CN106222799A - A kind of double-layer nested nanofiber and preparation method thereof - Google Patents
A kind of double-layer nested nanofiber and preparation method thereof Download PDFInfo
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- CN106222799A CN106222799A CN201610628911.8A CN201610628911A CN106222799A CN 106222799 A CN106222799 A CN 106222799A CN 201610628911 A CN201610628911 A CN 201610628911A CN 106222799 A CN106222799 A CN 106222799A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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Abstract
The present invention is configured to homogeneous precursor sol liquid by polymer and the slaine of different molecular weight, high-voltage electrostatic spinning technology is used to obtain nanofiber, in conjunction with gradient heat treatment process, obtain the nano material of the adjustable inner structure of high-quality contraction, the ingenious heating rate utilizing two stages different controls the catabolic process of composite fibre, accurately and controls to be formed nested structure and the most inside pattern of bilayer easily.
Description
Technical field
The invention belongs to technical field of nanometer material preparation.
Background technology
Along with the reach of science, the structure that great research discovery microcosmic is multistage can make material have many excellent property
Matter.Due to modern synthetic technology and the development of analysis test, microcosmic nano material also experiences this and drills from simple to complicated structure
Become.And then, greatly have stimulated many science at the third generation micrometer/nanometer material having more complicated inner structure in recent years
The research interest of family, because these structures have more excellent performance.It addition, one-dimensional nano structure, because of the character of its uniqueness
Cause the broad interest of researcher, and achieve the most excellent chemical property.Electrostatic spinning tool in ownership Preparation Method
Have a clear superiority in.Device is simple, spinning is with low cost, it is various to spin substance classes, technique is controlled with its manufacture for electrostatic spinning
Advantage, it has also become effectively one of main path preparing nano-fiber material.Electrostatic spinning technique has been prepared for abundant species
Nanofiber, the compound and inorganic nano-fiber including organic, organic/inorganic.Such as, Xiang et al. is also with this technology
Synthesize CuO doughnut, and obtained the hollow Cu fiber of porous on this basis by hydrogen reduction process further
(CrystEngComm, 2011,13 (15): 4856-4860).Additionally, beading chain nanofiber, loose porous Nanowire
Dimension and Diffuse Coptosapelta shape nanofiber also have been reported.But, utilize electrostatic spinning technique to prepare nanofiber and be also faced with some need
Problem to be solved.First, in terms of preparing organic nanofibers, the natural polymer kind for electrostatic spinning the most extremely has
Limit, the research to structure of title compound and performance is the most perfect, and the application of final products is the most at the experimental stage, especially
The industrialization of these products produces and there is also bigger problem.Secondly, the performance of Static Spinning organic/inorganic composite nano fiber is not
Only relevant with the structure of nanoparticle, also with the clustered pattern of nanoparticle and synergisticing performance, the structural behaviour of polymeric matrix,
Particle is relevant with the interfacial structure performance of matrix and processing combination process etc..How to prepare and be suitable for needs, high-performance, many merits
The composite nano fiber of energy is the key of research.Additionally, the research of Static Spinning inorganic nano-fiber is substantially at initial period, nothing
Machine nanofiber has latent in multiple fields such as high temperature filtration, efficient catalytic, bioengineered tissue, photoelectric device, space flight equipment
Purposes, but, the fragility that Static Spinning inorganic nano-fiber is bigger limits its application performance and scope, therefore, exploitation tool
Have that production technology is simple, the nano material of pliability, seriality, structural integrity is technological difficulties.
Summary of the invention
In order to solve the problems referred to above, technical scheme is as follows:
The present invention is configured to homogeneous precursor sol liquid by polymer and the slaine of different molecular weight, and high-voltage electrostatic spinning obtains
Nanofiber, in conjunction with gradient heat treatment (gradient increased temperature speed and gradient temperature) process, it is thus achieved that high-quality contraction adjustable in
The inorganic nano material of structure, the ingenious heating rate utilizing two stages different controls the catabolic process of composite fibre, accurately
And control easily to be formed nested structure and the most inside pattern of bilayer.
