CN105047425A - Method for preparing graphene/spherical carbon/metal oxide composite material - Google Patents

Method for preparing graphene/spherical carbon/metal oxide composite material Download PDF

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CN105047425A
CN105047425A CN201510375421.7A CN201510375421A CN105047425A CN 105047425 A CN105047425 A CN 105047425A CN 201510375421 A CN201510375421 A CN 201510375421A CN 105047425 A CN105047425 A CN 105047425A
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solution
graphene
metal oxide
gel
oxide composite
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CN105047425B (en
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冯亚宁
毛梦琛
王海祺
陈苗苗
郭华
周汝豪
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Xian University of Technology
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Xian University of Technology
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Abstract

The invention discloses a method for preparing a graphene/spherical carbon/metal oxide composite material, and includes the steps of: weighing the following raw materials in mass percent: 8% to 20% of resorcinol solution or hydroquinone solution, 5% to 10% of formaldehyde solution or furfural solution, 65% to 80% of distilled water, 3% to 8% of graphene suspension, and 4% to 10% of catalyzer, and a content sum of the abovementioned components being 100%; mixing the abovementioned raw materials evenly to obtain a reaction initial solution; moving the reaction initial solution into a glass bottle with a sealing cover, covering the glass bottle with the bottle cover and placing the glass bottle in a drying box for gel reaction, thereby obtaining gel; and after wet gel is dried, dropwise adding saline solution till saturation, after drying, then dropwise adding alkaline solution till saturation, and after carbonization, the graphene/spherical carbon/metal oxide composite material is obtained. The prepared graphene/spherical carbon/metal oxide composite material has a high specific area, double-layer capacitance, relatively high specific capacitance and charge and discharge efficiency, improves electrical conductivity of an electrode, and can satisfy a high-power power supply requirement.

Description

A kind of preparation method of Graphene/Spherical Carbon/metal oxide composite
Technical field
The invention belongs to technical field of nanometer material preparation, relate to a kind of preparation method of Graphene/Spherical Carbon/metal oxide composite.
Background technology
With the nano-carbon material that carbon nano-tube, Graphene and carbon nano-fiber are representative, because the stability of its high-specific surface area, high conductivity and material with carbon element intrinsic, it is the study hotspot in current new energy materials field.Nano-sized carbon and metal oxide composite electrode materials application, at ultracapacitor, can significantly improve the ratio capacitance of ultracapacitor, specific power, specific capacity and efficiency for charge-discharge.But the preparation of existing nano-carbon material needs high temperature or overcritical or freeze drying, and preparation cost is high, and there is ratio capacitance, problem that specific power is lower, what limit electrode material should in scope.
Summary of the invention
The object of this invention is to provide a kind of preparation method of Graphene/Spherical Carbon/metal oxide composite, solve the problem needing high temperature, overcritical or freeze drying etc. to require compared with high technology that existing nano carbon material preparation method for material exists.
Technical scheme of the present invention is, a kind of preparation method of Graphene/Spherical Carbon/metal oxide composite, specifically implements according to following steps:
Step 1, to take by mass percentage: resorcinol solution or quinol solution 8% ~ 20%, formalin or furfuryl aldehyde solution 5% ~ 10%, distilled water 65% ~ 80%, Graphene suspension-turbid liquid 3% ~ 8%, catalyst 4% ~ 10%, the content summation of above component is 100%;
Step 2, the resorcinol solution taken through step 1 or quinol solution, formalin or furfuryl aldehyde solution, Graphene suspension-turbid liquid and catalyst to be added in the distilled water taken through step 1, stir, the initial liquid of obtained reaction;
Step 3, initial for the reaction obtained through step 2 liquid to be moved in the vial of band seal closure, cover bottle cap and be placed in drying box and carry out gel reaction process, obtained wet gel;
Step 4, the wet gel obtained through step 3 is carried out drying process, obtain desiccant gel;
Step 5, configuration quality concentration are the salting liquid of 25% ~ 35%, and salting liquid is dropwise instilled desiccant gel, and dripping quantity is 4-5 times of desiccant gel volume, then puts into drying box fully dry;
Step 6, repetition step 5 many times, until gel is saturated;
Step 7, alkaline solution is dropwise instilled the desiccant gel processed through step 6, put into drying box fully dry;
Step 8, the desiccant gel processed through step 7 is carried out carbonization treatment, obtained Graphene/Spherical Carbon/metal oxide composite.
