CN103979529A - Preparation method of porous carbon material and application of porous carbon material as electrode material - Google Patents
Preparation method of porous carbon material and application of porous carbon material as electrode material Download PDFInfo
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- CN103979529A CN103979529A CN201410244910.4A CN201410244910A CN103979529A CN 103979529 A CN103979529 A CN 103979529A CN 201410244910 A CN201410244910 A CN 201410244910A CN 103979529 A CN103979529 A CN 103979529A
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Abstract
The invention relates to a porous carbon material used in a cathode of a lithium ion battery, and a preparation method of the porous carbon material. The slit-type porous carbon material which mainly comprises micropores and mesopores is prepared by mixing layered plate-shaped magnesium-aluminum hydrotalcite used as a template with a carbon source, curing, carbonizing and performing acidification treatment. The preparation process is simple, the cost is low, and the specific surface area is adjustable. The slit-type porous carbon provided by the invention has good electrochemical properties when being used as a lithium ion electrode material.
Description
Technical field
The present invention relates to a kind of porous carbon material, preparation method and the application aspect lithium ion battery, belong to electrochemistry and new energy materials field.
Background technology
Lithium ion battery is than traditional lead-acid cell and nickel-cadmium cell, have that output voltage is high, energy density is high, safety performance is good, have extended cycle life, can fast charging and discharging and operating temperature range is wide, pollution-free and the advantage [lithium ion battery-application and practice/Wu Yu equality is write .-Beijing: Chemical Industry Press, 2004.3] such as memory-less effect.Lithium ion battery has been widely used in the small type mobile devices such as mobile phone, notebook computer, in recent years just actively to the development of Large-scale Mobile apparatus field, such as electromobile, mixed motivity type automobile and standing type standby power supply (UPS) etc.This has higher requirement to performances such as the energy density of power lithium-ion battery and power densities, and the negative material that research and development synthesize a kind of height ratio capacity is the key that improves lithium ion battery energy density.Carbon Materials has good electroconductibility, thermal conductivity and thermostability, is the focus of ion cathode material lithium area research always.Graphite is because of its good cycle performance and abundant reserves, by extensively should be as business-like lithium ion battery negative material, but because theory storage lithium specific storage is only 372mAh/g, have greatly limited its application on power lithium-ion battery.In order to replace graphite material, people start to explore the Carbon Materials of other form, as matrix material of Graphene, carbon nanotube, carbon fiber, porous carbon material and metal and metal oxide and charcoal etc.Wherein, porous carbon material can provide more hyperchannel for lithium ion transmission owing to having special pore passage structure, be conducive to improve the rate of migration of lithium ion, thereby give the high rate performance that material is good, therefore the research of porous charcoal negative material is in recent years subject to extensive concern.
The preparation method that porous carbon material is conventional mainly comprises catalytic activation method, organogel charring and template etc., and template is the most effective preparation method of regulation and control porous carbon material pore structure type, pore distribution.Song etc. [R. Song, et al. J. Mater. Chem., 2012,22,12369.] utilize linear phenolic resin for carbon matrix precursor, Cu (NO
3)
2for source metal, the copper nano particles that the original position of take forms has been prepared the porous carbon material with hierarchical porous structure as template, the nano-lamellar structure that this material is special and a large amount of middle macropore have shortened the migration distance of lithium ion effectively, its a large amount of micropores provide sufficient storage lithium position, as lithium cell negative pole, show height ratio capacity and good cyclical stability.Yang etc. [J. Yang, et al. Electrochim. Acta, 2011,56,8576.] utilize sucrose for carbon matrix precursor, SiO
2colloidal sol is as the synthetic porous carbon material of template, and its aperture is concentrated and is distributed in 10 nm left and right, and BET specific surface area is 420 m
2/ g, reversible charge/discharge capacity is 407.4 mAh/g.When utilizing the synthesizing porous Carbon Materials of template, template is the principal element of control punch structure, and therefore selecting suitable template is to control the key of porous carbon material pore structure.
Hydrotalcite (layered double hydroxide, LDH) is a kind of natural stratiform bimetallic oxide, is used to the various fields [Q. Wang, et al. Chem. Rev., 2012,112,4124.] such as petroleum industry, sewage disposal, catalyzer.LDHs lateral dimension is generally between tens nanometers are to several microns, individual layer laminate thickness is approximately 0.48nm [T. Hibino, et al. J. Mater. Chem., 2005,15,653.] [Z. Liu, et al. J. Am. Chem. Soc., 2006,128,4872.], its regular laminated structure makes it both can be used as the model system of research physical attribute, also can be used as the nano-complex that base mateiral and polyoxometallate, polymkeric substance and biomolecules assemble to build difference in functionality.In addition, by peeling off LDHs, can reduce its lamellar spacing, can be made into Multilayer ultrathin composite film material with polymkeric substance, such as [R. Ma, et al. J. Mater. Chem., 2006,16,3809.] such as Ma, by self-assembly layer by layer, prepare and peeled off Mg-Al-NO
3lDH/ anionic polymer (sodium polystyrene sulfonate) multi-layer ultrathin membrane.Based on this, can select magnesium aluminum-hydrotalcite (Mg
6al
2(OH)
16cO
34H
2o), as template, from the compound porous carbon material with special pore structure of preparing of different organism carbon sources, by regulating lateral dimension and the lamellar spacing of LDHs, thereby controllably regulate aperture and the pass of carbon matrix.
