CN104176721A - Carbon composite material, and preparation method and application thereof - Google Patents
Carbon composite material, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a carbon composite material. The carbon composite material comprises 0.1-35wt% of a carbon nanomaterial and 99.9-65wt% of amorphous carbon with a high surface area; the carbon nanometer is one or a mixture of more of carbon nanotubes, carbon fibers, graphene oxide and graphene; and the specific surface area, the pore volume and the conductivity of the composite material are not lower than 800m<2>/g, not lower than 0.3cm<3> and not lower than 4S/cm respectively, and the aperture of the composite material is 0.5-10nm. The carbon composite material has the respective characteristics of the carbon nanomaterial and the amorphous carbon, realizes the organic combination of the carbon nanomaterial and the amorphous carbon in functions, has high surface area and high conductivity, and can provide superior capacity and rate performance as an excellent electrode and conductive material of super capacitors, lithium ion capacitors, fuel batteries and lead carbon battery electrodes. The carbon composite material can remove impurities in water as an electrode material in water treatment devices.
Description
Technical field
The invention belongs to Material Field, be specifically related to a kind of carbon composite and its preparation method and application.
Background technology
The absorbent charcoal material with high-specific surface area is having a wide range of applications aspect environmental protection, pharmacy, electronics, catalysis, energy storage.High-specific surface area Carbon Materials generally consists of graphited crystallite and non-graphitized amorphous carbonaceous.Amorphous carbonaceous and greying crystallite are interconnected to constitute the gap structure of gac.The preparation of current absorbent charcoal material is mainly passed through after the carbonization of carbon elements presoma, reaction obtains high-specific surface area with activating reagent.Formed vesicular structure can cause the structural defect of amorphous carbon, causes the decline of conductivity and mechanical property.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, the object of this invention is to provide a kind of carbon composite, by the performance in conjunction with carbon nanomaterial and unformed Carbon Materials, form the carbon material simultaneously with high-specific surface area and high conductivity.Another object of the present invention is to provide a kind of method of preparing carbon composite.The present invention also has an object to be to provide the application of above-mentioned carbon composite.
Technical scheme: in order to realize foregoing invention object, the technical solution used in the present invention is as follows:
A carbon composite, is comprised of with the high surface area amorphous carbon that accounts for carbon composite gross weight 99.9 ~ 65% carbon nanomaterial that accounts for carbon composite gross weight 0.1 ~ 35%; Described carbon nanomaterial is one or more the mixture in carbon nanotube, carbon fiber, graphite flake, graphene oxide and Graphene; Described matrix material specific surface area is not less than 800m
2/ g, pore volume is not less than 0.3cm
3/ g, specific conductivity is not less than 4S/cm, and the pore size of matrix material is 0.5 ~ 10 nanometer.
In described carbon nanomaterial, described carbon nanotube comprises Single Walled Carbon Nanotube and multi-walled carbon nano-tubes; The tube wall layer number of multi-walled carbon nano-tubes is 2-100 layer; The length of single nanotube is not less than 500 nanometers.
In described carbon nanomaterial, the area of Graphene or graphite flake is 1 ~ 400 square micron, and the number of plies of Graphene is 1 ~ 10 layer.
The diameter of described carbon fiber is 40-500 nanometer, and length is not less than 1 micron.
A method of preparing described carbon composite, comprises the following steps:
1) amorphous carbon precursor material is distributed in water, adds carbon nanomaterial, mix, 90 ~ 300 ℃ of temperature controls, react 0.5 ~ 48 hour; Cool to room temperature, collects product;
2) product and activating reagent are mixed, be transferred in High Temperature Furnaces Heating Apparatus, under protection of inert gas, at 600 ~ 900 ℃, process 0.5 ~ 48 hour; Cool to room temperature, by product deionized water rinsing, dries; Described activating reagent comprises phosphoric acid, sodium hydroxide, potassium hydroxide, zinc chloride and calcium chloride; Described rare gas element comprises argon gas, nitrogen and helium; The weight ratio of activator and product is 10:1 ~ 1:10;
Or,
Product is transferred in High Temperature Furnaces Heating Apparatus, passes into mixed gas, 600 ~ 900 ℃ process 0.5-48 hour after cool to room temperature; Described mixed gas is selected from nitrogen, argon gas, helium, account for the water vapour of cumulative volume 0.01 ~ 99.99%, account for one or more in the carbonic acid gas of cumulative volume 0.01 ~ 99.99%.
