CN106353299B - A kind of quantitative analysis method of graphene composite conductive slurry - Google Patents
A kind of quantitative analysis method of graphene composite conductive slurry Download PDFInfo
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- 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
Abstract
The present invention relates to a kind of quantitative analysis methods of graphene composite conductive slurry, by a series of conductive agent for preparing different graphene contents, then it carries out repeatedly taking spectrum using conductive agent of the Raman spectrometer to different graphene contents, the peak D of same conductive agent and the average value and its ratio of the peak 2D peak area are calculated using raman spectrum, graphene content in a series of corresponding slurry of ratios is done into a curve, is considered as standard curve.Then same method takes carbon nanotube to be measured-graphene composite conductive peak agent D and the peak 2D peak area ratio, and the ratio corresponding graphene content on standard curve is the content of graphene in carbon nanotube to be measured-graphene composite conductive agent.This method is easy to operate, quick, can be applied to the quantitative analysis of other carbon-based material combined conductive agent slurries, has potential application prospect in terms of the rapid evaluation of carbon-based material conductive agent slurry.
Description
Technical field
The present invention relates to a kind of quantitative analysis methods of combined conductive agent slurry, and in particular to a kind of graphene composite conductive
The quantitative analysis method of slurry.
Background technique
Conductive agent has important shadow to performance of lithium ion battery as the important component in pulp of lithium ion battery
It rings.After a small amount of conductive agent is even added to electrode, it can improve between electrode interior active material particle and and collector
Between contact, to reduce electrode interior Ohmic resistance；In addition, not only may be used after conductive agent is evenly spread in electrode material
To play the role of micro- collector, it will increase the migration velocity of electrode interior electronics and improve the Potential distribution on electrode, and
And the stability, electrode interior imbibition holding capacity and the distribution of electrolyte solution etc. that can also improve electrode structure, Jin Erzeng
The utilization rate of active material in power-up extremely.
Graphene (Graphene), also known as mono-layer graphite are to arrange the two dimension formed in honeycomb lattice by single layer of carbon atom
Material is removed from graphite material, the thickness of only one carbon atom.This structure makes graphene have biggish specific surface
Long-pending, good chemical stability, high electron mobility and excellent mechanical property, theoretical specific surface area are up to 2630m2/
G, thermal coefficient be about 5000W/ (mK), elasticity modulus up to 1100GPa and at room temperature electron mobility is about
200000cm2/ (Vs), and resistivity only has 10-6Ω cm or so, it is lower than copper or silver, it is that current resistivity is minimum
Material.Since graphene has the above special advantage, electricity can largely be improved by only needing to add minute quantity in the electrodes
The performance of pole, therefore graphene is often compound with other carbon materials, is used as conductive agent to improve electrode performance.The synthesis of graphene refers to
Mark is better than the existing high-end carbon-based material conductive agent products such as carbon nanotube, carbon nano-fiber, therefore carbon-based material composite conducting
The content of graphene determines its comprehensive performance in agent.
Currently, further including other carbon-based material components, example in conventional graphene composite conductive agent other than graphene
Such as carbon nanotube, graphite, carbon nano-fiber, Ketjen black, because the elemental composition of conductive agent is all carbon, conventional detection
Method can not well distinguish graphene and other carbon-based materials, therefore also can quantitatively divide without good method
Graphene in graphene-carbon nano tube combined conductive agent slurry is analysed, so that graphene content has no idea to determine in conductive agent, this
So that the quality identification of electrocondution slurry is difficult to realize.Raman spectrum detection has quick, high sensitivity, fingerprint recognition characteristic,
Can be distinguished in conjunction with Raman spectrum be both carbon-based material amorphous carbon, graphite, graphene, therefore Raman spectroscopy is quantitative
Analyzing graphene content in carbon-based material combined conductive agent has very big advantage.As shown in Figure 1, Fig. 1 is above-mentioned common several
The raman spectrum of carbon-based material.
Summary of the invention
The purpose of the present invention is to provide a kind of quantitative analysis methods of graphene composite conductive slurry, realize to carbon nanometer
The accurate quantitative analysis of graphene in pipe-graphene composite conductive agent, to guarantee that carbon nanotube-graphene composite conductive agent performance reaches
To requirement.
