阅读说明：本技术 一种氮掺杂碳纤维包覆类石墨烯层间复合材料的制备方法 (A kind of preparation method of nitrogen-doped carbon fiber cladding class graphene interlayer composite ) 是由 阚侃 王珏 马宇良 张晓臣 张伟君 于 2019-09-05 设计创作，主要内容包括：一种氮掺杂碳纤维包覆类石墨烯层间复合材料的制备方法,涉及电极材料制备技术领域。本发明的目的是要解决现有碳材料缺少孔结构,无法提升电解液离子的传输效率,不利于提高电极材料的比电容的问题。方法：对可膨胀石墨原料进行膨化处理,得到膨胀石墨；将十六烷基三甲基溴化铵加入到酸性溶液中,加入膨胀石墨和过硫酸铵,搅拌均匀,在冰水浴条件下,滴加吡咯单体,继续反应,用清洗液洗涤至中性,烘干,得到中间体材料；将中间体材料在惰性气体的保护下,升温至700℃～900℃,冷却至室温,得到一种氮掺杂碳纤维包覆类石墨烯层间复合材料。本发明可获得一种氮掺杂碳纤维包覆类石墨烯层间复合材料的制备方法。(A kind of preparation method of nitrogen-doped carbon fiber cladding class graphene interlayer composite, is related to electrode material preparation technical field.The invention aims to solve existing carbon material to lack pore structure, the efficiency of transmission of electrolyte ion can not be promoted, is unfavorable for the problem of improving the specific capacitance of electrode material.Method: expanding treatment is carried out to expansible graphite raw material, obtains expanded graphite；Cetyl trimethylammonium bromide is added in acid solution, expanded graphite and ammonium persulfate is added, stirs evenly, under the conditions of ice-water bath, pyrrole monomer is added dropwise, the reaction was continued, is washed with cleaning solution to neutrality, drying obtains intermediary material；By intermediary material under the protection of inert gas, 700 DEG C~900 DEG C are warming up to, is cooled to room temperature, obtains a kind of nitrogen-doped carbon fiber cladding class graphene interlayer composite.The present invention can get a kind of preparation method of nitrogen-doped carbon fiber cladding class graphene interlayer composite.)

1. a kind of preparation method of nitrogen-doped carbon fiber cladding class graphene interlayer composite, it is characterised in that the preparation method It completes according to the following steps:

One, the expanding treatment for carrying out 15s~60s to expansible graphite raw material using microwave expansion method, obtains expanded graphite；By ten Six alkyl trimethyl ammonium bromides are added in acid solution, and stirring and dissolving, expanded graphite are then added, and in magnetic agitation item Ammonium persulfate is added under part, continues to be stirred until homogeneous, then under the conditions of 0 DEG C~5 DEG C of ice-water baths, with 15 drops/min~30 drops/min Rate pyrrole monomer is added dropwise, the reaction was continued 12h~36h is washed with cleaning solution to neutrality, finally in 60 DEG C~100 DEG C conditions Lower drying 6h~12h, obtains intermediary material；The volume of the quality and acid solution of the cetyl trimethylammonium bromide Than for (10g~20g): the mass ratio of (100mL~500mL), the expanded graphite and cetyl trimethylammonium bromide is (1 ~5): the mass ratio of (10~20), the expanded graphite and ammonium persulfate is (1~5): (5~20), the matter of the expanded graphite The ratio of amount and the volume of pyrrole monomer is (1g~5g): (10mL~30mL)；

Two, intermediary material is placed in atmosphere tube type furnace, under the protection of inert gas, with 2 DEG C/min~10 DEG C/min Heating rate is warming up to 700 DEG C~900 DEG C, and 1h~5h is kept the temperature at 700 DEG C~900 DEG C, then cools to room temperature, obtains nitrogen Doped carbon fiber coats class graphene interlayer composite.

2. a kind of preparation method of nitrogen-doped carbon fiber cladding class graphene interlayer composite according to claim 1, It is characterized in that the partial size of expansible graphite raw material described in step 1 is 30 μm~160 μm.

3. a kind of preparation method of nitrogen-doped carbon fiber cladding class graphene interlayer composite according to claim 1, It is characterized in that acid solution described in step 1 is the hydrochloric acid solution of concentration 1.0mol/L~3.0mol/L.

4. a kind of preparation method of nitrogen-doped carbon fiber cladding class graphene interlayer composite according to claim 1, It is characterized in that cleaning solution described in step 1 is dehydrated alcohol and deionized water, washes of absolute alcohol 3 is first used in step 1 It is secondary~5 times, then be washed with deionized to neutrality.

5. a kind of preparation method of nitrogen-doped carbon fiber cladding class graphene interlayer composite according to claim 1, It is characterized in that the ratio of the volume of the quality and acid solution of cetyl trimethylammonium bromide described in step 1 is 14.6g:200mL。

6. a kind of preparation method of nitrogen-doped carbon fiber cladding class graphene interlayer composite according to claim 1, It is characterized in that the mass ratio of expanded graphite described in step 1 and cetyl trimethylammonium bromide is 3.22:14.6.

7. a kind of preparation method of nitrogen-doped carbon fiber cladding class graphene interlayer composite according to claim 1, It is characterized in that the mass ratio of expanded graphite described in step 1 and ammonium persulfate is 3.22:13.7.

