CN104674383A - Carbon nano fiber aerogel electrostatic spinning construction method - Google Patents
Carbon nano fiber aerogel electrostatic spinning construction method Download PDFInfo
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- CN104674383A CN104674383A CN201510074631.2A CN201510074631A CN104674383A CN 104674383 A CN104674383 A CN 104674383A CN 201510074631 A CN201510074631 A CN 201510074631A CN 104674383 A CN104674383 A CN 104674383A
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Abstract
The invention provides a carbon nano fiber aerogel electrostatic spinning construction method, and belongs to the technical field of nano materials. The carbon nano fiber aerogel electrostatic spinning construction method particularly comprises the following steps: (a) preparing an electrostatic spinning solution; (b) selecting a proper solvent and directly receiving electrostatic spinning nano fibers so as to obtain a nano fiber solution; (c) sizing the nano fiber solution, refrigerating, putting into a freeze dryer and drying so as to obtain nano fiber aerogel; and (d) pre-oxidizing, carbonizing and activating so as to obtain the carbon nano fiber aerogel. The carbon nano fiber aerogel electrostatic spinning construction method not only is simple and feasible, is good in repeatability, but also the prepared carbon nano fiber aerogel is easy to control in formation and structure; the composite carbon nano fiber aerogel with diversified structures can be constructed so as to meet different requirements in practical application.
Description
Technical field
The present invention relates to technical field of nano material, particularly relate to the electrostatic spinning construction method of carbon nano-fiber aeroge.
Background technology
Carbon aerogels is a kind of novel light nano-porous materials first found by U.S. Pekblb, its basic characteristics are that porosity is high, specific area is large and variable density scope is wide, has property, have a wide range of applications in electricity, calorifics and optics etc.Such as super capacitor, catalyst carrier, hydrogen storage material, electrode material, absorbent and detector etc. can be used as.Wherein light weight and the carbon aerogels containing doping have great application prospect especially.Such as, the graphene-structured of ultralight N doping is used as absorbent and electrode of super capacitor, shows great absorptive capacity and special electric capacity.The carbon aerogels of doping metals has higher hydrogen storage performance.
Prior art discloses the multiple method preparing carbon aerogels, but the carbon aerogels that most methods is difficult to one-step method, simple preparation contains various ingredients doping, and be not easy to the structure of carbon aerogels.Therefore, limit more that it is applied widely.
Electrospun nano-fibers is by making high-pressure electrostatic on polymer solution band, and when electric field force is enough large, polymer drop overcomes surface tension and forms injection thread, polymer jet slenderizing, bending, splitting simultaneously, solvent evaporation or solidification, be deposited on dash receiver and form nanofiber.Various ingredients can be integrated in same fiber by Electrospun nano-fibers technology jointly, thus prepares composite nano fiber, can realize the preparation of polymer/polymer, polymer/inorganic thing and inorganic matter/inorganic matter composite fibre.In addition, by changing preparation parameter (as changed nozzle structure, Control release condition etc.), electrostatic spinning technique can prepare the nano-fiber material (as solid, hollow, the superfine fibre of nucleocapsid structure or the two-dimensional fiber film etc. of spider reticulation structure) of various structures.At present, most of electrostatic spinning technique is using metal material as receiver.Therefore, institute is generally nano fibrous membrane, and obtain nanofiber solution must be distributed to nano fibrous membrane in appropriate solvent again.This is not only consuming time, and tunica fibrosa is difficult to be uniformly dispersed, and in dispersion, be easy to fracture.
Summary of the invention
Solve in current carbon aerogels preparation method, be difficult to one-step method, simple preparation multi-component doped, the technical problem of the carbon aerogels of structure-controllable, the present invention discloses a kind of electrostatic spinning construction method of carbon nano-fiber aeroge, the method simply, fast can prepare multicomponent, and the carbon nano-fiber aeroge of structure diversification, significantly improves the performance of carbon nano-fiber aeroge, meet different demand in reality, expand its application prospect.
In order to achieve the above object, the following steps of the present invention's employing:
Step a) preparation electrostatic spinning liquid;
Step b) selects suitable solvent directly to receive Electrospun nano-fibers, obtains nanofiber solution;
Step c), by freezing for the sizing of nanofiber solution, be then placed in freeze drier dry, obtain nanofiber aeroge;
Described nanofiber aeroge is carried out pre-oxidation, carbonization and activation by step d), obtains carbon nano-fiber aeroge.
advantage of the present invention is
1) directly receive Electrospun nano-fibers with suitable solvent, achieve one-step method and obtain disperseing homogeneous nanofiber solution, and nanofiber can not rupture, and keeps good continuity, be conducive to improving carbon nano-fiber aeroge performance.