To achieve the above object, the invention adopts the following technical scheme:
A kind of quantitative analysis method of graphene composite conductive slurry, comprising the following steps:
(1) graphene and carbon nanotube conducting slurry of different proportion are prepared；
(2) prepared electrocondution slurry is quantitatively measured respectively in glass container, is placed on Raman spectrometer sample stage simultaneously
It is fixed, multiple raman spectrums are obtained respectively；
(3) raman spectrum that will acquire carries out data processing, calculates the peak face at the peak carbon D and the peak carbon 2D in raman spectrum
Product, and calculate the peak area average value at the peak carbon D and the peak carbon 2D in all raman spectrums of slurry of the same race；
(4) peak carbon 2D in obtained slurry raman spectrum of the same race and the peak carbon D peak area average value are carried out than worth A2D/
AD；
(5) A that will be obtained2D/ADGraphene content does curve in the corresponding slurry of ratio, obtain graphene content with
A2D/ADCurve of value, as standard curve；
(6) it takes and carries out Raman spectrum survey with the carbon nanotube to be measured of step (1) same amount-graphene composite conductive agent slurry
Examination, obtains multiple raman spectrums, and calculate A2D/ADRatio；
(7) A obtained in step (6)2D/ADValue corresponding graphene content on step (4) resulting standard curve is
For the content of graphene in the combined conductive agent to be measured.
The quantitative analysis method of the graphene composite conductive slurry, in step (1), the stone for preparing different proportion
Black alkene and carbon nanotube conducting slurry, the solvent used is N-Methyl pyrrolidone.
The quantitative analysis method of the graphene composite conductive slurry, in step (1), the mass fraction of graphene is distinguished
It is 40%, 50%, 60%, 70%, 80%, 90%.
The quantitative analysis method of the graphene composite conductive slurry, in step (1), the electrocondution slurry further includes matter
Measure the polyvinylpyrrolidone that score is 0.5%.
As shown from the above technical solution, the present invention can be distinguished using Raman spectrum be both carbon-based material graphene, carbon
The advantage of nanotube, amorphous carbon and graphite is realized and is carried out to the graphene in graphene-carbon nano tube combined conductive agent slurry
Quantitative analysis guarantees that carbon graphite alkene-carbon nanotube composite conductive agent slurry performance reaches requirement.This method operation letter
It is single, quick, it can be used for the constituent analysis in other carbon-based material combined conductive agent slurries, in carbon-based material conductive agent slurry
There is potential application prospect in terms of rapid evaluation.
Detailed description of the invention
Fig. 1 is the raman spectrum of several carbon-based materials；
Fig. 2 is that the present invention prepares different proportion graphene and the resulting raman spectrum of carbon nanotube conducting slurry；
Fig. 3 is the graphene of graphene-carbon nano tube combined conductive agent slurry to be measured in the embodiment of the present invention one containing spirogram；
Fig. 4 is the graphene of graphene-carbon nano tube combined conductive agent slurry to be measured in comparative example one of the present invention containing spirogram；
Fig. 5 is the graphene of graphene-carbon nano tube combined conductive agent slurry to be measured in comparative example two of the present invention containing spirogram；
Fig. 6 is the graphene of graphene-carbon nano tube combined conductive agent slurry to be measured in comparative example three of the present invention containing spirogram.
Specific embodiment
The present invention will be further described with reference to the accompanying drawing:
Embodiment 1:
(1) graphene and carbon nanotube conducting slurry of a series of different proportions are prepared, solvent is N-Methyl pyrrolidone,
Wherein the mass fraction of graphene is respectively 40%, 50%, 60%, 70%, 80%, 90%, remaining is carbon nanotube and polyvinyl pyrrole
Alkanone (PVP), PVP are dispersing agent, and mass fraction is fixed as 0.5%；
(2) configured slurry in 1 milliliter of step (1) is taken to be placed on Raman spectrometer sample stage in glass container respectively
And it is fixed, raman spectrum is obtained, slurry of the same race takes six spectrograms；As shown in Fig. 2, Fig. 2 is graphene and carbon nanotube ratio is
The resulting raman spectrum of the slurry of 4:6,5:5,6:4,3:7,2:8,1:9, graphene contains in slurry shown in spectrogram from top to bottom
Amount is respectively 90%, 80%, 70%, 60%, 50% and 40%.