Described amorphous carbon precursor is selected from polyethylene, poly-the third ethene, polycarbonate, phenol, formaldehyde, glucose, sucrose, fructose, Mierocrystalline cellulose, xylogen, resol and polyvinyl alcohol.
The application of described carbon composite in the middle of water treatment.
Beneficial effect: compared with prior art, carbon composite of the present invention and its preparation method and application, raw material is easy to get, with low cost, and preparation condition is gentle, and is convenient to industrial amplification production.Material has the feature of carbon nanomaterial and amorphous carbon material simultaneously, carbon nanomaterial and the combination of amorphous carbon material in function have been realized, there is high surface area and high conductivity simultaneously, overcome the defect that current carbon material is difficult to possess high-specific surface area and high conductivity in application simultaneously, can be used as good electrode and the electro-conductive material of super capacitor, lithium-ion capacitor, fuel cell and plumbous carbon battery electrode, superior capacity and high rate performance is provided.Matrix material also can be used as the electrode materials in water treating equipment, utilizes its high-specific surface area and high conductivity to purify the impurity in water.There is good practicality, can produce good economic benefit and social effect.
Accompanying drawing explanation
Fig. 1 is the preparation process figure of carbon composite;
Fig. 2 is the structural representation of carbon composite;
Fig. 3 is the scanning electron microscope microgram of carbon composite;
Fig. 4 is the comparative result figure of carbon composite and conventional material super capacitor electrode.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment 1
The preparation of carbon composite, as shown in Figure 1, takes 4 grams of polyethylene powders, is distributed in 30 ml waters.Add 0.34 gram of carbon nanotube, stir; Mixture, at 120 ℃, is heated 2 hours, and cool to room temperature, collects product.Product and sodium hydroxide are mixed by weight 1:2, be transferred in High Temperature Furnaces Heating Apparatus, under rare gas element (argon gas, nitrogen and helium arbitrarily than) protection, be heated to 600 ℃, react 2 hours; Cool to room temperature, by product deionized water rinsing, dries 12 hours, standby.
The capacity of matrix material and high rate performance are obtained by cyclic voltammetry test: get carbon composite, graphitized carbon black and LA132 that weight ratio is 90:5:5, stir, on aluminium foil pole piece surface, be coated with.After after pole piece is dry, Kun presses, gauge control is at 50 ~ 200 microns.It is the circular electrode of 1 centimetre that pole piece is cut into diameter, in glove box, circular electrode is anodal, barrier film, and circular electrode negative pole stacks in order to inject and is assembled into button electrical condenser after electrolytic solution and tests.
Capacity and high rate performance are tested by cyclic voltammetric method on electrochemical workstation.Wherein positive and negative electrode voltage range is 0-2.7V, and voltage changing rate is respectively 5 and 200mV/s.
The specific surface area of matrix material obtains (Autosorb iQ, U.S. Kang Ta company) by the nitrogen test on specific surface tester that is adsorbed on from the teeth outwards.The pattern scanning electron microscope of matrix material characterizes and obtains.
The structure of carbon composite as shown in Figure 2, the scanning electron microscope microgram of carbon composite, as shown in Figure 3, test result shows that matrix material specific surface area is higher than 2200m
2/ g, pore volume is higher than 0.5cm
3/ g, electric conductivity is higher than 20S/cm, the specific storage of product 5,10,20,50,100 and 200mV/s under higher than 150,130,120,100,80 and 70F/g.
