CN103021674A - Carbon-based ionic intercalation energy-storage electrode material and preparation process thereof - Google Patents
Carbon-based ionic intercalation energy-storage electrode material and preparation process thereof Download PDFInfo
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Abstract
The invention discloses a carbon-based ionic intercalation energy-storage electrode material and a preparation process thereof and belongs to the technical field of carbon-based electrode materials. The material is composed of ordered graphite-like micro-crystals and unordered turbostratic carbon structures, wherein typical unordered turbostratic carbon structures are arranged around ordered graphite-like micro-crystal structures. The preparation process comprises the steps of conducting a thermal polycondensation reaction at the temperature of 320-400 DEG C with coal-tar pitch or ethylene tar pitch serving as a raw material, carbonizing the pitch powder which is subjected to thermal polycondensation at the temperature of 600-900 DEG C, conducting potassium hydroxide (KOH) activation at the temperature of 600-900 DEG C, and finally obtaining the material. The material has the advantages of being simple to operate, continuous in process, good in controllability and capable of achieving large-scale production easily. The prepared carbon-based ionic intercalation energy-storage electrode material has a unique structure of ordered and unordered inlaying and is high in capacitance and high in voltage resistance.
Description
Technical field
The present invention relates to a kind of charcoal base ion intercalation energy storage electrode material and preparation method thereof, belong to charcoal base electrode material technology field.
Background technology
The characteristics such as physical and chemical performance is stable, cheap, wide material sources, environmental friendliness are widely used in the electrochemical energy storage field, the particularly application of double electric layer capacitor, lithium ion battery electrode material to Carbon Materials because having.At present, the Carbon Materials that is applied to the energy storage field mainly contains: active carbon, activated carbon fiber, carbon nano-tube, metal carbides base Carbon Materials, hard charcoal, graphite etc.Wherein, electric double layer stores electric charge with electrode material such as the main solid/liquid interfaces electric double layer that produces between electrode/electrolyte that relies on such as active carbon, activated carbon fiber, produces the capacitance of farad level.Energy density computing formula according to capacitor
E=1/2
CV 2(wherein
CRepresentative is than electric capacity,
VThe expression operating voltage) as can be known, (1 ~ 5wh/kg) has limited its further developing in the energy storage field to the energy density that traditional double electric layer capacitor is lower.
Many researchers are devoted to from improving
CAngle make great efforts to improve the energy density of device
EAs template, dopamine is carbon matrix precursor to Li Chunzhong etc. with the porous magnesia nanometer sheet, has prepared to have a kind of mesoporous carbon nanometer sheet electrode material for super capacitor, under the 0.1A/g current density, with 1mol/dm
3Sulfuric acid solution is the double electric layer capacitor of electrolyte, and this electrode material quality is 216F/g (CN201210190112.9) than electric capacity.But the ratio electric capacity based on the porous carbon material of electric double layer energy storage principle
CRaising leeway limited, mainly be subject to the difficulty of further raising porous carbon material specific area.At present, the specific area of porous charcoal can be accomplished 3200m
2/ g if further improve, can cause declining to a great extent of the energy storage density of electrode material under unit volume.Therefore, more focus has been transferred to the voltage-resistent characteristic that improves the carbonaceous electrode in recent years
VRaising on.The larger specific area of tradition porous carbon electrode causes the outstanding bond number amount of carbon to increase, the electrochemical reaction avtive spot that is the porous charcoal surface increases, and then cause being higher than the irreversible electrochemical reaction of appearance more than the 2.7V, this condition restriction the trouble free service voltage of organic system electrochemical capacitor must be lower than 2.7V (although the voltage range of organic electrolyte 4.0 ~ 4.5V) causes the electrochemical capacitor energy density limited.Hold high up and bigly mediumly (CN201210135516.8) adopt liquid phase to process away inorganic oxide carrier, metal at " a kind of purification process of the carbon nano-electrode material for ultracapacitor ", metal sulfide, metal carbides etc., the methods such as freeze drying, high temperature weak oxide gas treatment have obtained the ultracapacitor carbon nano-electrode material at 4 ~ 6.5V withstand voltage properties, but above-mentioned preparation method's technological operation is comparatively complicated, and cost is higher.
