CN101697322B - Method for preparing porous carbon electrode material - Google Patents
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- CN101697322B CN101697322B CN2009100193484A CN200910019348A CN101697322B CN 101697322 B CN101697322 B CN 101697322B CN 2009100193484 A CN2009100193484 A CN 2009100193484A CN 200910019348 A CN200910019348 A CN 200910019348A CN 101697322 B CN101697322 B CN 101697322B
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Abstract
The invention belongs to the technical field of carbon material preparations, which relates to a method for preparing a porous carbon electrode material with large capacitance by using peanuts shells as a raw material. The electrode material prepared by the method is used for preparing a super capacitor and a lithium ion battery. The method comprises the steps of porous carbon preparation, porouscarbon electrode preparation, porous carbon electrode testing, charging and discharging performances of a battery testing and the like. In the method, the peanut shells are washed and dried; the peanut shells are cut into pieces; the pieces are placed into an alkaline solution for soaking; the soaked pieces are placed into a resistance furnace for carbonization; and hydrofluoric acid treatment isperformed to prepare the porous carbon and the porous carbon is ground into powder serving as a material for preparing the porous carbon electrode, wherein the superficial area of the prepared porouscarbon material is large and mostly porous; when the porous carbon electrode is prepared by using the porous carbon material, the porous carbon electrode has the advantages that the capacitance can reach a high capacitance about 400 F/g when the current intensity is 1A/g, the capacitance loss rate is small after charging and discharging repeatedly at a large current intensity, the raw material isobtained, the preparing process is simple, the porous effect is good, the prepared porous carbon electrode material performance is strong and the like.
Description
Technical field:
The invention belongs to the material with carbon element preparing technical field, relating to a kind of is the method for the porous carbon electrode material of the big electric capacity of feedstock production with the peanut shell, and electrode material is used for the preparation of ultracapacitor and lithium ion battery.
Background technology:
In recent years, high performance electrical energy storage device requires the application in harsh many fields to cause concern widely at hybrid vehicle and stand-by power supply etc. to chemical power source.Because the usefulness of traditional capacitor is lower, can not be at the enough energy of limited volume and weight stored, thereby the research of ultracapacitor has caused worldwide research interest.Ultracapacitor (supercapacitor) claims electrochemical capacitor (electrochemicalcapacitor) again, is a kind of novel energy-storage travelling wave tube, comprises two kinds in double electric layer capacitor and fake capacitance capacitor.Because of it has both the high and high advantage of secondary cell energy density of traditional capacitor power density, and can realize transient large current discharge, very unique character such as the charging interval is short, efficient is high, long service life, memory-less effect and basic Maintenance free and receiving much attention, particularly have broad application prospects and be subjected to extensive studies at aspects such as information technology, electric automobile, space flight and aviation and science and techniques of defence.At present, porous carbonaceous electrode material is to carry out one of the most frequently used electrode material of double electric layer capacitor research, though the active carbon specific area greatly still mostly is the turnover that micropore is unfavorable for the ion that atomic radius is big, thereby limited the electric capacity of active carbon electrode material, in general the electric capacity of activated carbon electrodes can not surpass 45F/g in the aqueous electrolyte; Orderly mesoporous material can increase the electric capacity of double electric layer capacitor, can utilize mesoporous silicon to be the template for preparing mesoporous carbon, but this method technology is too complicated, the electrode material difficult quality guarantee of preparation.Rising in recent years utilize biomaterial directly to prepare porous carbon, B é guin etc. utilizes sodium alginate to prepare the porous carbon materials that electric capacity can reach 200F/g under 600 ℃, people such as Yong-Jung Kim utilize bamboo to prepare the porous carbon materials that electric capacity is lower than 70F/g at 800 ℃ after naoh treatment, utilize the capacitance of these porous carbon materials preparations not high, be difficult to satisfy the requirement of modern electrode material and electric power development.At present; nearly 1,450 ten thousand tons of China's peanut annual productions; account for 42% of Gross World Product; produce 4,500,000 tons of peanut shells every year approximately; these Organic Ingredients are except that small part is used as feed; overwhelming majority peanut shells are taken as fuel and burn, and not only cause environmental pollution but also form the wasting of resources, and therefore research is made the feedstock production porous carbon electrode material with peanut shell and had environmental protection and the double-deck meaning of economic benefit.