Embodiment 2
Take 4 grams of resol powder, be distributed in 30 ml waters.After adding 0.34 gram of carbon fiber, stir.Mixture was heated after 2 hours at 150 ℃, after cool to room temperature, collect product.Product and KOH are transferred in High Temperature Furnaces Heating Apparatus after 1:3 mixes, react 1 hour be heated to 750 ℃ under rare gas element (argon gas, nitrogen and helium arbitrarily than) protection after.After cool to room temperature, product is standby after 12 hours with lower oven dry after deionized water rinsing.Matrix material specific surface area is 2200m
2/ g, pore volume is higher than 0.5cm
3/ g, electric conductivity is higher than 30S/cm, the specific storage of product 5,10,20,50 and 100mV/s under higher than 130,110,90,80 and 70F/g.
Embodiment 3
Take 10.625 grams of sucrose powder, be distributed in 30 ml waters.After adding 0.34 gram of carbon nanotube and Graphene mixture (weight ratio 1:1), stir.Mixture was heated after 2 hours at 220 ℃, after cool to room temperature, collect product.After product and phosphoric acid (weight ratio 1:3) weight ratio are mixed, be transferred in High Temperature Furnaces Heating Apparatus, react 1 hour be heated to 800 ℃ under rare gas element (argon gas, nitrogen and helium arbitrarily than) protection after.After cool to room temperature, product is standby after 12 hours with lower oven dry after deionized water rinsing.
After testing, matrix material specific surface area is 2000m
2/ g, pore volume is higher than 0.5cm
3/ g, electric conductivity is higher than 30S/cm.The specific storage of matrix material 5,10,20,50,100 and 200mV/s under higher than 140,130,120,110,100 and 90F/g.
Embodiment 4
Take 8 grams of pva powders, be distributed in 30 ml waters.After adding 0.34 gram of carbon nanotube, stir.Mixture was heated after 2 hours at 250 ℃, after cool to room temperature, collect product.After product and zinc chloride (weight ratio 1:2) are mixed, be transferred in High Temperature Furnaces Heating Apparatus, react 1 hour be heated to 850 ℃ under rare gas element (argon gas, nitrogen and helium arbitrarily than) protection after.After cool to room temperature, product is standby after 12 hours with lower oven dry after deionized water rinsing.
After testing, matrix material specific surface area is not less than 2000m
2/ g, pore volume is higher than 0.6cm
3/ g, electric conductivity is higher than 40S/cm.The specific storage of product 5,10,20,50,100 and 200mV/s under higher than 120,100,90,80,70 and 65F/g.
Embodiment 5
Take 10 grams of glucose powder, be distributed in 30 ml waters.After adding 0.17 gram of Graphene, stir.Mixture was heated after 12 hours at 180 ℃, after cool to room temperature, collect product.After product and sodium hydroxide (weight ratio 1:3) are mixed, be transferred in High Temperature Furnaces Heating Apparatus, react 2 hours be heated to 700 ℃ under rare gas element (argon gas, nitrogen and helium arbitrarily than) protection after.After cool to room temperature, product is standby after 12 hours with lower oven dry after deionized water rinsing.
After testing, the specific storage of product under 5mV/s higher than 110F/g.
Embodiment 6
As shown in Figure 1, take 10 grams of fructose powder, be distributed in 30 ml waters.After adding 3.4 milligrams of carbon nanotubes, stir.Mixture was heated after 12 hours at 180 ℃, after cool to room temperature, collect product.After product and sodium hydroxide (weight ratio 1:3) are mixed, be transferred in High Temperature Furnaces Heating Apparatus, react 1 hour be heated to 850 ℃ under rare gas element (argon gas, nitrogen and helium arbitrarily than) protection after.After cool to room temperature, product is standby after 12 hours with lower oven dry after deionized water rinsing.
After testing, the specific storage of product under 5mV/s higher than 95F/g.
