectrogram, the peak shape needs to be completely copied (such as asymmetric tailing and half peak width), and on the basis, the addition of symmetric spectral peaks corresponding to other chemical states is carried out.
In the embodiment, by providing the operation steps of the peak separation processing, the accurate data can be accurately obtained in specific implementation, and the accuracy and the reliability of the data are improved.
Confirming the chemical states and corresponding content changes of other elements: since the sample before and after modification only contains C, O element and the carbon nanotube sample before modification contains trace O element, it can be seen from observing fig. 13 (a) that O in the sample is in the chemical state of C-O, C = O, and the content of O element in each chemical state is significantly increased after the acidification treatment (as shown in fig. 13 (b)).
Verifying the content change trend and the chemical state matching condition of each element: the sample before and after the acidification treatment modification only contains C, O element, wherein the content of C element in the carbon element under the chemical state of C-C, C-O, C = O is obviously increased; and the whole content of the O element and the content of the O element in the chemical state of C-O, C = O also show an increasing trend. The variation trends of the elements and the chemical state contents are matched.
In still other embodiments, referring to fig. 14-15 (c), the process of performing the alkylation modification process on the carbon nanotubes and obtaining the corresponding XPS data is described as an example:
also observing the full-scan spectrum of the carbon nanotube after the alkylation modification (hydrophobic modification) (as shown in fig. 14), it can be seen that a small amount of Si element is detected on the surface of the sample in addition to the increase of O element.
Fitting the C1s data of the alkylated modified carbon nanotube modified carbon material by using the same method, and finding that C elements in a sample exist in a C-C/C-Si chemical state except C = C chemical state C elements, and the content increase of O elements is irrelevant to the C elements; through O, si element data analysis, it can be found that the O element is mainly combined with the Si element, and the data analysis result is consistent with the C element analysis result.
C = C chemical state corresponding to C1s spectrum peak shape asymmetry, half-peak width fitting randomness, and absolute and subjective results of single data obtained overall results are main factors influencing accurate analysis of XPS data of the current novel carbon material. Under the current situation, the results obtained by fitting the same C1s data are different on the premise that the error levels are similar and each method can well fit the data. If the XPS data analysis method is improper, more unnecessary errors and even wrong results can be introduced, and correct understanding and research of the novel carbon material performance regulation and control process mechanism are interfered. The peak of the carbon nanotube C1s spectrum before modification is taken as a reference, and the change of the content of each element and the chemical state of the carbon material before and after modification is mainly concerned. And the data analysis method is unified and standardized by carrying out data analysis on the half-peak width and different samples in the same batch, so that the accuracy of XPS characterization on the surface elements and chemical state quantification of the novel carbon material is further improved, and a technical guarantee is provided for the surface modification mechanism and process improvement research of the carbon material.
According to the technical scheme, the initial parameters of the carbon material are obtained, then the carbon material is modified according to the preset improved parameters, the current parameters after the carbon material is modified are obtained, the current parameters are analyzed and compared with the initial parameters, then the current modification effect is obtained, whether the current modification effect meets the preset modification requirement or not is judged, and when the preset modification requirement is met, the carbon material modification effect is judged to be qualified. In the specific implementation process, the initial parameters before modification and the current parameters after modification treatment are obtained, the initial parameters and the current parameters are analyzed and compared to obtain the corresponding current modification effect after modification treatment by adopting the preset modification parameters, and the carbon material meeting the preset modification requirements is defined as a qualified material by analyzing and comparing the current modification effect, so that the modification effect of the carbon material can be accurately verified, and the technical defect that the effect of modification treatment cannot be accurately tested or verified after the carbon material is modified by related technologies is overcome.
The above description is only an alternative embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A method for verifying the modification effect of a carbon material is characterized by comprising the following steps:
acquiring initial parameters of the carbon material; the initial parameters comprise an initial element group of the carbon material and initial contents corresponding to elements in the initial element group;
according to preset modification parameters, carrying out modification treatment on the carbon material and obtaining current parameters of the modified carbon material; the current parameters comprise a current element group of the carbon material and current contents corresponding to each element in the current element group;
analyzing and comparing the current parameters with the initial parameters to obtain the current modification effect of the carbon material;
judging whether the current modification effect meets the preset modification requirement or not;
and when the preset modification requirement is met, judging that the modification effect of the carbon material is qualified.