The preparation method of described fiber, it is characterised in that:
1) weigh respectively the middle-molecular-weihydroxyethyl of the polyacrylamide of high molecular of 0.3 ~ 1.5g, 0.78 ~ 1g polyacrylamide,
The polyacrylamide of the low-molecular-weight of 0.4 ~ 0.8g, and the precipitant of the slaine of 2 ~ 3mmol and 4 ~ 7mmol is added simultaneously to 28
~ 39mL deionized water, puts it to magnetic agitation 6h in the thermostat water bath of 70 ~ 88 DEG C and makes it all dissolve, formed transparent
Solution；Slaine one in the nitrate of Mg, Al, Zn, Zr and Fe, sulfate, acetate, chloride and oxalates
Or it is multiple；In described precipitant selected from phosphoric acid, ammonium phosphate, ammonium dihydrogen phosphate, diammonium phosphate, ammonia, ammonium fluoride, ammonium carbonate,
One or more in ammonium hydrogen carbonate and oxalic acid；
2) by step 1) precursor solution joins in injection, in positive high voltage 17 ~ 20kV, the condition of negative high voltage-1.1 ~ 1.9kV
Under carry out electrostatic spinning, receive nanofiber with aluminium foil, syringe needle is adjusted to 13 ~ 18 cm with the distance receiving plate, and spinning liquid advances
Speed 1 ~ 1.5mL/h；
3) to step 2) nanofiber that obtains is positioned in 120 DEG C of baking ovens and is dried 5h；
4) by step 3) in the complex nanofiber that obtains of electrostatic spinning, under inert gas atmosphere first with 20 DEG C of min-1Hurry up
Heating rate to 380 DEG C, be incubated 1.5h, then with 2 DEG C of min-1Slow heating rate is to 550 DEG C and is incubated 4h, i.e. available by
The nested nanofiber of small nano-particle composition；
Nanofiber a length of 5～15 μm obtained, is formed by inside and outside two layer nestings, is hollow-core construction between layers, outer layer
A diameter of 200～400 nm, a diameter of the 80 of internal layer～120nm, ectonexine spacing is 40～70 nm, layer wall thickness 20～30
nm.Have more than or equal to 130m2The specific surface area of/g.
Noble gas is preferably nitrogen.Slaine is preferably selected from the nitrate of Mg, Fe, sulfate and oxalates
Plant or multiple；Selected from phosphoric acid, ammonium phosphate, ammonium dihydrogen phosphate, diammonium phosphate in described precipitant.
The Molecular Weight for Polyacrylamide of high molecular is 300 2,200 ten thousand, the Molecular Weight for Polyacrylamide of middle-molecular-weihydroxyethyl is
100-200 ten thousand, the molecular weight of polyacrylamide of low-molecular-weight are less than 1,000,000.
Owing to high, medium and low molecular weight polyisoprene propylene milling amine has different viscosity and surface tension, at the work of high-pressure electrostatic
Under with, three at nano wire in the radial direction in layered distribution, formed three coaxial configurations (i.e. high molecular outermost layer, low point
Zi Liang center, middle-molecular-weihydroxyethyl are between).But inorganic salt is uniformly distributed in nanofiber.First, electrospun nanofiber is fine
Dimension is with 20 DEG C of min-1Fast heating rate to 380 DEG C, crystalline rate Vc of inorganic salt is less than Polymer-pyrolysis speed Vp, and this will lead
Cause moving direction by internal layer outer layers, formation hollow.Then, it is incubated 1.5h at 380 DEG C, because capillary force and polymer pipe are soft
Essence will cause outer polymeric layer to shrink.Last with 2 DEG C of min-1Heating rate be heated to 550 DEG C, be incubated 4h.Because low
Heating rate under Vp more than Vc, moving direction to both sides, is formed bivalve by centre.Finally, at high temperature, inorganic matter is further
Crystallization, forms the nanostructured shunk.