2) the carbon nano-fiber aeroge prepared of this method, its raw material sources are extensive, and can be not only macromolecular material, also can be multiple organic/inorganic composite material.
3) the carbon nano-fiber aeroge prepared of this method, its nanofiber is prepared from by electrostatic spinning technique.Therefore, various ingredients can be integrated in jointly in same fiber easily, thus prepare composite nano fiber, effectively improve carbon nano-fiber aeroge performance.
4) the carbon nano-fiber aerogel structure prepared of this method controlled (as fiber whether hollow, fibre diameter, specific area and density etc.), therefore according to different demand, can prepare the carbon nano-fiber aeroge of optimum structure.
Accompanying drawing explanation
Fig. 1 is under embodiment one condition, the optical picture of carbon nano-fiber aeroge.
Fig. 2 is under embodiment one condition, the scanning electron microscope (SEM) photograph (SEM) of carbon nano-fiber aeroge.
Detailed description of the invention
Now the present invention is further described with detailed description of the invention by reference to the accompanying drawings.
Embodiment one
1) preparation of spinning solution: fine (PAN) powder of polypropylene and the 0.3 g graphene oxide (GO) that take 2 g, join in the 100 mL conical flasks containing 20 g dimethyl formamide (DMF) solvents, be placed in 60 DEG C of water-bath heating and be stirred to dissolving, be configured to PAN-GO mixed solution.
2) preparation of nanofiber: the Electrospun liquid in step 1) is placed in 10 ml syringes, collects nanofiber using the plastic containers be filled with water as the receiver of nanofiber.Spinning parameter is: voltage 15 kV, spinning nozzle internal diameter 0.6 mm, spinning solution flow velocity 0.9 mL/h, spinning head is 15 cm to the distance of the reception water surface, time of reception 3 h, environmental condition: temperature 30 ± 5 DEG C, relative humidity 50 ± 5%, receiver moves around speed 0.5 cm/s.
3) preparation of nanofiber aeroge: by the nanofiber solution of the collection in step 2, according to desired density and shape, shape, is then placed in-4 DEG C of refrigerator and cooled and freezes 5 h; Then the nanofiber of freeze forming is placed in dry 2 d of freeze drier, obtains nanofiber aeroge.
4) preparation of carbon nano-fiber aeroge: the nanofiber aeroge in step 3 is placed in 280 DEG C of baking ovens, pre-oxidation 60 min; Then in tubular type Muffle furnace, at N
2with after the ramp to 600 of, 5 DEG C/min DEG C under protection, keep 0.5 h; Then again with the ramp to 900 DEG C of 5 DEG C/min, at CO
2under environment, activate 0.5 h, finally cool to room temperature with the speed of 5 DEG C/min, obtain the carbon nano-fiber aeroge containing Graphene.
5) the capacitive property test of carbon nano-fiber aeroge: using the carbon nano-fiber aeroge in step 4 as working electrode.Make reference electrode with Ag/AgCl electrode, platinum filament is done electrode, in 1 mol/L KOH electrolyte, adopts classical three-electrode system, carries out cyclic voltammetric and charge-discharge test at electrochemical workstation.
Embodiment two
1) preparation of spinning solution: fine (PAN) powder of polypropylene and the 0.1 g iron chloride (FeCl that take 2 g
3), join in the 100 mL conical flasks containing 20 g dimethyl formamide (DMF) solvents, be placed in 60 DEG C of water-bath heating and be stirred to dissolving, be configured to PAN-FeCl
3mixed solution.
2) preparation of nanofiber: the Electrospun liquid in step 1) is placed in 10 ml syringes, collects nanofiber using the plastic containers be filled with water as the receiver of nanofiber.Spinning parameter is: voltage 15 kV, spinning nozzle internal diameter 0.6 mm, spinning solution flow velocity 0.9 mL/h, spinning head is 15 cm to the distance of the reception water surface, time of reception 3 h, environmental condition: temperature 30 ± 5 DEG C, relative humidity 50 ± 5%, receiver moves around speed 0.5 cm/s.
3) preparation of nanofiber aeroge: by the nanofiber solution of the collection in step 2, according to desired density and shape, shape, is then placed in-4 DEG C of refrigerator and cooled and freezes 5 h; Then the lumps of nanofibers of freeze forming is placed in freeze drier and carries out dry 2 d, obtain nanofiber aeroge.
4) preparation of carbon nano-fiber aeroge: the nanofiber aeroge in step 3 is placed in tubular type Muffle furnace, at N
2with after the ramp to 600 of, 5 DEG C/min DEG C under protection, keep 0.5 h; Then again with the ramp to 800 DEG C of 5 DEG C/min, under water vapor atmosphere, activate 0.5 h, finally cool to room temperature with the speed of 3 DEG C/min, obtain the carbon nano-fiber aeroge of doping iron.