2. The method of verifying the effect of modifying a carbon material of claim 1, wherein said step of obtaining initial parameters of said carbon material comprises:
scanning the carbon material before modification by using XPS to obtain a full scanning spectrum of the carbon material before modification;
determining the initial element group of the carbon material according to the full-scanning spectrogram;
and acquiring an initial high-resolution narrow-scan spectrogram of the initial element group to obtain the initial parameters.
3. The method of verifying the modifying effect of a carbon material as claimed in claim 2, wherein the initial element group comprises an initial carbon element and a first element group other than the initial carbon element;
the step of obtaining the initial high-resolution narrow-scan spectrogram of the initial element group to obtain the initial parameters comprises:
respectively acquiring an initial C1s spectrogram of the initial carbon element and an initial element spectrogram corresponding to each element in the first element group;
and acquiring the initial content corresponding to the initial carbon element and each element in the first element group according to the initial C1s spectrogram and the initial element spectrogram to obtain the initial parameter.
4. The method for verifying the modification effect of the carbon material as claimed in claim 3, wherein the step of obtaining the initial content of each element in the initial carbon element and the first element group according to the initial C1s spectrum and the initial element spectrum to obtain the initial parameter comprises:
acquiring an initial functional group in the carbon material according to the initial C1s spectrogram and the initial element spectrogram;
obtaining the initial element chemical state corresponding to each functional group from the initial functional group;
and acquiring the initial carbon element and the initial content corresponding to each element in the first element group according to the chemical state of the initial element to obtain the initial parameter.
5. The method for verifying the modification effect of the carbon material as claimed in claim 3, wherein the step of modifying the carbon material according to the preset modification parameters and obtaining the modified current parameters of the carbon material comprises:
performing hybridization treatment on the carbon material according to the preset modification parameters;
collecting and acquiring the current parameters of the carbon material after hybridization treatment.
6. The method for verifying the modification effect of a carbon material according to claim 5, wherein the step of collecting and acquiring the current parameter of the carbon material after hybridization processing comprises:
scanning the modified carbon material by using XPS to obtain a current full-scanning spectrogram of the modified carbon material;
determining the current element group of the carbon material according to the current full-scanning spectrogram;
and acquiring and obtaining a current high-resolution narrow-scan spectrogram corresponding to each element in the current element group to obtain the current parameter.
7. The method for verifying the modification effect of the carbon material as claimed in claim 6, wherein the current element group includes a current carbon element and a second element group other than the current carbon element;
the step of acquiring and obtaining the current high-resolution narrow-scan spectrogram corresponding to each element in the current element group to obtain the current parameter includes:
respectively acquiring a current C1s spectrogram of the current carbon element and a current element spectrogram corresponding to each element in the second element group;
and acquiring the current content corresponding to each element in the current carbon element and the second element group according to the current C1s spectrogram and the current element spectrogram to obtain the current parameters.
8. The method for verifying carbon material modification effect according to claim 7, wherein the step of obtaining the current content of each element in the current carbon element and the second element group according to the current C1s spectrogram and the current element spectrogram to obtain the current parameter comprises:
acquiring a current functional group in the carbon material according to the current C1s spectrogram and the current element spectrogram;
acquiring the current element chemical state corresponding to each functional group from the current functional group;
and obtaining the current carbon element and the current content corresponding to each element in the second element group according to the chemical state of the current element to obtain the current parameter.
9. The method of verifying the modification effect of the carbon material as claimed in claim 8, wherein the step of comparing the current parameter with the initial parameter to obtain the current modification effect of the carbon material comprises:
taking the initial C1s spectrogram as a reference spectrogram, and respectively carrying out corresponding peak-splitting fitting on the current C1s spectrogram and the current high-resolution narrow-scan spectrogram according to preset fitting indexes to obtain corresponding fitting data;
comparing the fitting data to obtain a corresponding change value of the current parameter relative to the initial parameter; wherein the preset fitting index comprises a half-peak width A corresponding to the modified carbon element, and A is more than or equal to 0.5eV and less than or equal to 2 eV;
and acquiring the current modification effect of the carbon material according to the corresponding change value.
10. The method for verifying the modification effect of the carbon material as claimed in any one of claims 1 to 9, further comprising, after the step of determining whether the current modification effect satisfies a preset modification requirement:
when the preset modification requirement is not met, judging that the carbon material modification effect is unqualified;
and obtaining a first modification parameter, taking the first modification parameter as the preset modification parameter, and returning to execute the step of modifying the carbon material according to the preset modification parameter and obtaining the modified corresponding current parameter of the carbon material until the modification effect of the carbon material is judged to be qualified.
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