Feature of the present invention is also,
In step 1, the mass concentration of resorcinol solution or quinol solution is 10% ~ 50%; The mass concentration of formalin or furfuryl aldehyde solution is 10% ~ 50%; Graphene-containing 10mg ~ 15mg in often liter of Graphene suspension-turbid liquid; Catalyst is CoCl 26H 2o, NiCl 22H 2o, CuCl 22H 2o or ZnAc2H 2o.
In step 2, stirring means is magnetic agitation, mixing time 2 ~ 3h.
In step 3, gel reaction temperature is 80 DEG C ~ 95 DEG C, and the gel reaction time is 30min ~ 60min.
In step 4, the specific implementation method of dry process is: the drying box inner drying 1 ~ 3 hour obtained wet gel being positioned over 80 DEG C ~ 100 DEG C.
In step 5, salting liquid is CoCl 26H 2o, NiCl 22H 2o, CuCl 22H 2o or ZnAc2H 2o solution.
In step 7, alkaline solution is the NaOH solution of mass concentration 35% ~ 45%, KOH solution or ammoniacal liquor.
In step 8, the specific implementation method of carbonization treatment is: the tube furnace using both ends open, pass into by 40cc ~ 60cc flow the nitrogen that air or purity are not less than 99.999%, be warmed up to 650 DEG C ~ 700 DEG C according to 10 DEG C ~ 50 DEG C speed per minute and be incubated 2 ~ 4 hours, Temperature fall.
The invention has the beneficial effects as follows, a kind of preparation method of Graphene/Spherical Carbon/metal oxide composite, three-dimensional porous structure material is prepared by in-situ method, then repeatedly infusion method is passed through, composite material-i.e. the super capacitor material of Graphene/Spherical Carbon/metal oxide is obtained after carbonization, there is high specific area, thus possess electric double layer capacitance, the redox reaction of metal oxide is appraised at the current rate and possesses fake capacitance, the two synergy, obtain higher ratio capacitance and efficiency for charge-discharge, improve the conductivity of electrode, high-power power demands can be met.
Accompanying drawing explanation
Fig. 1 is Graphene/Spherical Carbon/metal oxide composite stereoscan photograph prepared by the present invention;
Fig. 2 is the transmission electron microscope photo of Graphene/Spherical Carbon/metal oxide composite prepared by the present invention;
Fig. 3 is the electrochemical properties figure of Graphene/Spherical Carbon/metal oxide composite prepared by the present invention.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
The preparation method of a kind of Graphene/Spherical Carbon/metal oxide composite of the present invention, specifically implements according to following steps:
Step 1, to take by mass percentage: resorcinol solution or quinol solution 8% ~ 20%, formalin or furfuryl aldehyde solution 5% ~ 10%, distilled water 65% ~ 80%, Graphene suspension-turbid liquid 3% ~ 8%, catalyst 4% ~ 10%, the content summation of above component is 100%; Wherein, the mass concentration of resorcinol solution or quinol solution is 10% ~ 50%; The mass concentration of formalin or furfuryl aldehyde solution is 10% ~ 50%; Graphene-containing 10mg ~ 15mg in often liter of Graphene suspension-turbid liquid; Catalyst is CoCl 26H 2o, NiCl 22H 2o, CuCl 22H 2o or ZnAc2H 2o;
Step 2, the resorcinol solution taken through step 1 or quinol solution, formalin or furfuryl aldehyde solution, Graphene suspension-turbid liquid and catalyst are added in the distilled water taken through step 1, magnetic agitation 2h ~ 3h, the initial liquid of obtained reaction;