Nanofiber and preparation method thereof in the present invention, compared to prior art, has a following beneficial effect:
(1) present invention has prepared the metal composite oxide nanofiber with double-layer nested structure, and inside and outside wall is the most inwardly received
Contracting, can the overall tap density improving nanofiber, footpath is distributed in narrower region, has preferable structural integrity and
Fixed magnetic；
(2) present invention is configured to homogeneous precursor sol liquid, high-voltage electrostatic spinning by polymer and the slaine of different molecular weight
Obtain nanofiber, in conjunction with gradient heat treatment (gradient increased temperature speed and gradient temperature) process, it is thus achieved that high-quality contraction can
The inorganic nano material of inner structure, the ingenious heating rate utilizing two stages different is adjusted to control the catabolic process of composite fibre,
Accurately and control to be formed the pattern of nested structure easily.
Accompanying drawing explanation
Fig. 1 is nanofiber stereoscan photograph of the present invention
Detailed description of the invention
Embodiment 1
1) weigh respectively the polyacrylamide of high molecular of 1.1g, the polyacrylamide of middle-molecular-weihydroxyethyl of 0.8g, 0.8g low
The polyacrylamide of molecular weight, and the precipitant of the slaine of 2.3mmol and 4.7mmol is added simultaneously to 2.9mL deionized water,
Putting it to magnetic agitation 6h in the thermostat water bath of 70 ~ 88 DEG C makes it all dissolve, and forms transparent solution；Slaine is selected from
Ferric nitrate；Selected from phosphoric acid in described precipitant；
2) by step 1) precursor solution joins in injection, carries out under conditions of positive high voltage 18kV, negative high voltage-1.8kV
Electrostatic spinning, receives nanofiber with aluminium foil, and syringe needle and the distance receiving plate are adjusted to 18 cm, spinning liquid fltting speed
1.4mL/h；
3) to step 2) nanofiber that obtains is positioned in 120 DEG C of baking ovens and is dried 5h；
4) by step 3) in the complex nanofiber that obtains of electrostatic spinning, under inert gas atmosphere first with 20 DEG C of min-1Hurry up
Heating rate to 380 DEG C, be incubated 1.5h, then with 2 DEG C of min-1Slow heating rate is to 550 DEG C and is incubated 4h, i.e. available by
The nested nanofiber of small nano-particle composition；
A length of 13 μm of nanofiber obtained, are formed by inside and outside two layer nestings, are hollow-core construction between layers, outer layer diameter
For 300nm, a diameter of 100nm of internal layer, ectonexine spacing is 55 nm, layer wall thickness 21 nm.
Embodiment 2
1) polyacrylamide of high molecular of 1g, the polyacrylamide of middle-molecular-weihydroxyethyl of 1g, the low molecule of 0.8g are weighed respectively
The polyacrylamide of amount, and the precipitant of the slaine of 2mmol and 5mmol is added simultaneously to 30mL deionized water, puts it to
In the thermostat water bath of 70 DEG C, magnetic agitation 6h makes it all dissolve, and forms transparent solution；Slaine is selected from magnesium chloride；Institute
State in precipitant selected from diammonium phosphate；
2) by step 1) precursor solution joins in injection, carries out under conditions of positive high voltage 18kV, negative high voltage-1.4kV
Electrostatic spinning, receives nanofiber with aluminium foil, and syringe needle and the distance receiving plate are adjusted to 15 cm, spinning liquid fltting speed 1mL/
h；
3) to step 2) nanofiber that obtains is positioned in 120 DEG C of baking ovens and is dried 5h；
4) by step 3) in the complex nanofiber that obtains of electrostatic spinning, under inert gas atmosphere first with 20 DEG C of min-1Hurry up
Heating rate to 380 DEG C, be incubated 1.5h, then with 2 DEG C of min-1Slow heating rate is to 550 DEG C and is incubated 4h, i.e. available by
The nested nanofiber of small nano-particle composition；
A length of 11 μm of nanofiber obtained, are formed by inside and outside two layer nestings, are hollow-core construction between layers, outer layer diameter
Being 255 nm, a diameter of 85nm of internal layer, ectonexine spacing is 48nm, layer wall thickness 25nm.