Summary of the invention:
The objective of the invention is to overcome the shortcoming that prior art exists, seek to provide a kind of process of utilizing organic carbonization peanut shell to prepare the porous carbon electrode material of high-ratio surface, big electric capacity, electric capacity good cycling stability.
To achieve these goals, the present invention is that base-material prepares porous carbon materials and comprises steps such as porous carbon preparation, porous carbon electrodes preparation, porous carbon electrodes test and battery charging and discharging performance test with the Organic Ingredients peanut shell, and the specific area of the porous carbon materials that obtains is big and mostly be micropore; When the porous carbon materials that adopts peanut shell to prepare prepares porous carbon electrodes, the porous carbon electrodes that obtains has when current density is 1A/g electric capacity and can obtain the high capacitance of nearly 400F/g and discharge and recharge repeatedly the loss late of back electric capacity under high current density very little, and its concrete preparation process may further comprise the steps:
(1). the porous carbon preparation
Earlier that the peanut shell clean dry is standby; The dry good peanut shell of part is cut into small pieces, the potassium hydroxide aqueous slkali of putting into concentration and be 1mol/L soaks down for 80 ℃ and carried out preliminary treatment, clean dry then in 12 hours again; The peanut shell that to handle through alkali lye and put into 800 ℃ of following carbonizations of tube type resistance furnace nitrogen atmosphere 90 minutes respectively without the peanut shell that alkali lye is handled, gained sample are that 20% hydrofluoric acid dips was made porous carbon after 72 hours through mass percent concentration; The porous carbon of preliminary treatment peanut shell preparation is designated as C-1, and the porous carbon for preparing without the preliminary treatment peanut shell is designated as C-2.
(2). the preparation of porous carbon electrodes
Selecting aqueous electrolyte concentration for use is potassium hydroxide (KOH) solution of 6mol/L; Mass percent is that 60% polytetrafluoroethylene (PTFE) emulsion is a binding agent; It is the bulk of 1 * 1cm size that nickel foam is cut out; With prepared porous carbon sample C-1 and C-2 grind into powder respectively, by porous carbon: electrically conductive graphite: the PTFE emulsion is to mix formation viscosity mud shape thing after 0.85: 0.1: 0.05 mass ratio takes by weighing; Viscosity mud shape thing is transferred on the aluminium foil, be pressed into plate object and transfer on the dry load weighted foam nickel block uniform spreading after the sheet and open, weighing after 110 ℃ of following vacuumize then, be the good nickel foam bag of drying sandwich-like with aluminium foil again, suppressed 3 minutes under 12.5MP pressure with hydraulic press, obtain electrode slice, porous carbon sample C-1 and the prepared electrode slice of C-2 are designated as EC-1 and EC-2 respectively; So that calculate the quality of active material on the nickel foam, then EC-1 and EC-2 were soaked after 12-24 hour standby in aqueous electrolyte the electrode slice weighing that suppresses.
(3). the test of porous carbon electrodes
Choosing three-electrode system is respectively:
The self-control porous carbon electrodes is a work electrode; The Ag/AgCl electrode is a reference electrode; Platinized platinum is to electrode; The KOH electrolyte of measuring 8ml joins in the electrolytic cell, three-electrode system installed the logical nitrogen in back 30 minutes, remove the oxygen in the solution, test its cyclic voltammetry curve figure and constant current charge-discharge curve chart respectively, and the capacity-cycle-index curve that under the 2A/g current density, discharges and recharges 500 gained.
(4). the test of simulation lithium ion battery charge-discharge performance
The porous carbon, acetylene black, the Kynoar (PVDF) that obtain after the processing of potassium hydroxide alkali lye are assembled lithium ion battery by 0.85: 0.5: 0.1 mass ratio, be designated as LC-1, simulated battery after the assembling is carried out charge-discharge test, test condition is: at room temperature, discharge and recharge between the 0.005V from open circuit voltage with the 0.2A constant current, find that discharge capacity is approximately 245mAh/g first, discharge capacity decays to 45mAh/g for the second time.
The present invention compares with prior art and material has following advantage: the one, and selecting peanut shell for use is raw material cheapness and wide material sources; The 2nd, the part peanut shell carried out the porous carbon of gained has obvious quality characteristic and advantage after the preliminary treatment; The 3rd, test result shows that prepared porous carbon electrodes electric capacity is big, good cycling stability; The 4th, the gained porous carbon materials can be used as the high-quality electrode material of assembling lithium ion battery.
