CN112663329A - Simple acid treatment method for graphite felt - Google Patents
Simple acid treatment method for graphite felt Download PDFInfo
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- CN112663329A CN112663329A CN202011537375.3A CN202011537375A CN112663329A CN 112663329 A CN112663329 A CN 112663329A CN 202011537375 A CN202011537375 A CN 202011537375A CN 112663329 A CN112663329 A CN 112663329A
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- graphite felt
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- bath kettle
- nitric acid
- acid treatment
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 154
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 151
- 239000010439 graphite Substances 0.000 title claims abstract description 151
- 238000010306 acid treatment Methods 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 50
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 49
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 238000005520 cutting process Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims description 12
- 230000007935 neutral effect Effects 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 239000002699 waste material Substances 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 abstract description 7
- 239000013543 active substance Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 230000004913 activation Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- -1 nitric acid activated graphite Chemical class 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- 238000003860 storage Methods 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
- 125000000524 functional group Chemical group 0.000 description 9
- 239000001301 oxygen Substances 0.000 description 9
- 238000005259 measurement Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- XOJVVFBFDXDTEG-UHFFFAOYSA-N Norphytane Natural products CC(C)CCCC(C)CCCC(C)CCCC(C)C XOJVVFBFDXDTEG-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
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Abstract
The invention discloses a method for treating a graphite felt by acid. The invention aims to solve the problem of hydrophobicity of the graphite felt, improve electrochemical performance of the graphite felt and enable growth of active substances to be more beneficial. The chemicals used in the invention are mainly graphite felt and concentrated nitric acid. The preparation method of the medium-concentration nitric acid activated graphite felt comprises the following steps: firstly, cutting a graphite felt into a proper size and mixing the graphite felt with concentrated nitric acid in a beaker; secondly, heating the water bath kettle to 100 ℃; thirdly, putting the beaker filled with the concentrated nitric acid and the graphite felt into a water bath kettle, and timing, wherein the time is preferably 1 hour; and fourthly, after the activation is finished, taking out the graphite felt, cleaning and drying the graphite felt overnight in a constant temperature environment of 60 ℃. The invention has the advantages that: firstly, the method for treating the graphite felt by the concentrated nitric acid is simple and easy to operate, and the instrument is flexible to use; secondly, the hydrophobicity of the graphite felt after acid treatment is greatly improved; finally, the electrochemical performance of the graphite felt after acid treatment is greatly improved, and compared with the untreated graphite felt, the charge storage capacity is hundreds of times.
Description
Technical Field
The invention belongs to the field of electrochemistry, and relates to a method for treating a graphite felt by concentrated nitric acid and a method for modifying the surface of the graphite felt and introducing oxygen-containing functional groups.
Background
With the continuous development of scientific technology, the demand of energy is increasing, and traditional fossil fuels cause serious environmental pollution, so that green energy is greatly expected, however, the construction of energy storage devices with high energy density is a hot research spot due to the instability of green energy. Compared with most materials, the graphite felt has the advantages of low cost, large specific surface area, high stability, capability of being bent to be made into wearable equipment and the like, and the graphite felt has commercial advantages. However, graphite felt also has its own problems. For example, the limited capacity of graphite felt fundamentally restricts its direct application in energy storage; on the other hand, the graphite felt is hydrophobic in nature, which makes it not very strong, easy to fall off or impossible to bond with some non-metallic oxides. Therefore, the processing of the carbon-based electrode has important significance for further improving the electrochemical performance of the carbon-based electrode under the condition of keeping the advantages of the carbon-based electrode. The graphite felt based on concentrated nitric acid simple treatment shows excellent electrochemical performance. In KOH solution, the volume of the graphite felt after the concentrated nitric acid treatment is changed from the original 0.01mF cm-2Lifting to 272.6mF cm-2In addition, the hydrophobicity of the graphite felt was also found to be greatly improved by contact angle measurement. In the stability test, the treated graphite felt was subjected to many charge-discharge cycles in KOH solution, and its capacity loss was almost negligible.