Summary of the invention
The object of the invention is for fear of the existing weak point of above-mentioned prior art, provide that a kind of technique is simple, lower-cost porous carbon material and preparation method thereof, take polymkeric substance as carbon source, make pore-creating template with laminate shape magnesium aluminum-hydrotalcite, through charing and acidification, obtain the porous carbon material in slit-type hole.When the porous carbon material that the method makes is used as lithium ion battery negative material, show high specific storage and excellent high rate performance.
The invention provides a kind of porous charcoal that laminate shape magnesium aluminum-hydrotalcite prepared as template of take, its pore texture is slit-shaped, take micropore and mesopore as main, and specific surface area is 150-1000 m
2/ g.The present invention also provides a kind of preparation method of this porous carbon material, comprises the steps:
Step 1: template, carbon source and solidifying agent are dissolved in respectively in solvent, then three are evenly mixed.
Step 2: treat that solvent evaporates is complete, mixture is placed in to vacuum drying oven in 100-180 ℃ of curing 3-6 hour.Then cured product is placed in to charring furnace, under inert atmosphere protection, in 400-1000 ℃ of charing 2-10 hour, obtains embedding the carbon composite of sheet template.
Step 3: carbonizing production is removed to metal oxide wherein with excess acid or alkaline purification.Through repeatedly centrifugal, clean, dry after, obtain porous carbon material.
Preferably, in step 1, selected carbon source comprises resol, urea-formaldehyde resin, furfuryl resin, pitch or sucrose etc.
Preferably, in step 1, selected solvent comprises dehydrated alcohol, acetone, ether or pyridine.
Preferably, in step 1, selected solidifying agent is that this area is conventional, as hexamethylenetetramine etc.
When preferably, template described in step 1 is mixed with carbon source, the mass ratio of hydrotalcite and carbon source is (1:1)-(4:1).
The charing that step 2 relates to is treated to universal process prepared by Carbon Materials, and under protection of inert gas, (as nitrogen, argon gas etc.) are warming up to outlet temperature with certain temperature rise rate, and stops certain hour in this temperature.
The porous charcoal pore texture the present invention relates to is slit-shaped, take micropore and mesopore as main, and specific surface area is 150-1000 m
2/ g.Its mesopore is mainly derived from the occupy-place of the sheet oxide compound forming after magnesium aluminum-hydrotalcite decomposes, and after removal template, forms corresponding slit-shaped apertures in carbon matrix.Because template particle size is little, micropore and mesopore mainly be take as main in the hole of formation.Its special pore structure not only can provide a large amount of storage lithium positions, also be conducive to increase effective contact area of electrode materials and electrolytic solution simultaneously, shorten ion the evolving path, improve transmission efficiency, be suitable for as lithium ion battery negative material and electrode material for super capacitor.
The present invention adopts the test of carrying out with the following method associated electrical chemical property: the ratio by this porous carbon material, conductive agent acetylene black and binding agent polyvinylidene difluoride (PVDF) with mass ratio 8:1:1 mixes, drip N-Methyl pyrrolidone, fully grind to form uniform paste, be coated in nickel foam, made the button cell that model is CR2032.
The porous charcoal the present invention relates to, as lithium ion battery negative material, is under 50 mA/g in current density, and reversible capacity is 450-1000 mAh/g first, circulate after 50 times, and the stable 340-806 mAh/g that remains on of capacity.Under high current charge-discharge mechanism, when current density is 200 mA/g, reversible capacity is 390-670 mAh/g; When current density is increased to 1 A/g, the reversible capacity after 20 times that circulates remains on 200-290 mAh/g.The graphite negative electrodes material no matter reversible capacity or high-rate performance are all used higher than industrialization at present, shows good actual application value.
These results show, the porous carbon material that the preparation method that the present invention relates to of usining prepares is as electrode materials, and storage lithium performance and high rate performance are superior, and the method technological process is simple, cost is lower, environmental friendliness, are easy to realize technical scale preparation.
accompanying drawing explanation:
Fig. 1-4 are the embodiment of the present invention 1 hydrotalcite and resol mass ratio is 3:1, through 600 ℃ of charings, remove the test data of the porous carbon material that template obtains after 6 hours.