Description of drawings:
Fig. 1 for the present invention through the alkali lye preliminary treatment with without the infrared figure of pretreated peanut shell.
The adsorption isotherm of the porous carbon C-1 that Fig. 2 makes for the present invention.
The graph of pore diameter distribution of the porous carbon C-1 that Fig. 3 makes for the present invention.
The cyclic voltammetry curve figure of the EC-1 that Fig. 4 makes for the present invention.
The cyclic voltammetry curve figure of the EC-2 that Fig. 5 makes for the present invention.
The charge-discharge test figure of the EC-1 that Fig. 6 makes for the present invention.
Fig. 7 is the charge-discharge test figure of the EC-2 of system of the present invention.
Capacity-cycle-index curve chart of the EC-1 that Fig. 8 makes for the present invention.
The charging and discharging curve figure of the LC-1 that Fig. 9 makes for the present invention.
Embodiment:
Also be described further in conjunction with the accompanying drawings below by embodiment.
Embodiment:
1. porous carbon preparation: it is base stock that present embodiment is selected common dry peanut shell for use, earlier that the peanut shell clean dry is standby; The dry good peanut shell of part is cut into small pieces, and the aqueous slkali of putting into 1mol/L soaks 12h down for 80 ℃ and carries out preliminary treatment, then clean dry; To handle peanut shell and put into 800 ℃ of 90min of tube type resistance furnace carbonization (nitrogen atmosphere) respectively without alkali lye processing peanut shell through alkali lye, the gained sample be made porous carbon after the HF of 20% concentration acid soak is handled 72h; Get the gained sample test, the porous carbon of preliminary treatment peanut shell preparation is designated as C-1, and the porous carbon for preparing without the preliminary treatment peanut shell is designated as C-2; Fig. 1 is the infrared figure of C-1 and C-2, pass through the alkali lye preliminary treatment as seen from Figure 1 after, materials such as the colloid in the peanut shell are removed; Fig. 2 and Fig. 3 are respectively adsorption/desorption curve chart and the graph of pore diameter distribution of C-1, can find out that by two figure the C-1 sample well mostly is micropore greatly, and the aperture mostly is 0.8nm greatly; Following table 1 is the pore structure parameter of C-1 and C-2.
Table 1:
aThe BET specific area,
bAverage pore volume,
cAverage pore size
2. the preparation of porous carbon electrodes: select the water system electrolyte solution for use, 6mol/L KOH solution; Commercially available 60% PTFE emulsion is a binding agent; It is the size of 1 * 1cm that nickel foam is cut out; With prepared porous carbon sample C-1 and C-2 grind into powder respectively, porous carbon: electrically conductive graphite: PTFE is that 0.85: 0.1: 0.05 ratio takes by weighing with mass ratio, mixes the mud shape thing that forms viscosity after weighing; The sticking mud shape matter sample for preparing is transferred on the aluminium foil, be pressed into sheet with sample vial, sheet sample is transferred on the dry load weighted nickel foam, uniform spreading is opened on nickel foam, then 110 ℃ of following vacuumizes; Dry intact back weighing after weighing is intact, is the good nickel foam bag of drying a sandwich-like with aluminium foil, presses down 3min with hydraulic press at 12.5MP pressure; The electrode that obtains pressing, the prepared electrode slice of porous carbon sample C-1 and C-2 is designated as EC-1 and EC-2 respectively; The electrode weighing that presses so that calculate the quality that foam is pinched active material, is steeped 12-24h in the electrolyte solution with EC-1 and EC-2 then.
3. the test of porous carbon electrodes: utilize three-electrode system; Work electrode is the self-control porous carbon electrodes; Reference electrode is the Ag/AgCl electrode; To electrode is platinized platinum; The KOH electrolyte solution of measuring about 8ml joins in the electrolytic cell, and three-electrode system installs, and logical then nitrogen 30min removes the oxygen in the solution; Fig. 4 and Fig. 5 are respectively EC-1 and EC-2 cyclic voltammetry curve figure, and figure is near rectangle, and negative electrode and anodic process be symmetry substantially, shows that electrode has capacitive property preferably; Fig. 6 and Fig. 7 are respectively the constant current charge-discharge curve chart of EC-1 and EC-2; The electric capacity computing formula:
In the formula: I---constant current value, A
t
d---charge/discharge time, s
M---the quality of active material on the electrode slice, g
Δ v---charge/discharge voltage rising/reduction mean value
Table 2: for utilizing EC-1 that this formula calculates by Fig. 6 and Fig. 7 and the capacitance of EC-2
Fig. 8 is for discharging and recharging EC-1 the capacity-cycle-index curve of 500 gained under the 2A/g current density, the initial capacitance of EC-1 under the 2A/g current density is 207F/g, under the high current density of 2A/g the circulation 500 times after the capacitance loss rate be 4% only, show that EC-1 has good cyclical stability.