(3) a series of raman spectrums in step (2) are subjected to data processing, calculate separately the peak carbon D and the carbon in spectrogram
The peak area at the peak 2D, and calculate the peak area average value at the peak carbon D and the peak carbon 2D in all spectrograms of slurry of the same race；
(4) peak carbon 2D in slurry spectrogram of the same race obtained in step (3) and the peak carbon D peak area average value are carried out than being worth
A2D/AD；
(5) by A obtained in step (4)2D/ADGraphene content does curve in the corresponding slurry of ratio, and stone can be obtained
Black alkene content and A2D/ADCurve of value, is considered as standard curve；
(6) existing a kind of graphene-carbon nano tube composite conducting slurry, graphene mass content account for carbon-based material 75~
85%, remaining 15~25% be mainly carbon nanotube, takes 1 milliliter of this kind of graphene-by step (2), step (3) and step (4)
Carbon nanotube composite conducting slurry carries out Raman spectrum test, equally takes six spectrograms and calculates A2D/ADRatio；
(7) A obtained in step (6)2D/ADValue corresponding graphene content on step (4) resulting standard curve is
72%, i.e. it is the present embodiment graphene-carbon nano tube composite guide to be measured that graphene content, which is 72%, Fig. 3, in this kind of conductive agent slurry
Electric agent slurry is in A2D/ADResulting graphene is corresponded on curve and contains spirogram, and a curve is mark described in embodiment one in figure
Directrix curve, dotted line ordinate corresponding with an intersections of complex curve is the A of graphene slurry to be measured in figure2D/ADValue, dotted line are corresponding
Content be graphene content, as shown in figure 3, graphene actual content is close in result and the conductive agent slurry.
Comparative example 1:
(1) graphene and carbon nanotube conducting slurry of a series of different proportions are prepared, solvent is N-Methyl pyrrolidone,
Wherein the mass fraction of graphene is respectively 40%, 50%, 60%, 70%, 80%, 90%, remaining is carbon nanotube and polyvinyl pyrrole
Alkanone (PVP), PVP are dispersing agent, and mass fraction is fixed as 0.5%；
(2) configured slurry in 1 milliliter of step (1) is taken to be placed on Raman spectrometer sample stage in glass container respectively
And it is fixed, raman spectrum is obtained, slurry of the same race takes six spectrograms；
(3) a series of raman spectrums in step (2) are subjected to data processing, calculate separately the peak carbon G and the carbon in spectrogram
The peak area at the peak 2D, and calculate the peak area average value at the peak carbon G and the peak carbon 2D in all spectrograms of slurry of the same race；
(4) peak carbon 2D in slurry spectrogram of the same race obtained in step (3) and the peak carbon G peak area average value are carried out than being worth
A2D/AG；
(5) by A obtained in step (4)2D/AGGraphene content does curve in the corresponding slurry of ratio, and stone can be obtained
Black alkene content and A2D/AGCurve of value, is considered as standard curve；
(6) existing a kind of graphene-carbon nano tube composite conducting slurry, graphene mass content account for carbon-based material 75~
85%, remaining 15~25% be mainly carbon nanotube, takes 1 milliliter of this kind of graphene-by step (2), step (3) and step (4)
Carbon nanotube composite conducting slurry carries out Raman spectrum test, equally takes six spectrograms and calculates A2D/AGRatio；
(7) A obtained in step (6)2D/AGValue corresponding graphene content on step (4) resulting standard curve is
59%, i.e. graphene content is 59% in this kind of conductive agent slurry, as shown in figure 4, a curve is described in this comparative example in figure
Standard curve, dotted line ordinate corresponding with an intersections of complex curve is the A of graphene slurry to be measured in figure2D/AGValue, dotted line
Corresponding content is graphene content；As shown in figure 4, test result is differed with graphene actual content in the conductive agent slurry
Farther out.