8. a kind of preparation method of nitrogen-doped carbon fiber cladding class graphene interlayer composite according to claim 1, It is characterized in that the ratio of the volume of the quality and pyrrole monomer of expanded graphite described in step 1 is 3.22g:16.1mL.

9. a kind of preparation method of nitrogen-doped carbon fiber cladding class graphene interlayer composite according to claim 1, It is characterized in that inert gas described in step 2 is nitrogen, and the rate that is filled with of nitrogen is 60mL/min~100mL/min.

10. a kind of preparation method of nitrogen-doped carbon fiber cladding class graphene interlayer composite according to claim 1, It is characterized in that intermediary material is placed in atmosphere tube type furnace in the step 2, under the protection of inert gas, with 2 DEG C/ Min~10 DEG C/min heating rate is warming up to 800 DEG C, and 1h~5h is kept the temperature at 800 DEG C.

Technical field

The present invention relates to electrode material preparation technical fields.

Background technique

Supercapacitor is a kind of passive energy-storage travelling wave tube of high-energy density, it has, and the charging time is short, long service life, Good temp characteristic, it is energy saving and environmentally protective the features such as.Supercapacitor is widely used, the power balance as hoisting apparatus Power supply, it is possible to provide the electric power of super-large current；As vehicle launch power supply, starting efficiency and reliability are all than traditional battery Height can completely or partially substitute traditional battery；Traction energy as vehicle can produce electric car, substitution tradition Internal combustion engine, the existing trolleybus of transformation；With the smooth starting that militarily can guarantee the battlebuses such as tank, panzer, especially It is in cold winter；It can also be used as the pulse energy of laser weapon simultaneously.Existing carbon material is mostly graphite material electrode, Although its laminated structure specific surface area is larger and excellent electric conductivity is due to lacking pore structure can not promote electrolyte ion Efficiency of transmission, therefore be unfavorable for improve electrode material specific capacitance.

Summary of the invention

The invention aims to solve existing carbon material to lack pore structure, the transmission effect of electrolyte ion can not be promoted Rate is unfavorable for the problem of improving the specific capacitance of electrode material, and provides multiple between a kind of nitrogen-doped carbon fiber cladding class graphene layer The preparation method of condensation material.

A kind of preparation method of nitrogen-doped carbon fiber cladding class graphene interlayer composite, is completed according to the following steps:

One, the expanding treatment for carrying out 15s~60s to expansible graphite raw material using microwave expansion method, obtains expanded graphite； Cetyl trimethylammonium bromide is added in acid solution, and stirring and dissolving, expanded graphite is then added, and stir in magnetic force Ammonium persulfate is added under the conditions of mixing, continues to be stirred until homogeneous, then under the conditions of 0 DEG C~5 DEG C of ice-water baths, with 15 drops/min~30 Pyrrole monomer is added dropwise in drop/min rate, and the reaction was continued 12h~36h is washed with cleaning solution to neutrality, finally 60 DEG C~100 6h~12h is dried under the conditions of DEG C, obtains intermediary material；The quality of the cetyl trimethylammonium bromide and acid solution The ratio of volume is (10g~20g): (100mL~500mL), the quality of the expanded graphite and cetyl trimethylammonium bromide Than for (1~5): the mass ratio of (10~20), the expanded graphite and ammonium persulfate is (1~5): (5~20), the expansion stone The ratio of the volume of the quality and pyrrole monomer of ink is (1g~5g): (10mL~30mL)；

Two, intermediary material is placed in atmosphere tube type furnace, under the protection of inert gas, with 2 DEG C/min~10 DEG C/ The heating rate of min is warming up to 700 DEG C~900 DEG C, and 1h~5h is kept the temperature at 700 DEG C~900 DEG C, then cools to room temperature, Obtain nitrogen-doped carbon fiber cladding class graphene interlayer composite.

For the present invention using the method for template assemblies in situ, the crosslinking shape carbon fiber of controlledly synthesis N doping coats class graphite Alkene (NFNS) interlayer composite, interconnected nitrogen-doped carbon nano-fiber are uniformly coated on class graphene film layer surface. The unique structure of NFNS interlayer composite has the advantage that it when as electrode material for super capacitor

(1) class graphene sheet layer has preferable electric conductivity, can be used as small current-collector in charge and discharge process and accelerates The transmitting of electronics；

(2) carbon nano-fiber clad specific surface area with higher, the nitrogen-doped carbon fiber package that the present invention is prepared The specific surface area for covering class graphene interlayer composite is more than 420m²/ g is conducive to the infiltration of electrolyte, electrolyte can be improved The diffusion velocity of ion；

(3) the electroactive of electrode material surface can be improved in the doping nitrogen from PPy, generates the ratio that fake capacitance improves material Capacitor.

The present invention can get a kind of preparation method of nitrogen-doped carbon fiber cladding class graphene interlayer composite.

Detailed description of the invention

Fig. 1 is the SEM figure that nitrogen-doped carbon fiber prepared by embodiment one coats class graphene interlayer composite；

Fig. 2 is the SEM figure that nitrogen-doped carbon fiber prepared by embodiment two coats class graphene interlayer composite；

Fig. 3 is the SEM figure that nitrogen-doped carbon fiber prepared by embodiment three coats class graphene interlayer composite.

Specific embodiment