4. simulation lithium ion battery charge-discharge performance test: the mass ratio of choosing the porous carbon sample that obtains after alkali lye is handled and acetylene black, PVDF is that 0.85: 0.5: 0.1 ratio is assembled lithium ion battery, be designated as LC-1, the charge-discharge test of the simulated battery after the assembling is to carry out on the emerging battery test system PB-110 of Wuhan power, test condition is: at room temperature, discharge and recharge between the 0.005V from open circuit voltage with the 0.2A constant current; Find that discharge capacity is approximately 245mAh/g first, capacity attenuation is 45mAh/g for the second time; Can find out also that by Fig. 9 discharge capacity decay for the second time is bigger; Because the simplicity of the cheapness of peanut shell and preparation porous carbon can be used as C-1 the primary cell material.
Claims (1)
1. the preparation method of a porous carbon electrode material is characterized in that the porous carbon preparation is earlier that the peanut shell clean dry is standby; The dry good peanut shell of part is cut into small pieces, the potassium hydroxide aqueous slkali of putting into concentration and be 1mol/L soaks down for 80 ℃ and carried out preliminary treatment, clean dry then in 12 hours again; To put into 800 ℃ of following carbonizations of tube type resistance furnace nitrogen atmosphere 90 minutes respectively through the pretreated peanut shell of aqueous slkali with without the pretreated peanut shell of aqueous slkali, the gained sample is that 20% hydrofluoric acid dips is made two kinds of porous carbons after 72 hours through mass percent concentration; The porous carbon of preliminary treatment peanut shell preparation is designated as C-1, and the porous carbon for preparing without the preliminary treatment peanut shell is designated as C-2;
The preparation of porous carbon electrodes is that to select aqueous electrolyte concentration for use be the potassium hydroxide solution of 6mol/L; Mass percent is that 60% ptfe emulsion is a binding agent; It is the bulk of 1 * 1cm size that nickel foam is cut out; With prepared porous carbon sample C-1 and C-2 grind into powder respectively, by porous carbon: electrically conductive graphite: ptfe emulsion is to mix formation viscosity mud shape thing after 0.85: 0.1: 0.05 mass ratio takes by weighing; Viscosity mud shape thing is transferred on the aluminium foil, be pressed into plate object and transfer on dry and the load weighted foam nickel block uniform spreading after the sheet and open, weighing after 110 ℃ of following vacuumize then, be the good nickel foam bag of drying sandwich-like with aluminium foil again, suppressed 3 minutes under 12.5MP pressure with hydraulic press, obtain electrode slice, porous carbon sample C-1 and the prepared electrode slice of C-2 are designated as EC-1 and EC-2 respectively; So that calculate the quality of active material on the nickel foam, then EC-1 and EC-2 were soaked after 12-24 hour standby in aqueous electrolyte the electrode slice weighing that suppresses;
Three-electrode system is chosen in the test of porous carbon electrodes, and wherein making porous carbon electrodes by oneself is work electrode, and the Ag/AgCl electrode is a reference electrode, and platinized platinum is to electrode; The potassium hydroxide electrolyte of measuring 8ml joins in the electrolytic cell, three-electrode system installed the logical nitrogen in back 30 minutes, remove the oxygen in the solution, test its cyclic voltammetry curve figure and constant current charge-discharge curve chart respectively, and the capacity-cycle-index curve that under the 2A/g current density, discharges and recharges 500 gained;
The test of simulation lithium ion battery charge-discharge performance is that porous carbon, acetylene black, the Kynoar that will obtain after the preliminary treatment of potassium hydroxide aqueous slkali are assembled the lithium ion simulated battery by 0.85: 0.5: 0.1 mass ratio, be designated as LC-1, simulated battery after the assembling is carried out charge-discharge test, test condition is: at room temperature, discharge and recharge between the 0.005V from open circuit voltage with the 0.2A constant current, record first that discharge capacity is 245mAh/g, discharge capacity decays to 45mAh/g for the second time.
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