Disclosure of Invention
The invention provides a simple method for treating a graphite felt by acid, in particular to a method for improving the electrochemical performance of the graphite felt by introducing oxygen-containing functional groups, which aims to solve the problems of low energy storage and poor binding capacity with other active substances of the existing graphite felt.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for simple acid treatment of graphite felt comprises the following steps:
firstly, cutting a graphite felt into 2.5 multiplied by 2.5cm, and manufacturing two graphite felts with the same size for later use;
step two, opening the water bath kettle, setting the temperature of the water bath kettle to be 100 ℃, and waiting for the water bath kettle to be heated;
step three, measuring 40ml of concentrated nitric acid, pouring the concentrated nitric acid into a beaker with a proper size, putting the graphite felt in the step one into the beaker, and transferring the graphite felt into a water bath kettle in the step two;
fourthly, after the water bath kettle is heated to 100 ℃, timing is started, and the reaction time is 1 h;
fifthly, after the concentrated nitric acid in the fourth step is fully reacted with the graphite felt, taking the beaker out of the water bath kettle, closing the water bath kettle, taking the graphite felt out of the beaker, and carefully treating the waste liquid;
sixthly, repeatedly washing the graphite felt until the PH value of the washing solution is neutral;
and seventhly, transferring the cleaned graphite felt to a vacuum drying oven, and adjusting the temperature to 60 ℃ for drying.
In the above-mentioned method, the first step of the method,
in the first step, the selected graphite felt is preferably 1mm thick.
And in the third step, when the water bath kettle is heated to about 60 ℃, the beaker is transferred into the water bath kettle.
In the fourth step, the cover of the water bath kettle is covered to keep the temperature stable.
In the fifth step, the solution in the beaker is taken out and turns brown yellow.
In the sixth step, after the first cleaning solution is neutral, the next cleaning is still needed, and then the pH test of the cleaning solution is carried out to ensure that the nitric acid does not remain on the graphite felt.
In the seventh step, the graphite felt drying time needs to be more than 8 hours to ensure that the graphite felt is completely dried.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention adopts concentrated nitric acid as a main chemical for treating the graphite felt, and has low cost.
(2) The temperature adopted by the invention is 100 ℃, is the boiling temperature of water, can directly provide the required temperature requirement by using the water bath kettle, and has the advantages of relatively simple and convenient operation and good reproducibility.
(3) The graphite felt prepared by the invention has excellent electrochemical performance, the stability of the graphite felt is not damaged while the capacity is greatly improved, and meanwhile, the improvement of the hydrophilicity is also beneficial to the combination of the graphite felt and other active substances, and the capacity of an electrode is further improved.
Drawings
FIG. 1 is an SEM image of a raw graphite felt;
FIG. 2 is an SEM image of a graphite felt after concentrated nitric acid treatment;
FIG. 3 is a contact angle measurement of a raw graphite felt;
FIG. 4 is a contact angle measurement of a graphite felt after concentrated nitric acid treatment;
FIG. 5 is a CV diagram of raw graphite felt in KOH solution;
FIG. 6 is a CV diagram of the graphite felt in KOH solution after concentrated nitric acid treatment;
FIG. 7 is an XPS survey of a graphite felt after treatment with virgin graphite felt and concentrated nitric acid;
FIG. 8 is a C1s spectrum of a graphite felt after concentrated nitric acid treatment;
FIG. 9 Raman plots of the original graphite felt and the graphite felt after concentrated nitric acid treatment;
fig. 10 is a graph of the nitrogen adsorption profile of the graphite felt after treatment with virgin graphite felt and concentrated nitric acid.
Detailed Description
The present invention will be further described with reference to the following examples and the accompanying drawings.
The reaction time, which is sensitive to the final product, must be strictly controlled in the steps of the present invention.
The reaction temperature must be strictly controlled in the steps of the invention, and the temperature needs to be kept stable in the experimental process.
The amount of reactants must be strictly controlled in the steps of the invention, and the reaction ratio of the concentrated nitric acid and the graphite felt is certain.
Example 1
A simple graphite felt acid treatment mode and a method for improving the electrochemical performance of graphite felt acid by introducing oxygen-containing functional groups comprises the following steps:
firstly, cutting the graphite felt into 2.5 multiplied by 2.5cm, and manufacturing two pieces of graphite felt with the same size for later use. (ii) a
Step two, opening the water bath kettle, setting the temperature of the water bath kettle to be 100 ℃, and waiting for the water bath kettle to be heated;
thirdly, 40ml of concentrated nitric acid is measured and poured into a beaker with a proper size, and the graphite felt in the first step is added
Putting into a beaker, and then transferring into a water bath kettle in the second step;
fourthly, after the water bath kettle is heated to 100 ℃, timing is started, and the reaction time is 1 h;
fifthly, after the concentrated nitric acid in the fourth step is fully reacted with the graphite felt, taking the beaker out of the water bath kettle, closing the water bath kettle, taking the graphite felt out of the beaker, and carefully treating the waste liquid;
sixthly, repeatedly washing the graphite felt until the PH value of the washing solution is neutral;
and seventhly, transferring the cleaned graphite felt to a vacuum drying oven, and adjusting the temperature to 60 ℃ for drying.