Embodiment 7
Take 10 grams of sucrose powder, be distributed in 30 ml waters.After adding 0.34 milligram of carbon nanotube, stir.Mixture was heated after 12 hours at 180 ℃, after cool to room temperature, collect product.After product and sodium hydroxide (weight ratio 1:3) are mixed, be transferred in High Temperature Furnaces Heating Apparatus, react 1 hour be heated to 850 ℃ under rare gas element (argon gas, nitrogen and helium arbitrarily than) protection after.After cool to room temperature, product is standby after 12 hours with lower oven dry after deionized water rinsing.
After testing, the specific storage of product under 5mV/s higher than 90F/g.
Embodiment 8
Take 10 grams of xylogen powder, be distributed in 30 ml waters.After adding 0.85 gram of graphene oxide, stir.Mixture was heated after 2 hours at 250 ℃, after cool to room temperature, collect product.After product and calcium chloride are mixed, be transferred in High Temperature Furnaces Heating Apparatus, react 3 hours be heated to 800 ℃ under rare gas element (argon gas, nitrogen and helium arbitrarily than) protection after.After cool to room temperature, product is standby after 12 hours with lower oven dry after deionized water rinsing.The specific storage of product is higher than 100F/g under 5mV/s, and electric conductivity is higher than 40S/cm.
Embodiment 9
Take 10 grams of cellulose powders, be distributed in 30 ml waters.After adding 1.8 grams of carbon nanotubes, stir.Mixture was heated after 12 hours at 180 ℃, after cool to room temperature, collect product.After product and potassium hydroxide are mixed, be transferred in High Temperature Furnaces Heating Apparatus, react 0.5 hour be heated to 900 ℃ under rare gas element (argon gas, nitrogen and helium arbitrarily than) protection after.After cool to room temperature, product is standby after 12 hours with lower oven dry after deionized water rinsing.The specific storage of product is higher than 100F/g under 5mV/s, and electric conductivity is higher than 40S/cm.
Embodiment 10
Take 8 grams of polyvinyl alcohol, be dissolved in 30 ml waters.After adding 0.8 gram of carbon nanotube, stir after 2 hours, transfer in the hydrothermal reaction kettle of 100 milliliters, at 280 ℃, heat after 12 hours, by reactor cool to room temperature, collect product.Product, with after a large amount of washed with de-ionized water, is dried in vacuum drying oven.Product is transferred in tube furnace, under argon shield, be heated to after 900 ℃, pass into the argon gas of moisture vapor (5% volume ratio), process 6 hours, obtain product.
Material performance test method is as embodiment 1, and the specific surface area of resulting matrix material is higher than 1000m
2/ g, pore volume is higher than 0.5cm
3/ g, electric conductivity is higher than 60S/cm, and specific storage is being swept under fast 5mV/s over 120F/g.
Embodiment 11
Get 15 grams of polypropylene, be distributed in 30 ml waters, stir after adding 0.3 gram of carbon nanotube.Transfer in reaction vessel heat treated at 300 ℃.To after product cool to room temperature, filter and collect.After product is dried in vacuum drying oven, and after zinc chloride mixes, under rare gas element (argon gas, nitrogen and helium arbitrarily than) protection, be heated to 900 ℃ and process 30 minutes.After product being washed till to neutrality with deionized water, in baking oven, dry.
Material properties test is as embodiment 1, and the specific surface area of resulting matrix material is higher than 1100m
2/ g, pore volume is higher than 0.45cm
3/ g, electric conductivity is higher than 50S/cm, and specific storage is being swept under fast 5mV/s higher than 120F/g.