Step 3, moved in the vial of band seal closure by initial for the reaction obtained through step 2 liquid, cover bottle cap and be placed in drying box and carry out gel reaction process, gel reaction temperature is 80 DEG C ~ 95 DEG C, and the gel reaction time is 30min ~ 60min, obtained wet gel;
Step 4, the wet gel obtained through step 3 is carried out drying process, obtained wet gel is positioned over the drying box inner drying 1 ~ 3 hour of 80 DEG C ~ 100 DEG C, obtains desiccant gel;
Step 5, configuration quality concentration are the salting liquid of 25% ~ 35%, and wherein, salting liquid is CoCl 26H 2o, NiCl 22H 2o, CuCl 22H 2o or ZnAc2H 2o solution, dropwise instills desiccant gel by salting liquid, and dripping quantity is 4-5 times of desiccant gel volume, then puts into drying box fully dry;
Step 6, repetition step 5 many times, until gel is saturated;
Step 7, alkaline solution is dropwise instilled the desiccant gel processed through step 6, put into drying box fully dry; Wherein, alkaline solution is the NaOH solution of mass concentration 35% ~ 45%, KOH solution or ammoniacal liquor;
Step 8, the desiccant gel processed through step 7 is carried out carbonization treatment, use the tube furnace of both ends open, the nitrogen that air or purity are not less than 99.999% is passed into by 40cc ~ 60cc flow, be warmed up to 650 DEG C ~ 700 DEG C according to 10 DEG C ~ 50 DEG C speed per minute and be incubated 2 ~ 4 hours, Temperature fall, obtained Graphene/Spherical Carbon/metal oxide composite.
Embodiment 1
Take by mass percentage: resorcinol solution 8%, formalin 5%, distilled water 80%, Graphene suspension-turbid liquid 3%, CoCl 26H 2o4%, the content summation of above component is 100%; Wherein, the mass concentration of resorcinol solution is 10%; The mass concentration of formalin is 10%; Graphene-containing 10mg in often liter of Graphene suspension-turbid liquid; By the resorcinol solution, formalin, Graphene suspension-turbid liquid and the CoCl that take 26H 2o adds in the distilled water taken, magnetic agitation 2h, the initial liquid of obtained reaction; Moved in the vial of band seal closure by initial for obtained reaction liquid, cover bottle cap and be placed in drying box and carry out gel reaction process, gel reaction temperature is 80 DEG C, and the gel reaction time is 30min, obtained wet gel; Obtained wet gel is positioned over the drying box inner drying 1 hour of 80 DEG C, obtains desiccant gel; Configuration quality concentration is the salting liquid of 25%, and wherein, salting liquid is CoCl 26H 2o, dropwise instills desiccant gel by salting liquid, and dripping quantity is 4 times of desiccant gel volumes, then puts into drying box fully dry, repeatedly, until gel is saturated; The NaOH solution of mass concentration 35% is dropwise instilled the desiccant gel of process, put into drying box fully dry; The desiccant gel of process is carried out carbonization treatment, use the tube furnace of both ends open, the nitrogen that air or purity are not less than 99.999% is passed into by 40cc flow, be warmed up to 650 DEG C according to 10 DEG C of speed per minute and be incubated 2 hours, Temperature fall, obtained Graphene/Spherical Carbon/metal oxide composite.