Example 2
A simple graphite felt acid treatment mode and a method for improving the electrochemical performance of graphite felt acid by introducing oxygen-containing functional groups comprises the following steps:
firstly, cutting the graphite felt into 2.5 multiplied by 2.5cm, and manufacturing two pieces of graphite felt with the same size for later use. (ii) a
Step two, opening the water bath kettle, setting the temperature of the water bath kettle to be 100 ℃, and waiting for the water bath kettle to be heated;
step three, measuring 40ml of concentrated nitric acid, pouring the concentrated nitric acid into a beaker with a proper size, putting the graphite felt in the step one into the beaker, and transferring the graphite felt into a water bath kettle in the step two;
fourthly, after the water bath kettle is heated to 100 ℃, timing is started, and the reaction time is 1 h;
fifthly, after the concentrated nitric acid in the fourth step is fully reacted with the graphite felt, taking the beaker out of the water bath kettle, closing the water bath kettle, taking the graphite felt out of the beaker, and carefully treating the waste liquid;
sixthly, repeatedly washing the graphite felt until the PH value of the washing solution is neutral;
and seventhly, transferring the cleaned graphite felt to a vacuum drying oven, and adjusting the temperature to 60 ℃ for drying.
Example 3
A simple graphite felt acid treatment mode and a method for improving the electrochemical performance of graphite felt acid by introducing oxygen-containing functional groups comprises the following steps:
firstly, cutting the graphite felt into 2.5 multiplied by 2.5cm, and manufacturing two pieces of graphite felt with the same size for later use. (ii) a
Step two, opening the water bath kettle, setting the temperature of the water bath kettle to be 100 ℃, and waiting for the water bath kettle to be heated;
step three, measuring 40ml of concentrated nitric acid, pouring the concentrated nitric acid into a beaker with a proper size, putting the graphite felt in the step one into the beaker, and transferring the graphite felt into a water bath kettle in the step two;
fourthly, after the water bath kettle is heated to 100 ℃, timing is started, and the reaction time is 1 h;
fifthly, after the concentrated nitric acid in the fourth step is fully reacted with the graphite felt, taking the beaker out of the water bath kettle, closing the water bath kettle, taking the graphite felt out of the beaker, and carefully treating the waste liquid;
sixthly, repeatedly washing the graphite felt until the PH value of the washing solution is neutral;
and seventhly, transferring the cleaned graphite felt to a vacuum drying oven, and adjusting the temperature to 60 ℃ for drying.
Example 4
A simple graphite felt acid treatment mode and a method for improving the electrochemical performance of graphite felt acid by introducing oxygen-containing functional groups comprises the following steps:
firstly, cutting the graphite felt into 2.5 multiplied by 2.5cm, and manufacturing two pieces of graphite felt with the same size for later use. (ii) a
Step two, opening the water bath kettle, setting the temperature of the water bath kettle to be 100 ℃, and waiting for the water bath kettle to be heated;
step three, measuring 40ml of concentrated nitric acid, pouring the concentrated nitric acid into a beaker with a proper size, putting the graphite felt in the step one into the beaker, and transferring the graphite felt into a water bath kettle in the step two;
fourthly, after the water bath kettle is heated to 100 ℃, timing is started, and the reaction time is 1 h;
fifthly, after the concentrated nitric acid in the fourth step is fully reacted with the graphite felt, taking the beaker out of the water bath kettle, closing the water bath kettle, taking the graphite felt out of the beaker, and carefully treating the waste liquid;
sixthly, repeatedly washing the graphite felt until the PH value of the washing solution is neutral;
and seventhly, transferring the cleaned graphite felt to a vacuum drying oven, and adjusting the temperature to 60 ℃ for drying.
The structure of the graphite felt after the acid treatment is kept after the graphite felt reacts with acid and is not greatly damaged; the surface of the graphite felt is changed from hydrophobic to hydrophilic; oxygen-containing functional groups are introduced to the surface of the graphite felt, so that the electrochemical performance of the graphite felt is improved. The volume of the graphite felt after the concentrated nitric acid treatment is 0.01mF cm-2Lifting to 272.6mF cm-2And meanwhile, the hydrophobicity of the graphite felt is also greatly improved.