Embodiment 12
0.5 gram of SBR is dissolved in 10 ml deionized water, stirs 2 hours, add the carbon composite of 9.5 grams of embodiment, 4 preparations, stir after 2 hours to obtaining uniform sizing material.By slurry coating, at aluminium foil surface, coat-thickness is 60-100 micron.Coating pole piece toasts and after 24 hours, is cut into the circular electrode that diameter is 1cm under vacuum condition.In glove box, circular electrode is anodal, barrier film, circular electrode negative pole becomes button electrical condenser after stacking in order rear injection electrolytic solution encapsulation.The capacity of electrical condenser calculates by the cyclic voltammetry curve area of sweeping in fast situation in 0-2.7V difference.The specific storage of electrode 5,10,20,50,100 and 200mV/s under higher than 120,110,100,80,60 and 40F/g.Compare down, conventional gac gram volume is under the same conditions 84,78,66,35,19 and 11F/g.
Embodiment 13
0.5 gram of SBR is dissolved in 10 ml deionized water, stirs after 2 hours, to add in 9 grams of embodiment 1 and continue to stir 2 hours to obtaining uniform sizing material after carbon composite and 0.5 gram of graphitized carbon black.By slurry coating, at aluminium foil surface, coat-thickness is 60-100 micron.Coating pole piece toasts and after 24 hours, is cut into the circular electrode that diameter is 1cm under vacuum condition.In glove box, circular electrode is anodal, barrier film, circular electrode negative pole becomes button electrical condenser after stacking in order rear injection electrolytic solution encapsulation.The capacity of electrical condenser calculates by the cyclic voltammetry curve area of sweeping in fast situation in 0-2.7V difference.The specific storage of electrode 5,10,20,50,100 and 200mV/s under higher than 120,110,100,90,60 and 50F/g.Compare down, conventional gac gram volume is under the same conditions 84,81,80,74,58,45 and 33F/g.
Embodiment 14
Super capacitor electrode preparation method 1: see the anode preparation method in patent application 201201287097.X: get carbon nanotube and gac (YP50F, Kurray), after ball milling mixes in ball mill.Under slowly stirring, join in the nmp solution of 10 milliliters of poly-inclined to one side tetrafluoroethylene (10wt%).Wherein, the weight ratio of carbon nanotube, gac and PVDF is 4:86:10.After mixture is stirred, on aluminium foil pole piece surface, be coated with.After Kun presses, coating thickness is controlled at 50 ~ 200 microns.After being cut into, pole piece is cut into diameter and is the circular electrode of 1 centimetre, and in glove box, circular electrode is anodal, barrier film, circular electrode negative pole stacks in order to inject and is assembled into button electrical condenser after electrolytic solution and tests.Capacity and high rate performance are tested by cyclic voltammetric method on electrochemical workstation.Wherein positive and negative electrode voltage range is 0-2.7V, and voltage changing rate is respectively 5,10,20,50,100,200mV/s, and the capacity of electrical condenser calculates by the area of cyclic voltammetry curve.
Super capacitor electrode preparation method 2: 0.5 gram of LA133 is dissolved in 10 ml deionized water, stirs after 2 hours and add in embodiment 1 and continue after 9.5 grams of carbon composites to stir 2 hours to obtaining uniform sizing material.By slurry coating, at aluminium foil surface, coat-thickness is 60-100 micron.Coating pole piece toasts and after 24 hours, is cut into diameter under vacuum condition is the circular electrode of 1 centimetre.In glove box, circular electrode is anodal, barrier film, circular electrode negative pole becomes button electrical condenser after stacking in order rear injection electrolytic solution encapsulation.Voltage changing rate is respectively 5,10,20,50,100,200mV/s, and the capacity of electrical condenser calculates by the area of cyclic voltammetry curve.Carbon composite Performance Ratio prepared by two kinds of methods is shown in Fig. 4, and the Capacitance reserve performance that the material that preparation method 2 obtains is swept under speed in difference is better than the material that preparation method 1 obtains.