Embodiment 2
Take by mass percentage: resorcinol solution 20%, furfuryl aldehyde solution 5%, distilled water 65%, Graphene suspension-turbid liquid 5%, NiCl 22H 2o5%, the content summation of above component is 100%; Wherein, the mass concentration of resorcinol solution is 20%; The mass concentration of furfuryl aldehyde solution is 20%; Graphene-containing 11mg in often liter of Graphene suspension-turbid liquid; By the resorcinol solution, furfuryl aldehyde solution, Graphene suspension-turbid liquid and the NiCl that take 22H 2o adds in the distilled water taken, magnetic agitation 2.5h, the initial liquid of obtained reaction; Moved in the vial of band seal closure by initial for obtained reaction liquid, cover bottle cap and be placed in drying box and carry out gel reaction process, gel reaction temperature is 85 DEG C, and the gel reaction time is 40min, obtained wet gel; Obtained wet gel is positioned over the drying box inner drying 1.5 hours of 85 DEG C, obtains desiccant gel; Configuration quality concentration is the salting liquid of 30%, and wherein, salting liquid is NiCl 22H 2o solution, dropwise instills desiccant gel by salting liquid, and dripping quantity is 4.5 times of desiccant gel volumes, then puts into drying box fully dry, repeatedly, until gel is saturated; The KOH solution of mass concentration 40% is dropwise instilled the desiccant gel of process, put into drying box fully dry; The desiccant gel of process is carried out carbonization treatment, use the tube furnace of both ends open, the nitrogen that air or purity are not less than 99.999% is passed into by 45cc flow, be warmed up to 660 DEG C according to 20 DEG C of speed per minute and be incubated 3 hours, Temperature fall, obtained Graphene/Spherical Carbon/metal oxide composite.
Embodiment 3
Take by mass percentage: quinol solution 10%, formalin 7%, distilled water 65%, Graphene suspension-turbid liquid 8%, CuCl 22H 2o10%, the content summation of above component is 100%; Wherein, the mass concentration of quinol solution is 30%; The mass concentration of formalin is 30%; Graphene-containing 12mg in often liter of Graphene suspension-turbid liquid; By take quinol solution, formalin, Graphene suspension-turbid liquid and CuCl 22H 2o adds in the distilled water taken, magnetic agitation 2.5h, the initial liquid of obtained reaction; Moved in the vial of band seal closure by initial for obtained reaction liquid, cover bottle cap and be placed in drying box and carry out gel reaction process, gel reaction temperature is 90 DEG C, and the gel reaction time is 50min, obtained wet gel; Obtained wet gel is positioned over the drying box inner drying 2 hours of 90 DEG C, obtains desiccant gel; Configuration quality concentration is the salting liquid of 30%, and wherein, salting liquid is CuCl 22H 2o solution, dropwise instills desiccant gel by salting liquid, and dripping quantity is 5 times of desiccant gel volumes, then puts into drying box fully dry, repeatedly, until gel is saturated; The ammoniacal liquor of mass concentration 40% is dropwise instilled the desiccant gel of process, put into drying box fully dry; The desiccant gel of process is carried out carbonization treatment, use the tube furnace of both ends open, the nitrogen that air or purity are not less than 99.999% is passed into by 50cc flow, be warmed up to 670 DEG C according to 35 DEG C of speed per minute and be incubated 3 hours, Temperature fall, obtained Graphene/Spherical Carbon/metal oxide composite.
Embodiment 4
Take by mass percentage: quinol solution 12%, furfuryl aldehyde solution 10%, distilled water 70%, Graphene suspension-turbid liquid 4%, ZnAc2H 2o4%, the content summation of above component is 100%; Wherein, the mass concentration of quinol solution is 50%; The mass concentration of furfuryl aldehyde solution is 50%; Graphene-containing 15mg in often liter of Graphene suspension-turbid liquid; By take quinol solution, furfuryl aldehyde solution, Graphene suspension-turbid liquid and ZnAc2H 2o adds in the distilled water taken, magnetic agitation 3h, the initial liquid of obtained reaction; Moved in the vial of band seal closure by initial for obtained reaction liquid, cover bottle cap and be placed in drying box and carry out gel reaction process, gel reaction temperature is 95 DEG C, and the gel reaction time is 60min, obtained wet gel; Obtained wet gel is positioned over the drying box inner drying 3 hours of 100 DEG C, obtains desiccant gel; Configuration quality concentration is the salting liquid of 35%, and wherein, salting liquid is ZnAc2H 2o solution, dropwise instills desiccant gel by salting liquid, and dripping quantity is 5 times of desiccant gel volumes, then puts into drying box fully dry, repeatedly, until gel is saturated; The NaOH solution of mass concentration 45% is dropwise instilled the desiccant gel of process, put into drying box fully dry; The desiccant gel of process is carried out carbonization treatment, use the tube furnace of both ends open, the nitrogen that air or purity are not less than 99.999% is passed into by 60cc flow, be warmed up to 700 DEG C according to 50 DEG C of speed per minute and be incubated 4 hours, Temperature fall, obtained Graphene/Spherical Carbon/metal oxide composite.