FIG. 1 is an SEM image of a raw graphite felt; the results of the tests on the treated graphite felt of examples 1-4 are shown in FIGS. 2-10:
FIG. 2 is an SEM image of the graphite felt after concentrated nitric acid treatment, and it can be seen that there is no great difference in surface morphology and the structure of the graphite felt is not destroyed;
FIG. 3 is a contact angle measurement of a pristine graphite felt for 10 minutes, and the size of the drop before and after the test is not greatly changed, indicating that the pristine graphite felt is hydrophobic;
FIG. 4 is a contact angle measurement of a graphite felt after concentrated nitric acid treatment, immediately after the liquid drop just contacted the graphite felt during the test, showing that the graphite felt becomes hydrophilic after concentrated nitric acid treatment;
FIG. 5 is a CV plot of the raw graphite felt in KOH solution at a sweep rate of 100mV/s with the area of the CV curve representing the electrode capacity, and it can be seen that the capacity of the raw graphite felt in KOH solution is very small;
FIG. 6 is a CV diagram of graphite felt in KOH solution after concentrated nitric acid treatment at a sweep rate of 100mV/s, which is a large increase in capacity compared to FIG. 5, mainly due to the introduction of oxygen-containing functional groups after concentrated nitric acid treatment of the graphite felt;
FIG. 7 is XPS full spectra of original graphite felt and graphite felt after concentrated nitric acid treatment, which can clearly find that graphitization (C element) of the graphite felt is obviously reduced and content of O element is obviously increased after concentrated nitric acid treatment;
fig. 8 is a C1s spectrum of the graphite felt after concentrated nitric acid treatment, and it can be found that the oxygen-containing functional groups introduced by the graphite felt after concentrated nitric acid treatment are mainly C-O-R, O-C ═ O, and C ═ O;
FIG. 9 is a Raman diagram of the original graphite felt and the graphite felt after the concentrated nitric acid treatment, wherein the ratio of D to G is the defect expression of the graphite felt, and the defect of the graphite felt is increased after the concentrated nitric acid treatment, which also indicates that the structure of the graphite felt is not damaged.
FIG. 10 is a graph showing the nitrogen adsorption of the original graphite felt and the graphite felt after concentrated nitric acid treatment, with a significant increase at P/P0<0.1, indicating the presence of micropores in both samples, while the graphite felt after concentrated nitric acid treatment has a significant hysteresis loop at higher pressures, indicating the presence of mesopores.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (7)
1. A simple acid treatment method for a graphite felt is characterized by comprising the following steps:
firstly, cutting a graphite felt into 2.5 multiplied by 2.5cm, and manufacturing two graphite felts with the same size for later use;
step two, opening the water bath kettle, setting the temperature of the water bath kettle to be 100 ℃, and waiting for the water bath kettle to be heated;
step three, measuring 40ml of concentrated nitric acid, pouring the concentrated nitric acid into a beaker with a proper size, putting the graphite felt in the step one into the beaker, and transferring the graphite felt into a water bath kettle in the step two;
fourthly, after the water bath kettle is heated to 100 ℃, timing is started, and the reaction time is 1 h;
fifthly, after the concentrated nitric acid in the fourth step is fully reacted with the graphite felt, taking the beaker out of the water bath kettle, closing the water bath kettle, taking the graphite felt out of the beaker, and carefully treating the waste liquid;
sixthly, repeatedly washing the graphite felt until the PH value of the washing solution is neutral;
and seventhly, transferring the cleaned graphite felt to a vacuum drying oven, and adjusting the temperature to 60 ℃ for drying.
2. The method for simple acid treatment of graphite felt according to claim 1, wherein the method comprises the following steps: in the first step, the selected graphite felt is 1mm thick.
3. The method for simple acid treatment of graphite felt according to claim 1, wherein the method comprises the following steps: and in the third step, when the water bath kettle is heated to about 60 ℃, the beaker is transferred into the water bath kettle.
4. The method for simple acid treatment of graphite felt according to claim 1, wherein the method comprises the following steps: in the fourth step, the cover of the water bath kettle is covered to keep the temperature stable.
5. The method for simple acid treatment of graphite felt according to claim 1, wherein the method comprises the following steps: and in the fifth step, taking out the beaker, and changing the color of the solution into brown yellow.
6. The method for simple acid treatment of graphite felt according to claim 1, wherein the method comprises the following steps: and sixthly, after the first cleaning solution is neutral, the next cleaning is still needed, and then the PH test of the cleaning solution is carried out to ensure that the nitric acid does not remain on the graphite felt.
7. The method for simple acid treatment of graphite felt according to claim 1, wherein the method comprises the following steps: in the seventh step, the graphite felt drying time needs to be more than 8 hours to ensure that the graphite felt is completely dried.
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2020
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CN106356203A (en) * | 2016-10-31 | 2017-01-25 | 福州大学 | Nickel cobaltate nano-sheet/graphite felt composite material and preparation and application thereof |
CN109546163A (en) * | 2018-11-15 | 2019-03-29 | 电子科技大学 | A kind of method of modifying of organic flow battery graphite felt electrode |
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