Fig. 1 is scanning electron microscope (SEM) photo of porous charcoal in the embodiment of the present invention 1;
Fig. 2 is the N of porous charcoal in the embodiment of the present invention 1
2isothermal adsorption curve;
Fig. 3 is cycle charge discharge electrograph under 50 mA/g current densities during as lithium ion battery negative;
Fig. 4 is cycle charge discharge electrograph under 50 mA/g-1 A/g current densities during as lithium ion battery negative.
embodiment:
Mode with embodiment illustrates the present invention below, but is not construed as limiting the invention.
embodiment 1
By resol 1g and magnesium aluminum-hydrotalcite 3g, and solidifying agent hexamethylenetetramine 0.35g, be dissolved in respectively dehydrated alcohol, to be dissolvedly mix after completely, naturally stir until ethanol volatilization is complete.Mixture is placed at 150 ℃ of vacuum drying ovens and is solidified 4 hours, afterwards cured product is placed in to charring furnace, under nitrogen protection, be warming up to 600 ℃ of charings 6 hours.By carbonizing production, successively with excessive hydrochloric acid and KOH solution-treated, more centrifugal, deionized water is washed till neutrality, dry, obtains target product porous carbon material.
As shown in Figure 1, this porous carbon material is loose block, and its pore texture is slit-shaped.Its isothermal nitrogen adsorption curve presents obvious hysteresis loop, has illustrated that a large amount of mesopores form (Fig. 2).Total specific surface area of this porous carbon material is 887 m
2/ g, wherein micropore specific area 327 m
2/ g, outer pore specific surface area is 560 m
2/ g.
For investigating reversible capacity, cycle performance, the high rate performance of this material, battery is carried out to constant current charge-discharge test analysis.Test condition is: current density 50 mA/g and 0.1 ~ 1 A/g, and voltage range 0.01-3V, cycle index is respectively 50 times and 20 times.
As shown in Figure 3, Figure 4, as lithium ion battery negative material, in current density, be under 50 mA/g, reversible capacity is 877 mAh/g first, circulate after 50 times, stable 759 mAh/g that remain on of capacity.Under high current charge-discharge mechanism, during current density 200 mA/g, reversible capacity, up to 633 mAh/g, circulates and is stabilized in 587 mAh/g 20 times; When current density is increased to 500 mA/g, reversible capacity remains on 451 mAh/g; During 1 A/g, reversible capacity is still up to 282 mAh/g.
embodiment 2
Operational condition is with embodiment 1, and difference is to change hydrotalcite quality into 1g, and carbonization condition is 800 ℃ of insulations 6 hours.
Gained porous carbon material specific surface area 503 m
2/ g.Adopt the method identical with embodiment 1 to carry out electro-chemical test, result shows, current density is that under 50 mA/g, reversible capacity reaches 652 mAh/g, circulates after 50 times, and capacity can remain on 503 mAh/g.Under large electric current, when current density is 1 A/g, reversible capacity is 214 mAh/g.
embodiment 3
Operational condition is with embodiment 1, and difference is to change resol into sucrose, and carbonization temperature used is 600 ℃ of insulations 2 hours.
Gained porous charcoal specific surface area is 780 m
2/ g.Adopt the method identical with embodiment 1 to carry out electro-chemical test, result shows, current density is that under 50 mA/g, reversible capacity reaches 884 mAh/g, circulates after 50 times, and capacity can remain on 690 mAh/g.Under large electric current, when current density is 200 mA/g, reversible capacity is 513 mAh/g, and during 1A/g, reversible capacity is 285 mAh/g.
embodiment 4
Operational condition is with embodiment 1, and difference is to change resol into mesophase pitch, and hydrotalcite consumption is 2g.
Gained porous charcoal specific surface area 156 m
2/ g.Adopt the method identical with embodiment 1 to carry out electro-chemical test, result shows, current density is that under 50 mA/g, reversible capacity reaches 458 mAh/g, circulates after 50 times, and capacity can remain on 349 mAh/g.Under large electric current, when current density is 200 mA/g, reversible capacity is 394 mAh/g first, and during 1A/g, reversible capacity is 276 mAh/g.
Claims (5)
1. the porous charcoal that the laminate shape magnesium aluminum-hydrotalcite of take is prepared as template, its pore texture is slit-shaped, take micropore and mesopore as main, specific surface area is 150-1000 m
2/ g.
2. a preparation method for porous carbon material described in claim 1, comprises following step:
(1) template, carbon source for being dispersed in solvent, the ratio of (1:1)-(4:1) are mixed after (part carbon source need be added solidifying agent) in mass ratio, the dry solvent of removing, gained solid is cured at 100-180 ℃, afterwards by cured product under inert atmosphere protection, 2-10 hour is processed in 400-1000 ℃ of charing;
(2) by excessive mineral acid or alkali immersion treatment for carbonizing production, remove the metal oxide that template forms, then through repeatedly centrifugal, clean to neutral, obtain slit-type hole porous charcoal after dry.