5) the capacitive property test of carbon nano-fiber aeroge: using the carbon nano-fiber aeroge in step 4 as working electrode.Make reference electrode with Ag/AgCl electrode, platinum filament is done electrode, in 1 mol/L KOH electrolyte, adopts classical three-electrode system, carries out cyclic voltammetric and charge-discharge test at electrochemical workstation.
Although specifically show in conjunction with preferred embodiment and describe the present invention; but those skilled in the art should be understood that; not departing from the spirit and scope of the present invention that appended claims limits; can make a variety of changes the present invention in the form and details, be protection scope of the present invention.
Claims (7)
1. the electrostatic spinning construction method of carbon nano-fiber aeroge, is characterized in that comprising the following steps:
Step a) preparation electrostatic spinning liquid;
Step b) selects suitable solvent directly to receive Electrospun nano-fibers, obtains nanofiber solution;
Step c), by freezing for the sizing of nanofiber solution, be then placed in freeze drier dry, obtain nanofiber aeroge;
Described nanofiber aeroge is carried out pre-oxidation, carbonization and activation by step d), obtains carbon nano-fiber aeroge.
2. the electrostatic spinning construction method of the carbon nano-fiber aeroge as described in claim 1, is characterized in that the electrostatic spinning liquid in described step a) comprises polymer solution, inorganic solution, polymer/inorganic thing composite solution; Its polymer solution comprises polyacrylonitrile, polyamide, Merlon, polyurethane, urethaneureas, polyvinyl chloride, Kynoar, polyethylene terephthalate, polybutylene terephthalate (PBT), polystyrene, poly-methyl methacrylate acid, one or more mixtures wherein such as polysulfones and polyether sulfone, and it is polymer-modified etc.; Inorganic matter comprises CNT, graphene oxide, Graphene, nano particle and nano particle precursor etc.
3. the electrostatic spinning construction method of carbon nano-fiber aeroge as claimed in claim 1, it is characterized in that the concrete steps of described step b) are, according to the physicochemical properties of institute's spinning nano fibre, select appropriate solvent to be placed in receiving vessel, one-step method forms nanofiber solution; Wherein solvent comprises water, ethanol, organic solvent, and their mixed solution etc.
4. the electrostatic spinning construction method of carbon nano-fiber aeroge as claimed in claim 1, it is characterized in that the concrete steps of described step c) are, the nanofiber solution fully disperseed is placed in freezing 10 ~ 60 min of liquid nitrogen, or be put in-4 ~-20 DEG C of refrigerator and cooled and freeze 1 ~ 12 h, then the nanofiber of sizing is placed in dry 1 ~ 3 d of freeze drier, obtains nanofiber aeroge.
5. the electrostatic spinning construction method of carbon nano-fiber aeroge as claimed in claim 1, is characterized in that the concrete steps of described step d) are, are placed in 180 ~ 350 DEG C of baking ovens by described nanofiber aeroge, pre-oxidation 10 ~ 120 min; Then, in Muffle furnace, with behind ramp to 500 ~ 700 of, 1 ~ 8 DEG C/min DEG C under inert gas shielding, 0.5 ~ 3 h is kept; Then again with ramp to 750 ~ 1200 DEG C of 1 ~ 8 DEG C/min, under the condition of active gases, activation 0.5 ~ 3 h; Finally be cooled to room temperature with the speed of 1 ~ 5 DEG C/min, obtain carbon nano-fiber aeroge.
6. the electrostatic spinning construction method of carbon nano-fiber aeroge as claimed in claim 1, it is characterized in that to add the material with strong mechanical performance in the nanofiber solution in step b), or crosslinking agent is carried out to nanofiber, to strengthen the mechanical strength of carbon nano-fiber aeroge.
7. the electrostatic spinning construction method of carbon nano-fiber aeroge as claimed in claim 1, is characterized in that can be used for preparing carrier material, sorbing material, hydrogen storage material, capacitance material, electrode material and pressure sensor etc.