Therefore the electrode based on electrochemical reaction (for example ion intercalation) is having larger advantage aspect the raising energy density.By the lithium-ion electric pool technology as can be known, Carbon Materials such as hard charcoal, graphite etc. can be embedded by lithium ion under more negative electromotive force, and then obtain higher energy density.Based on above-mentioned analysis, this paper proposes the charcoal base ion intercalation energy storage electrode material that has larger capacity and voltage-resistent characteristic with a kind of, this material is different from hard charcoal and graphite material, it is comprised of orderly class graphite microcrystal and unordered disorderly layer carbon structure, its ordered structure can be carried out the energy storage of ion intercalation under certain voltage, obtains higher capacitance; In addition, this material has higher voltage-resistent characteristic, the porous charcoal that is different from traditional high-specific surface area, this electrode material has lower specific area, and some hetero-atoms and functional group have been removed through high temperature carbonization, so that the content of material surface electrochemical reaction avtive spot is less, thereby reduced with the irreversible reaction of electrolyte active, simultaneously its disordered structure has spatially limited ordered lamellar structure and has come off because a large amount of ions carry out the lamella that intercalation causes, and then has improved significantly the withstand voltage properties of material.This material preparation process is simple, is easy to obtain.
Summary of the invention
The object of the present invention is to provide a kind of charcoal base ion intercalation energy storage electrode material and preparation method thereof, this material has higher specific capacity
CAnd operating voltage
V, its preparation method process is simple.
The present invention is realized by following technical proposals, a kind of charcoal base ion intercalation energy storage electrode material, and this material is average grain diameter 20 ~ 50 μ m, its specific area is 278 ~ 1048m
2/ g, pore volume are 0.12 ~ 0.5cm
3/ g is characterized in that, this material is comprised of orderly class graphite microcrystal and unordered disorderly layer carbon structure, and wherein orderly class graphite microcrystal is 5% ~ 10% of this charcoal base electrode material structure, and crystallite size is 2 ~ 10nm, and the interlamellar spacing of crystallite is 0.359～0.385nm; Be typical unordered disorderly layer carbon structure around the crystallite.
The charcoal base ion intercalation energy storage electrode material preparation method of said structure is characterized in that comprising following process:
1) coal tar asphalt or ethylene bottom oil pitch are added in the reactor, with 0.5 ~ 1.2m
3The speed of/h passes into nitrogen, continue to stir down, is warming up to 320 ~ 400 ℃ with 1 ~ 10 ℃/min of heating rate, carries out thermal polycondensation reaction 2 ~ 6h, and the softening point that obtains after the polycondensation is 150 ~ 220 ℃ of pitches;
2) step 1) being obtained pitch after the polycondensation pulverizes 20 ~ 50 μ m powder and adds in the retort, with 0.5 ~ 1.2m
3The speed of/h passes into nitrogen in retort, be warming up to 600 ~ 900 ℃ with the heating rate of 5 ~ 20 ℃/min, and constant temperature charing 0.5 ~ 4h naturally cools to room temperature, obtains the asphalt powder after the charing.
3) with step 2) asphalt powder after the charing that obtains and KOH 1:(0.5 ~ 2 in mass ratio), add in the retort and in nitrogen atmosphere, be warming up to 600 ~ 900 ℃ with 5 ~ 20 ℃/min heating rate, priming reaction 0.5 ~ 2h, naturally cool to room temperature, with 1M HCl solution boiling washing 3 ~ 5h, after being neutrality with deionized water cyclic washing to cleaning solution again, 80 ~ 120 ℃ of lower dry processing of temperature, obtain charcoal base ion intercalation energy storage electrode material.
Advantage of the present invention is as follows: preparation manipulation of the present invention is simple, process is continuous, and controllability is good, is easy to accomplish scale production.The electrode material of prepared charcoal base ion intercalation energy storage is different from hard charcoal and graphite type material, and it has the in order unordered unique texture of inlaying.Wherein orderly class graphite microcrystal growth is comparatively complete, and its crystallite size is 2 ~ 10nm, and the interlamellar spacing of crystallite is 0.359～0.385nm, and this crystallite can carry out the energy storage of ion intercalation under certain voltage, obtains higher capacitance; In addition, its disordered structure has kept the porousness feature of porous carbon material, guaranteed the mass transfer characteristic of electrolyte ion, spatially limited simultaneously ordered lamellar structure and come off because a large amount of ions carry out the lamella that intercalation causes, and then made this material have the higher voltage-resistent characteristic of 2.7 ~ 4.0V.