Embodiment 15
By specific surface area, be 2000m
2the carbon composite of/g, polyvinylidene difluoride (PVDF) and deionized water mix by the mass ratio of 68:8:24, and compound is evenly coated on electrically-conductive backing plate, and under 50 ℃ of conditions, vacuum-drying is 8 hours; Using aforesaid substrate as negative pole, being immersed into concentration is in 0.50mol/L plumbic acetate solution again, infiltrates after 20 minutes, take stereotype as anodal, in current density, is 100 mA/cm
2under condition, galvanic deposit is 16 seconds, and the pole plate after galvanic deposit is taken out, and is put in vacuum drying oven, dry under 50 ℃ of conditions, and desciccate is scraped from titanium plate, obtains plumbous carbon composite.Resulting plumbous carbon composite can be prepared lead-acid cell negative plates with lead powder and cream.
Embodiment 16
Active carbon powder, tetrafluoroethylene and graphitized carbon black are mixed according to the ratio of 87:8:5, using deionized water as solvent, after mixture is stirred and within l hour, makes it evenly, roll-in becomes the pole piece of thickness homogeneous, after will pole piece pressurization placing, make electrode.After being formed to positive and negative electrode, two electrode pairings under 1.2V, the negative ions in water is adsorbed.Utilize its high-specific surface area and high conductivity to purify the impurity in water, through test, adsorption-edulcoration is respond well.
Claims (7)
1. a carbon composite, is characterized in that: the carbon nanomaterial that accounts for carbon composite gross weight 0.1 ~ 35%, consist of with the high surface area amorphous carbon that accounts for carbon composite gross weight 99.9 ~ 65%; Described carbon nanomaterial is one or more the mixture in carbon nanotube, carbon fiber, graphite flake, graphene oxide and Graphene; Described matrix material specific surface area is not less than 800m
2/ g, pore volume is not less than 0.3cm
3/ g, specific conductivity is not less than 4S/cm, and the pore size of matrix material is 0.5 ~ 10 nanometer.
2. carbon composite according to claim 1, is characterized in that: in described carbon nanomaterial, described carbon nanotube comprises Single Walled Carbon Nanotube and multi-walled carbon nano-tubes; The tube wall layer number of multi-walled carbon nano-tubes is 2-100 layer; The length of single nanotube is not less than 500 nanometers.
3. carbon composite according to claim 1, is characterized in that: in described carbon nanomaterial, the area of Graphene or graphite flake is 1 ~ 400 square micron, and the number of plies of Graphene is 1 ~ 10 layer.
4. carbon composite according to claim 1, is characterized in that: the diameter of described carbon fiber is 40-500 nanometer, and length is not less than 1 micron.
5. a method of preparing carbon composite claimed in claim 1, is characterized in that, comprises the following steps:
1) amorphous carbon precursor material is distributed in water, adds carbon nanomaterial, mix, 90 ~ 300 ℃ of temperature controls, react 0.5 ~ 48 hour; Cool to room temperature, collects product;
2) product and activating reagent are mixed, be transferred in High Temperature Furnaces Heating Apparatus, under protection of inert gas, at 600 ~ 900 ℃, process 0.5 ~ 48 hour; Cool to room temperature, by product deionized water rinsing, dries; Described activating reagent comprises phosphoric acid, sodium hydroxide, potassium hydroxide, zinc chloride and calcium chloride; Described rare gas element comprises argon gas, nitrogen and helium; The weight ratio of activator and product is 10:1 ~ 1:10;
Or,
Product is transferred in High Temperature Furnaces Heating Apparatus, passes into mixed gas, 600 ~ 900 ℃ process 0.5-48 hour after cool to room temperature; Described mixed gas is selected from nitrogen, argon gas, helium, account for the water vapour of cumulative volume 0.01 ~ 99.99%, account for one or more in the carbonic acid gas of cumulative volume 0.01 ~ 99.99%.
6. prepare according to claim 5 the method for carbon composite, it is characterized in that: described amorphous carbon precursor is optional from polyethylene, poly-the third ethene, polycarbonate, phenol, formaldehyde, glucose, sucrose, fructose, Mierocrystalline cellulose, xylogen, resol and polyvinyl alcohol.
7. the application of carbon composite claimed in claim 1 in the middle of water treatment.
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