In step 1 of the present invention, select resorcinol solution or quinol solution 8% ~ 20%, formalin or furfuryl aldehyde solution 5% ~ 10%, because phenolic system is inner, take benzenediol as material of main part, formaldehyde is as bridge formation part, and formaldehyde is connected based on the carbon on phenyl ring in benzenediol, is formed with captain's chain structure; Select distilled water 65% ~ 80% as the solvent of sol-gel, determine the direction and macroporous structure that connect between phenolic aldehyde sphere, so distilled water is more, is interconnected between ball and there is more sufficient space.If but distilled water is too much, cause again phenolic aldehyde sphere floating and mutual not glue connects.Graphene suspension-turbid liquid 3% ~ 8% is because Graphene is as structural framing, because area is relatively large, very thin thickness, very light weight, density are minimum, so quality accounting is very little.Hydrosol-gel all can carry out under being prepared in weak acid, mild alkaline conditions, and range of catalysts is extensive.
In step 3 of the present invention, select in the vial of band seal closure, effectively can shorten gel time.
In step 4 of the present invention, using tube furnace and the inert gas shielding of both ends open, is not oxidized in order to ensure the carbon in organic substance in heat treatment process, and tube furnace both ends open, is convenient to air-flow turnover;
In step 5 of the present invention, dropwise instilling desiccant gel with salting liquid, is the metal ions M in order to make q.s +disperse fully, equably or be adsorbed on spherical phenolic aldehyde and graphenic surface, thus ensureing that follow-up carbonization forms stable metal oxide layer.
In step 7 of the present invention, dropwise instilling desiccant gel with alkaline solution, is to introduce enough OH -ion, makes the metal ions M in step 5 +be converted into metal base MOH, thus produce metal oxide when making carbonization.
As shown in Figure 1, through Graphene/Spherical Carbon/metal oxide composite that the present invention obtains, the Spherical Carbon adsorption of the about 2m of diameter the metal oxide layer that a layer thickness is approximately 10nm, and metal oxide particle is evenly distributed, layer thickness is even, does not have agglomeration.
As shown in Figure 2, through Graphene/Spherical Carbon/metal oxide composite that the present invention obtains, the ribbon graphene layer state that is interweaved in a three-dimensional structure, between graphene layer by Spherical Carbon and metal oxide spaced apart and do not occur again stacking.
Fig. 3 is the cyclic voltammetry curve figure of preparation method of the present invention and the Graphene/Spherical Carbon/metal oxide composite prepared by common preparation method, and wherein, metal oxide is ZnO sweep speed is 20mV/s.As seen from Figure 3, the closed area of preparation method's curve of the present invention is larger than the closed area of common preparation method curve, illustrate that the electrode specific capacity of homogenous quantities compares, preparation method of the present invention is larger than the electrode specific capacity of common preparation method, and, the measuring current amplitude maximum of preparation method of the present invention is about 5mA, the measuring current amplitude maximum of common preparation method is 0.78mA, the material current amplitude that the Graphene/Spherical Carbon/metal oxide composite prepared through the present invention is prepared than commonsense method is much larger, illustrate that there is more excellent electric property.