Description of drawings
Fig. 1 is the transmission electron micrograph of the charcoal base ion intercalation electrode material of the embodiment of the invention 1 preparation.
Fig. 2 is the X-ray diffraction spectrogram of the charcoal base ion intercalation electrode material of the embodiment of the invention 1 preparation.
Fig. 3 is the nitrogen Adsorption and desorption isotherms figure of the charcoal base ion intercalation electrode material of the embodiment of the invention 1 preparation.
Fig. 4 be the charcoal base ion intercalation electrode material of the embodiment of the invention 1 preparation in the 100mA/g current density, the constant current charge-discharge curve chart under the different operating voltage.
Embodiment
Embodiment 1
350g Jining pix carbonis praeparsta pitch (softening point is 33 ℃) is added in the reactor, with 1.2m
3The speed of/h passes into nitrogen, continue to stir down, is warming up to 400 ℃ with 10 ℃/min of heating rate, carries out thermal polycondensation reaction 3h, and stopped heating naturally cools to room temperature, obtains the 176g softening point and be pitch after 158 ℃ the polycondensation.Then asphalt powder is broken to 40 μ m after getting the 10g polycondensation, adds retort with 0.5m
3The speed of/h passes into nitrogen, and the heating rate of 10 ℃/min is warming up to 800 ℃, and charing 2h naturally cools to room temperature.Obtained 7.5g charing sample is mixed with 15gKOH in the adding retort, in nitrogen atmosphere, be warming up to 800 ℃ with 10 ℃/min heating rate, activation 2h, naturally cool to room temperature, with 500ml 1MHCl solution boiling washing 5h, be neutral with 100ml deionized water cyclic washing 3 times to cleaning solution again, 120 ℃ of lower dry processing, obtain 6.4g charcoal base ion intercalation energy storage carbon electrode material.
Charcoal base ion intercalation energy storage carbon electrode material obtained above adopts Tecnai G2 F20 type transmission electron microscope, D/MAX2500V/PC type X-ray diffractometer and TriStar3000 type N
2Adsorption instrument is tested, and the result shows that this material contains the comparatively complete class graphite microcrystal of 6% growth, and crystallite size is in 2 ~ 10nm scope, and interlamellar spacing is 0.359nm, and its BET specific area is 1018m
2/ g, pore volume is 0.48cm
3/ g.With the 0.5g sample, 0.059g conductive black (Carbon VXC 72) and 0.029g binding agent (polyvinylidene fluoride PVDF) are mixed, size mixing, and film, and the preparation carbon resistance rod is with 1mol/dm
3Et
4NBF
4The acetonitrile mixed solution be electrolyte, assembling coin shape simulation double electric layer capacitor.The LAND CT 2001A type cell tester that adopts Wuhan Jin Nuo Electrosource, Inc. to produce, constant current charge-discharge characteristic and the withstand voltage properties of study sample.The test voltage scope is 0 ~ 2.7V, 0 ~ 3.5V, 0 ~ 3.7V and 0 ~ 4.0V, and current density is 100mA/g.Record the carbon electrode material proof voltage up to 4.0V, and the energy density of capacitor is 29.4wh/kg.
Embodiment 2
The present embodiment difference from Example 1 is: change carbonization temperature into 900 ℃ by 800 ℃, carbonization time changes 1h into by 2h.Prepared charing sample becomes 7.2g by 7.5g, and activation process KOH consumption changes 14.4g into by 15g, finally makes charcoal base ion intercalation energy storage carbon electrode material quality and becomes 6.1g by 6.4g.