Comparative example 2:
(1) graphene and carbon nanotube conducting slurry of a series of different proportions are prepared, solvent is N-Methyl pyrrolidone,
Wherein the mass fraction of graphene is respectively 40%, 50%, 60%, 70%, 80%, 90%, remaining is carbon nanotube and polyvinyl pyrrole
Alkanone (PVP), PVP are dispersing agent, and mass fraction is fixed as 0.5%；
(2) configured slurry in 1 milliliter of step (1) is taken to be placed on Raman spectrometer sample stage in glass container respectively
And it is fixed, raman spectrum is obtained, slurry of the same race takes six spectrograms；
(3) a series of raman spectrums in step (2) are subjected to data processing, calculate separately the peak carbon D and the carbon in spectrogram
The peak intensity at the peak 2D, and calculate the peak intensity average value at the peak carbon D and the peak carbon 2D in all spectrograms of slurry of the same race；
(4) peak carbon 2D in slurry spectrogram of the same race obtained in step (3) and the peak carbon D peak intensity average value are carried out than being worth
I2D/ID；
(5) by I obtained in step (4)2D/IDGraphene content does curve in the corresponding slurry of ratio, and stone can be obtained
Black alkene content and I2D/IDCurve of value, is considered as standard curve；
(6) existing a kind of graphene-carbon nano tube composite conducting slurry, graphene mass content account for carbon-based material 75~
85%, remaining 15~25% be mainly carbon nanotube, takes 1 milliliter of this kind of graphene-by step (2), step (3) and step (4)
Carbon nanotube composite conducting slurry carries out Raman spectrum test, equally takes six spectrograms and calculates I2D/IDRatio；
(7) I obtained in step (6)2D/IDValue corresponding graphene content on step (4) resulting standard curve is
67.1%, i.e. graphene content is 67.1% in this kind of conductive agent slurry, as shown in figure 5, a curve is in this comparative example in figure
The standard curve, dotted line ordinate corresponding with an intersections of complex curve is the I of graphene slurry to be measured in figure2D/IDValue,
The corresponding content of dotted line is graphene content；As shown in figure 5, result is differed with graphene actual content in the conductive agent slurry
Farther out.
Comparative example 3:
(1) graphene and carbon nanotube conducting slurry of a series of different proportions are prepared, solvent is N-Methyl pyrrolidone,
Wherein the mass fraction of graphene is respectively 40%, 50%, 60%, 70%, 80%, 90%, remaining is carbon nanotube and polyvinyl pyrrole
Alkanone (PVP), PVP are dispersing agent, and mass fraction is fixed as 0.5%；
(2) configured slurry in 1 milliliter of step (1) is taken to be placed on Raman spectrometer sample stage in glass container respectively
And it is fixed, raman spectrum is obtained, slurry of the same race takes six spectrograms；
(3) a series of raman spectrums in step (2) are subjected to data processing, calculate separately the peak carbon G and the carbon in spectrogram
The peak intensity at the peak 2D, and calculate the peak intensity average value at the peak carbon G and the peak carbon 2D in all spectrograms of slurry of the same race；
(4) peak carbon 2D in slurry spectrogram of the same race obtained in step (3) and the peak carbon G peak intensity average value are carried out than being worth
I2D/IG；
(5) by I obtained in step (4)2D/IGGraphene content does curve in the corresponding slurry of ratio, and stone can be obtained
Black alkene content and I2D/IGCurve of value, is considered as standard curve；
(6) existing a kind of graphene-carbon nano tube composite conducting slurry, graphene mass content account for carbon-based material 75~
85%, remaining 15~25% be mainly carbon nanotube, takes 1 milliliter of this kind of graphene-by step (2), step (3) and step (4)
Carbon nanotube composite conducting slurry carries out Raman spectrum test, equally takes six spectrograms and calculates I2D/IGRatio；
(7) I obtained in step (6)2D/IGValue corresponding graphene content on step (4) resulting standard curve is
56%, i.e. graphene content is 56% in this kind of conductive agent slurry, as shown in fig. 6, a curve is described in this comparative example in figure
Standard curve, dotted line ordinate corresponding with an intersections of complex curve is the I of graphene slurry to be measured in figure2D/IGValue, dotted line
Corresponding content is graphene content；As shown in fig. 6, its test result and graphene actual content phase in the conductive agent slurry
Difference is farther out.