3. the preparation method of porous carbon material according to claim 2, is characterized in that: described carbon source is a kind of in resol, urea-formaldehyde resin, furfuryl resin, pitch or sucrose.
4. the preparation method of porous carbon material according to claim 2, is characterized in that: described solvent is selected from dehydrated alcohol, acetone, ether or pyridine.
5. the negative material for lithium ion battery, it is characterized in that: comprise porous carbon material claimed in claim 1 or the prepared porous carbon material of claim 2-4 any one, its reversible capacity during as lithium ion battery negative material is at 450-1000mAh/g.
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Cited By (10)
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| CN105826516A (en) * | 2016-03-29 | 2016-08-03 | 浙江吉利汽车研究院有限公司 | Lithium ion battery and negative pole piece thereof |
| CN106683910A (en) * | 2017-03-13 | 2017-05-17 | 黄冈师范学院 | Flaky carbonyl functionalized carbon material, preparation method thereof and application thereof in preparation of supercapacitor |
| CN106672966A (en) * | 2015-11-05 | 2017-05-17 | 长春工业大学 | Preparation method of ethylene tar-based porous carbon with narrow aperture distribution |
| CN106927445A (en) * | 2017-03-24 | 2017-07-07 | 武汉纺织大学 | A kind of method that utilization hydrotalcite prepares the carbide of lamellar structure |
| CN106992287A (en) * | 2017-03-24 | 2017-07-28 | 武汉纺织大学 | A kind of novel lamellar carbon electrode material and preparation method thereof |
| CN107068417A (en) * | 2017-03-13 | 2017-08-18 | 黄冈师范学院 | It is a kind of that there is multistage meso-hole structure graphene nanometer sheet and its preparation method and the application in ultracapacitor is prepared |
| CN108726500A (en) * | 2017-04-18 | 2018-11-02 | 中国科学院上海硅酸盐研究所 | A method of preparing porous carbon materials using bivalent metal ion soft template |
| CN109103453A (en) * | 2018-08-17 | 2018-12-28 | 东莞市凯金新能源科技股份有限公司 | A kind of preparation method and its material of the graphite cathode material of catalyzed graphitization |
| CN110473710A (en) * | 2018-05-10 | 2019-11-19 | 北京化工大学 | Porous carbon materials and its preparation method and application |
| CN114933294A (en) * | 2022-05-13 | 2022-08-23 | 西安交通大学 | High-volume-density multilayer compact porous carbon nanosheet and preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106672966A (en) * | 2015-11-05 | 2017-05-17 | 长春工业大学 | Preparation method of ethylene tar-based porous carbon with narrow aperture distribution |
| CN105826516A (en) * | 2016-03-29 | 2016-08-03 | 浙江吉利汽车研究院有限公司 | Lithium ion battery and negative pole piece thereof |
| CN105826516B (en) * | 2016-03-29 | 2019-04-09 | 浙江吉利汽车研究院有限公司 | A kind of lithium ion battery and its cathode pole piece |
| CN106683910A (en) * | 2017-03-13 | 2017-05-17 | 黄冈师范学院 | Flaky carbonyl functionalized carbon material, preparation method thereof and application thereof in preparation of supercapacitor |
| CN107068417A (en) * | 2017-03-13 | 2017-08-18 | 黄冈师范学院 | It is a kind of that there is multistage meso-hole structure graphene nanometer sheet and its preparation method and the application in ultracapacitor is prepared |
| CN106927445A (en) * | 2017-03-24 | 2017-07-07 | 武汉纺织大学 | A kind of method that utilization hydrotalcite prepares the carbide of lamellar structure |
| CN106992287A (en) * | 2017-03-24 | 2017-07-28 | 武汉纺织大学 | A kind of novel lamellar carbon electrode material and preparation method thereof |
| CN106992287B (en) * | 2017-03-24 | 2019-11-12 | 武汉纺织大学 | A kind of stratiform carbon electrode material and preparation method thereof |
| CN108726500A (en) * | 2017-04-18 | 2018-11-02 | 中国科学院上海硅酸盐研究所 | A method of preparing porous carbon materials using bivalent metal ion soft template |
| CN110473710A (en) * | 2018-05-10 | 2019-11-19 | 北京化工大学 | Porous carbon materials and its preparation method and application |
| CN109103453A (en) * | 2018-08-17 | 2018-12-28 | 东莞市凯金新能源科技股份有限公司 | A kind of preparation method and its material of the graphite cathode material of catalyzed graphitization |
| CN114933294A (en) * | 2022-05-13 | 2022-08-23 | 西安交通大学 | High-volume-density multilayer compact porous carbon nanosheet and preparation method and application thereof |
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Application publication date: 20140813 |