Charcoal base ion intercalation energy storage carbon electrode material obtained above adopts Tecnai G2 F20 type transmission electron microscope, D/MAX2500V/PC type X-ray diffractometer and TriStar3000 type N
2Adsorption instrument carries out test analysis, and the result shows that this material contains the comparatively complete class graphite microcrystal of 10% growth, and crystallite size is in 2 ~ 10nm scope, and interlamellar spacing is 0.378nm, and its BET specific area is 826m
2/ g, pore volume is 0.24cm
3/ g.With the 0.5g sample, 0.059g conductive black (Carbon VXC 72) and 0.029g binding agent (polyvinylidene fluoride PVDF) are mixed, size mixing, and film, and the preparation carbon resistance rod is with 1mol/dm
3Et
4NBF
4The acetonitrile mixed solution be electrolyte, assembling coin shape simulation double electric layer capacitor.The LAND CT 2001A type cell tester that adopts Wuhan Jin Nuo Electrosource, Inc. to produce, constant current charge-discharge characteristic and the withstand voltage properties of study sample.The test voltage scope is 0 ~ 2.7V, 0 ~ 3.5V, 0 ~ 3.7V and 0 ~ 4.0V, and current density is 100mA/g.Record the carbon electrode material proof voltage up to 4.0V, and the energy density of capacitor is 28.9wh/kg.
Embodiment 3
The present embodiment difference from Example 1 is: change the quality 15g of KOH into 3.75g.Finally make charcoal base ion intercalation energy storage carbon electrode material quality and become 6.9g by 6.4g.
Charcoal base ion intercalation energy storage carbon electrode material obtained above adopts Tecnai G2 F20 type transmission electron microscope, D/MAX2500V/PC type X-ray diffractometer and TriStar3000 type N
2Adsorption instrument carries out test analysis, and the result shows that this material contains the comparatively complete class graphite microcrystal of 7% growth, and crystallite size is in 2 ~ 10nm scope, and interlamellar spacing is 0.372nm, and its BET specific area is 278m
2/ g, pore volume is 0.13cm
3/ g.With the 0.5g sample, 0.059g conductive black (Carbon VXC 72) and 0.029g binding agent (polyvinylidene fluoride PVDF) are mixed, size mixing, and film, and the preparation carbon resistance rod is with 1mol/dm
3Et
4NBF
4The acetonitrile mixed solution be electrolyte, assembling coin shape simulation double electric layer capacitor.The LAND CT 2001A type cell tester that adopts Wuhan Jin Nuo Electrosource, Inc. to produce, constant current charge-discharge characteristic and the withstand voltage properties of study sample.The test voltage scope is 0 ~ 2.7V, 0 ~ 3.5V, 0 ~ 3.7V and 0 ~ 4.0V, and current density is 100mA/g.Record the carbon electrode material proof voltage up to 4.0V, and the energy density of capacitor is 26.3wh/kg.
The present embodiment difference from Example 1 is: change the quality 15g of KOH into 7.5g.Finally make charcoal base ion intercalation energy storage carbon electrode material quality and become 6.6g by 6.4g.
Charcoal base ion intercalation energy storage carbon electrode material obtained above adopts Tecnai G2 F20 type transmission electron microscope, D/MAX2500V/PC type X-ray diffractometer and TriStar3000 type N
2Adsorption instrument carries out test analysis, and the result shows that this material contains the comparatively complete class graphite microcrystal of 6% growth, and crystallite size is in 2 ~ 10nm scope, and interlamellar spacing is 0.368nm, and its BET specific area is 685m
2/ g, pore volume is 0.2cm
3/ g.With the 0.5g sample, 0.059g conductive black (Carbon VXC 72) and 0.029g binding agent (polyvinylidene fluoride PVDF) are mixed, size mixing, and film, and the preparation carbon resistance rod is with 1mol/dm
3Et
4NBF
4The acetonitrile mixed solution be electrolyte, assembling coin shape simulation double electric layer capacitor.The LAND CT 2001A type cell tester that adopts Wuhan Jin Nuo Electrosource, Inc. to produce, constant current charge-discharge characteristic and the withstand voltage properties of study sample.The test voltage scope is 0 ~ 2.7V, 0 ~ 3.5V, 0 ~ 3.7V and 0 ~ 4.0V, and current density is 100mA/g.Record the carbon electrode material proof voltage up to 4.0V, and the energy density of capacitor is 27.4wh/kg.