It is compound by embodiment 1 and comparative example 1, comparative example 2, the result of comparative example 3 and this kind of carbon nanotube-graphene
In conductive agent slurry graphene actual content comparison it is found that using carbon the peak D and the peak 2D peak area ratio (A2D/AD) draw
Standard curve is close with actual content come the content for quantifying graphene in conductive agent slurry, and gained work is bent in 3 kinds of comparative examples
Line quantitative result differs farther out with actual content, therefore uses the peak D and the peak 2D peak area ratio (A of carbon2D/AD) draw standard curve
Method quantify graphene content in carbon nanotube-graphene conductive agent slurry.
Embodiment described above only describe the preferred embodiments of the invention, not to model of the invention
It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention
The various changes and improvements that case is made should all be fallen into the protection scope that claims of the present invention determines.
Claims (3)
1. a kind of quantitative analysis method of graphene composite conductive slurry, which comprises the following steps:
(1) graphene and carbon nanotube conducting slurry of different proportion are prepared, solvent is N-Methyl pyrrolidone；
(2) prepared electrocondution slurry is quantitatively measured respectively in glass container, is placed on Raman spectrometer sample stage and fixed,
Multiple raman spectrums are obtained respectively；
(3) raman spectrum that will acquire carries out data processing, calculates the peak area at the peak carbon D and the peak carbon 2D in raman spectrum, and
Calculate the peak area average value at the peak carbon D and the peak carbon 2D in all raman spectrums of slurry of the same race；
(4) peak carbon 2D in obtained slurry raman spectrum of the same race and the peak carbon D peak area average value are carried out than worth A2D/AD；
(5) A that will be obtained2D/ADGraphene content does curve in the corresponding slurry of ratio, obtains graphene content and A2D/AD
Curve of value, as standard curve；
(6) it takes and carries out Raman spectrum test with the carbon nanotube to be measured of step (1) same amount-graphene composite conductive agent slurry, obtain
Multiple raman spectrums are taken, and calculate A2D/ADRatio；
(7) A obtained in step (6)2D/ADValue corresponding graphene content on step (4) resulting standard curve is should
The content of graphene in combined conductive agent to be measured.
2. the quantitative analysis method of graphene composite conductive slurry according to claim 1, it is characterised in that: step (1)
In, the mass fraction of the graphene is respectively 40%, 50%, 60%, 70%, 80%, 90%.
3. the quantitative analysis method of graphene composite conductive slurry according to claim 1, it is characterised in that: step (1)
In, the electrocondution slurry further includes the polyvinylpyrrolidone that mass fraction is 0.5%.
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| CN107561055B (en) * | 2017-08-16 | 2020-09-01 | 常州二维碳素科技股份有限公司 | Method for judging graphene component and content in material |
| CN107482222A (en) * | 2017-09-05 | 2017-12-15 | 深圳市比克动力电池有限公司 | Combined conductive agent, electrodes of lithium-ion batteries and lithium ion battery |
| CN108398417A (en) * | 2018-02-05 | 2018-08-14 | 合肥国轩高科动力能源有限公司 | A kind of method of conductive agent deployment conditions in evaluation based lithium-ion battery positive plate |
| CN109142405B (en) * | 2018-07-19 | 2021-02-09 | 合肥国轩高科动力能源有限公司 | Quantitative analysis method for graphene/carbon nanotube composite conductive slurry |
| CN110895234B (en) * | 2018-12-29 | 2020-11-06 | 江苏天奈科技股份有限公司 | Detection method of graphene composite slurry |
| CN110197481B (en) * | 2019-05-30 | 2021-04-09 | 苏州大学 | Graphene fingerprint peak analysis method based on big data analysis |
| CN111366572A (en) * | 2020-03-27 | 2020-07-03 | 苏州聚龙能源科技有限公司 | Method for quantitatively analyzing content of graphene in graphene composite conductive slurry |
| CN111596008A (en) * | 2020-05-14 | 2020-08-28 | 上海超碳石墨烯产业技术有限公司 | Quantitative analysis method for components of graphene mixture |
| CN111710371A (en) * | 2020-06-16 | 2020-09-25 | 齐鲁交通发展集团有限公司 | Method for determining component content of carbon fiber/graphene conductive asphalt concrete |
| CN112305429B (en) * | 2020-09-28 | 2022-08-09 | 合肥国轩高科动力能源有限公司 | Estimation method for discharge depth of lithium ion battery |
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