Claims (8)

1. a preparation method for Graphene/Spherical Carbon/metal oxide composite, is characterized in that, specifically implements according to following steps:
Step 1, to take by mass percentage: resorcinol solution or quinol solution 8% ~ 20%, formalin or furfuryl aldehyde solution 5% ~ 10%, distilled water 65% ~ 80%, Graphene suspension-turbid liquid 3% ~ 8%, catalyst 4% ~ 10%, the content summation of above component is 100%;
Step 2, the resorcinol solution taken through step 1 or quinol solution, formalin or furfuryl aldehyde solution, Graphene suspension-turbid liquid and catalyst to be added in the distilled water taken through step 1, stir, the initial liquid of obtained reaction;
Step 3, initial for the reaction obtained through step 2 liquid to be moved in the vial of band seal closure, cover bottle cap and be placed in drying box and carry out gel reaction process, obtained wet gel;
Step 4, the wet gel obtained through step 3 is carried out drying process, obtain desiccant gel;
Step 5, configuration quality concentration are the salting liquid of 25% ~ 35%, and salting liquid is dropwise instilled desiccant gel, and dripping quantity is 4 ~ 5 times of desiccant gel volumes, then puts into drying box fully dry;
Step 6, repetition step 5 many times, until gel is saturated;
Step 7, alkaline solution is dropwise instilled the desiccant gel processed through step 6, put into drying box fully dry;
Step 8, the desiccant gel processed through step 7 is carried out carbonization treatment, obtained Graphene/Spherical Carbon/metal oxide composite.
2. the preparation method of Graphene/Spherical Carbon/metal oxide composite according to claim 1, is characterized in that, in described step 1, the mass concentration of resorcinol solution or quinol solution is 10% ~ 50%; The mass concentration of formalin or furfuryl aldehyde solution is 10% ~ 50%; Graphene-containing 10mg ~ 15mg in often liter of Graphene suspension-turbid liquid; Catalyst is CoCl 26H 2o, NiCl 22H 2o, CuCl 22H 2o or ZnAc2H 2o.
3. the preparation method of Graphene/Spherical Carbon/metal oxide composite according to claim 1, is characterized in that, in described step 2, stirring means is magnetic agitation, mixing time 2 ~ 3h.
4. the preparation method of Graphene/Spherical Carbon/metal oxide composite according to claim 1, is characterized in that, in described step 3, gel reaction temperature is 80 DEG C ~ 95 DEG C, and the gel reaction time is 30min ~ 60min.
5. the preparation method of Graphene/Spherical Carbon/metal oxide composite according to claim 1, it is characterized in that, in described step 4, the specific implementation method of dry process is: the drying box inner drying 1 ~ 3 hour obtained wet gel being positioned over 80 DEG C ~ 100 DEG C.
6. the preparation method of Graphene/Spherical Carbon/metal oxide composite according to claim 1, is characterized in that, in described step 5, salting liquid is CoCl 26H 2o, NiCl 22H 2o, CuCl 22H 2o or ZnAc2H 2o solution.
7. the preparation method of Graphene/Spherical Carbon/metal oxide composite according to claim 1, is characterized in that, in described step 7, alkaline solution is the NaOH solution of mass concentration 35% ~ 45%, KOH solution or ammoniacal liquor.
8. the preparation method of Graphene/Spherical Carbon/metal oxide composite according to claim 1, it is characterized in that, in described step 8, the specific implementation method of carbonization treatment is: the tube furnace using both ends open, the nitrogen that air or purity are not less than 99.999% is passed into by 40cc ~ 60cc flow, be warmed up to 650 DEG C ~ 700 DEG C according to 10 DEG C ~ 50 DEG C speed per minute and be incubated 2 ~ 4 hours, Temperature fall.
CN201510375421.7A 2015-06-30 2015-06-30 A kind of preparation method of graphene/Spherical Carbon/metal oxide composite Expired - Fee Related CN105047425B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120034442A1 (en) * 2010-08-06 2012-02-09 Lawrence Livermore National Security, Llc Graphene aerogels
CN102515150A (en) * 2011-12-08 2012-06-27 同济大学 Method for preparing multilayer graphene-carbon material
CN102774824A (en) * 2012-06-11 2012-11-14 北京化工大学 Method for preparing graphene crosslinked type organic aerogel and carbon aerogel by normal-pressure drying

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120034442A1 (en) * 2010-08-06 2012-02-09 Lawrence Livermore National Security, Llc Graphene aerogels
CN102515150A (en) * 2011-12-08 2012-06-27 同济大学 Method for preparing multilayer graphene-carbon material
CN102774824A (en) * 2012-06-11 2012-11-14 北京化工大学 Method for preparing graphene crosslinked type organic aerogel and carbon aerogel by normal-pressure drying

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