Embodiment 5
275g coal tar asphalt (softening point is 88 ℃) is added in the reactor, with 1m
3The speed of/h passes into nitrogen, continue to stir down, is warming up to 360 ℃ with 10 ℃/min of heating rate, carries out thermal polycondensation reaction 6h, and stopped heating naturally cools to room temperature, obtains the 148g softening point and be pitch after 185 ℃ the polycondensation.Then asphalt powder after the 10g polycondensation is broken to 30 μ m, then adds tube furnace with 1m
3The speed of/h passes into nitrogen, and the heating rate of 5 ℃/min is warming up to 900 ℃, and charing 1h naturally cools to room temperature.Obtained 8g charing sample is mixed with 16gKOH.In nitrogen atmosphere, be warming up to 800 ℃ with 15 ℃/min heating rate, activation 2h, naturally cool to room temperature, with 500ml 1MHCl solution boiling washing 3h, after being neutrality with 100ml deionized water cyclic washing to cleaning solution again, 120 ℃ of lower dry processing, obtain 7g charcoal base ion intercalation energy storage carbon electrode material.
Charcoal base ion intercalation energy storage carbon electrode material obtained above adopts Tecnai G2 F20 type transmission electron microscope, D/MAX2500V/PC type X-ray diffractometer and TriStar3000 type N
2Adsorption instrument carries out test analysis, and the result shows that this material contains the comparatively complete class graphite microcrystal of 8% growth, and crystallite size is in 2 ~ 10nm scope, and interlamellar spacing is 0.375nm, and its BET specific area is 775m
2/ g, pore volume is 0.29cm
3/ g.With the 0.5g sample, 0.059g conductive black (Carbon VXC 72) and 0.029g binding agent (polyvinylidene fluoride PVDF) are mixed, size mixing, and film, and the preparation carbon resistance rod is with 1mol/dm
3Et
4NBF
4The acetonitrile mixed solution be electrolyte, assembling coin shape simulation double electric layer capacitor.The LAND CT 2001A type cell tester that adopts Wuhan Jin Nuo Electrosource, Inc. to produce, constant current charge-discharge characteristic and the withstand voltage properties of study sample.The test voltage scope is 0 ~ 2.7V, 0 ~ 3.5V, 0 ~ 3.7V and 0 ~ 4.0V, and current density is 100mA/g.Record the carbon electrode material proof voltage up to 4.0V, and the energy density of capacitor is 28.7wh/kg.
Embodiment 6
300g ethylene bottom oil pitch (softening point is 146 ℃) is added in the reactor, with 1m
3The speed of/h passes into nitrogen, continue to stir down, is warming up to 320 ℃ with 10 ℃/min of heating rate, carries out thermal polycondensation reaction 4h, and stopped heating naturally cools to room temperature naturally, obtains the 165g softening point and be pitch after 220 ℃ the polycondensation.Then asphalt powder after the 10g polycondensation is broken to 30 μ m, then adds tube furnace with 0.5m
3The speed of/h passes into nitrogen, and the heating rate of 5 ℃/min is warming up to 600 ℃, and charing 1h naturally cools to room temperature.Obtained 7.5g charing sample is mixed with 15gKOH.In nitrogen atmosphere, be warming up to 800 ℃ with 10 ℃/min heating rate, activation 2h, naturally cool to room temperature, with 500ml 1MHCl solution boiling washing 3h, after being neutrality with 100ml deionized water cyclic washing 3 times to cleaning solution again, 120 ℃ of lower dry processing, obtain 6.7g charcoal base ion intercalation energy storage carbon electrode material.
Charcoal base ion intercalation energy storage carbon electrode material obtained above adopts Tecnai G2 F20 type transmission electron microscope, D/MAX2500V/PC type X-ray diffractometer and TriStar3000 type N
2Adsorption instrument carries out test analysis, and the result shows that this material contains the comparatively complete class graphite microcrystal of 10% growth, and crystallite size is in 2 ~ 10nm scope, and interlamellar spacing is 0.382nm, and its BET specific area is 500m
2/ g, pore volume is 0.18cm
3/ g.With the 0.5g sample, 0.059g conductive black (Carbon VXC 72) and 0.029g binding agent (polyvinylidene fluoride PVDF) are mixed, size mixing, and film, and the preparation carbon resistance rod is with 1mol/dm
3Et
4NBF
4The acetonitrile mixed solution be electrolyte, assembling coin shape simulation double electric layer capacitor.The LAND CT 2001A type cell tester that adopts Wuhan Jin Nuo Electrosource, Inc. to produce, constant current charge-discharge characteristic and the withstand voltage properties of study sample.The test voltage scope is 0 ~ 2.7V, 0 ~ 3.5V, 0 ~ 3.7V and 0 ~ 4.0V, and current density is 100mA/g.Record the carbon electrode material proof voltage up to 4.0V, and the energy density of capacitor is 29.9wh/kg.