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Cited By (18)
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|---|---|---|---|---|
| CN104882588A (en) * | 2015-06-08 | 2015-09-02 | 中国工程物理研究院化工材料研究所 | Carbon fiber/carbon nanotube composite membrane as well as preparation method and application thereof |
| CN105161312A (en) * | 2015-09-24 | 2015-12-16 | 复旦大学 | Carbon nano fiber-graphene composite aerogel and cooperative assembly preparation method thereof |
| CN105304876A (en) * | 2015-10-25 | 2016-02-03 | 复旦大学 | Molybdenum sulfide/graphene/carbon nano fiber composite material and preparation method thereof |
| CN105923622A (en) * | 2016-05-10 | 2016-09-07 | 复旦大学 | Polyacrylonitrile nanofiber/polyimide-based carbon aerogel adsorption material and preparation method thereof |
| CN106345053A (en) * | 2016-08-23 | 2017-01-25 | 孟玲 | Electrostatic releaser |
| CN106552674A (en) * | 2016-09-28 | 2017-04-05 | 扬州云彩新材料科技有限公司 | Aerogel carried nickel-phosphorus alloy catalysis material of a kind of nanofiber and preparation method thereof |
| CN106567157A (en) * | 2016-08-17 | 2017-04-19 | 重庆大学 | Preparation method of graphene nanoribbon in situ toughened nano carbon fiber |
| CN106637490A (en) * | 2016-09-21 | 2017-05-10 | 东莞市联洲知识产权运营管理有限公司 | Porous conductive antibacterial fiber on basis of graphene and chitosan oligosaccharides and method for preparing porous conductive antibacterial fiber |
| CN106854779A (en) * | 2016-12-15 | 2017-06-16 | 华南理工大学 | A kind of carbon nano-tube oriented enhanced carbon fibre composite and preparation method thereof |
| CN106977763A (en) * | 2017-04-20 | 2017-07-25 | 哈尔滨工业大学 | A kind of preparation method of aramid nano-fiber aeroge |
| CN108328595A (en) * | 2017-01-20 | 2018-07-27 | 中国科学院物理研究所 | A kind of carbon aerogels and preparation method thereof and pressure sensor |
| CN108385127A (en) * | 2018-02-14 | 2018-08-10 | 中氧科技（广州）有限公司 | A kind of preparation method for the modification lead dioxide membrane electrode generating ozone |
| CN108404823A (en) * | 2018-05-11 | 2018-08-17 | 江南大学 | A kind of electrostatic spinning prepares the method and its resulting materials of high water absorption 3D nanofiber aeroges |
| CN108840656A (en) * | 2018-04-26 | 2018-11-20 | 东华大学 | One kind being based on Static Spinning SiO2Nanofiber aerogel heat-insulating material and its preparation and application |
| CN109056122A (en) * | 2018-07-04 | 2018-12-21 | 吉林农业大学 | A method of tool three-dimensional structure nanofiber aerogel material is prepared by electrostatic spinning |
| CN110204776A (en) * | 2019-06-05 | 2019-09-06 | 东华大学 | A kind of polyvinylidene fluoride nanometer fiber aerogel material and preparation method thereof |
| WO2020224431A1 (en) * | 2019-05-07 | 2020-11-12 | 清华大学 | Aeolotropic layered carbon-fiber-based aerogel material and preparation method therefor |
| CN115193348A (en) * | 2022-07-20 | 2022-10-18 | 天津工业大学 | Dynamic receiving device for continuous nanofiber and preparation method for constructing nanofiber aerogel by using dynamic receiving device |
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| CN105304876A (en) * | 2015-10-25 | 2016-02-03 | 复旦大学 | Molybdenum sulfide/graphene/carbon nano fiber composite material and preparation method thereof |
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| CN106567157A (en) * | 2016-08-17 | 2017-04-19 | 重庆大学 | Preparation method of graphene nanoribbon in situ toughened nano carbon fiber |
| CN106567157B (en) * | 2016-08-17 | 2022-03-08 | 重庆大学 | Preparation method of graphene nanoribbon in-situ toughening carbon nanofibers |
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| CN108328595A (en) * | 2017-01-20 | 2018-07-27 | 中国科学院物理研究所 | A kind of carbon aerogels and preparation method thereof and pressure sensor |
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| CN108404823A (en) * | 2018-05-11 | 2018-08-17 | 江南大学 | A kind of electrostatic spinning prepares the method and its resulting materials of high water absorption 3D nanofiber aeroges |
| CN108404823B (en) * | 2018-05-11 | 2021-01-05 | 江南大学 | Method for preparing high-water-absorption 3D nanofiber aerogel through electrostatic spinning and material obtained through method |
| CN109056122A (en) * | 2018-07-04 | 2018-12-21 | 吉林农业大学 | A method of tool three-dimensional structure nanofiber aerogel material is prepared by electrostatic spinning |
| WO2020224431A1 (en) * | 2019-05-07 | 2020-11-12 | 清华大学 | Aeolotropic layered carbon-fiber-based aerogel material and preparation method therefor |
| CN110204776A (en) * | 2019-06-05 | 2019-09-06 | 东华大学 | A kind of polyvinylidene fluoride nanometer fiber aerogel material and preparation method thereof |
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Application publication date: 20150603 |