Claims (2)
1. charcoal base ion intercalation energy storage electrode material, this material is average grain diameter 20 ~ 50 μ m, its specific area is 278 ~ 1048m
2/ g, pore volume is 0.12 ~ 0.5cm
3/ g is characterized in that, this material is comprised of orderly class graphite microcrystal and unordered disorderly layer carbon structure, and wherein orderly class graphite microcrystal is 5% ~ 10% of Carbon Materials structure, and crystallite size is 2 ~ 10nm, and the interlamellar spacing of crystallite is 0.359～0.385nm; Be typical unordered disorderly layer carbon structure around the crystallite.
2. press charcoal base ion intercalation energy storage electrode material preparation method claimed in claim 1 for one kind, it is characterized in that comprising following process:
1) coal tar asphalt or ethylene bottom oil pitch are added in the reactor, with 0.5 ~ 1.2m
3The speed of/h passes into nitrogen, continue to stir down, is warming up to 320 ~ 400 ℃ with 1 ~ 10 ℃/min of heating rate, carries out thermal polycondensation reaction 2 ~ 6h, and the softening point that obtains after the polycondensation is 150 ~ 220 ℃ of pitches;
2) step 1) being obtained pitch after the polycondensation pulverizes 20 ~ 50 μ m powder and adds in the retort, with 0.5 ~ 1.2m
3The speed of/h passes into nitrogen in retort, be warming up to 600 ~ 900 ℃ with the heating rate of 5 ~ 20 ℃/min, and constant temperature charing 0.5 ~ 4h naturally cools to room temperature, obtains the asphalt powder after the charing;
3) with step 2) asphalt powder after the charing that obtains and KOH 1:((0.5 ~ 2 in mass ratio), add in the retort and in nitrogen atmosphere, be warming up to 600 ~ 900 ℃ with 5 ~ 20 ℃/min heating rate, priming reaction 0.5 ~ 2h, naturally cool to room temperature, with 1M HCl solution boiling washing 3 ~ 5h, after being neutrality with deionized water cyclic washing to cleaning solution again, 80 ~ 120 ℃ of lower dry processing of temperature, obtain charcoal base ion intercalation energy storage electrode material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113327776A (en) * | 2021-05-31 | 2021-08-31 | 青岛科技大学 | KOH intercalated MXene/CNFs composite electrode material and preparation method thereof |
| CN116453877A (en) * | 2023-06-06 | 2023-07-18 | 深圳市智越盛电子科技有限公司 | Super capacitor electrode material and preparation method thereof |
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| JP2005235918A (en) * | 2004-02-18 | 2005-09-02 | Cataler Corp | Electric double-layer capacitor and carbon material therefor |
| CN101295587A (en) * | 2008-06-05 | 2008-10-29 | 华东理工大学 | Production method of high specific energy super capacitor carbonaceous electrode material |
| CN102336402A (en) * | 2005-09-30 | 2012-02-01 | 株式会社科特拉 | Carbon material for electric double layer capacitor and electric double layer capacitor |
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| JPH11317333A (en) * | 1998-03-03 | 1999-11-16 | Jeol Ltd | Carbon material for electric double-layer capacitor and manufacture of the same, and electric double-layer capacitor and manufacture of the same |
| JP2005235918A (en) * | 2004-02-18 | 2005-09-02 | Cataler Corp | Electric double-layer capacitor and carbon material therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113327776A (en) * | 2021-05-31 | 2021-08-31 | 青岛科技大学 | KOH intercalated MXene/CNFs composite electrode material and preparation method thereof |
| CN116453877A (en) * | 2023-06-06 | 2023-07-18 | 深圳市智越盛电子科技有限公司 | Super capacitor electrode material and preparation method thereof |
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Application publication date: 20130403 |