Comparative example 1
1) polyvinyl alcohol of high molecular of 1g, the polyvinyl alcohol of middle-molecular-weihydroxyethyl of 0.75g, the low molecule of 0.35g are weighed respectively
The polyvinyl alcohol molecule amount of amount, and the four water manganese acetates of the four water cobalt acetates of 1.5mmol and 3mmol are added simultaneously to 20mL
Ionized water, puts it to magnetic agitation 6h in the thermostat water bath of 80 DEG C and makes it all dissolve, form transparent solution；
2) by step 1) precursor solution joins in injection, carries out quiet under conditions of positive high voltage 15kV, negative high voltage-2kV
Electrospun, receives nanofiber with aluminium foil；
3) to step 2) nanofiber that obtains is positioned in 120 DEG C of baking ovens and is dried 5h；
4) by step 3) in the complex nanofiber that obtains of electrostatic spinning, in air atmosphere first with 1 DEG C of min-1Slow liter
Temperature speed to 280 DEG C, is incubated 1h, then with 10 DEG C of min-1Fast heating rate is to 500 DEG C and is incubated 3h, i.e. available by small
The nanofiber of contraction of nano-particle composition.
Comparative example 2
(1) Mn (NO3) the 2 solution addition weighing 0.4000g Fe2 (SO4) 3 and 0.36g 50wt% respectively fills 6 mL DMF's
In beaker, stirring, until all dissolving the solution obtaining clear homogeneous, adds 1g PVP, mixing and stirring, obtains transparent
The spinning solution of thickness；
(2) spinning solution prepared by step (1) is poured into carry out with in the syringe of the rustless steel syringe needle that external diameter is 0.8 mm
Electrostatic spinning, controls indoor temperature and relative humidity respectively at 15 DEG C and about 35%, and syringe needle and the distance receiving plate are adjusted to
20 cm, spinning liquid fltting speed is 0.9 mL/h, and the voltage of electrostatic spinning process is 16 kV, uses reception plate to collect and obtains ferrum
Manganese slaine and the composite nano fiber of polyvinylpyrrolidone；
(3) composite fibre prepared by step (2) being carried out calcine by steps, the first stage, with the heating rate of 1 DEG C/min, is warming up to
250 DEG C, second stage is warming up to 600 DEG C from 250 DEG C, use 10 DEG C/min heating rate, temperature retention time is 4 h, then with
Stove is cooled to room temperature, i.e. obtains ferrum-manganese metal composite oxide magnetic Nano fiber.
Material prepared by the present invention is as active substance, according to active substance: acetylene black: graphene oxide (binding agent)
Mass ratio be 7:2.5:0.5.In view of the dual pathways process (ion and electronics) of electrode reaction with preferably play its structure
Advantage, graphene oxide is used to replace the adhesive of insulation, and only accounting for the 5% of whole electrode but can increase the electrical conductivity of electrode.
First active substance is sufficiently mixed with acetylene black, is simultaneously introduced appropriate isopropanol and grinds uniformly, be eventually adding graphite oxide
Alkene makes active substance be bonded together with acetylene black.Then on twin rollers, mixture is pressed into diaphragm in uniform thickness, then cuts
It is cut in the same size, area and is about 0.8cm2Small pieces, put in the baking oven of 70 DEG C be dried 24h.With the diaphragm after tabletting for just
Pole, metal lithium sheet be negative pole, stainless (steel) wire be collector, shell is CR2016 type battery case, and diaphragm paper is that Celgard2400 is micro-
Hole polypropylene screen, electrolyte is ethylene carbonate (EC)/dimethyl carbonate (the DMC) (VEC:VDMC=of 1.0mol/LLiPF6
1:1) solution, assembles lithium ion battery in the glove box (moisture Control is at below 8ppm) of full argon and seals, by made
Standby battery standing just can carry out electrochemical property test after one day.
Average size under the different electric current density of table 1
Test result indicate that the present invention has the high rate performance of excellence.
Cycle performance under the electric current density of table 2 200mA g-1, after 140 times circulate, discharge capacity 200mA g-1's
Cycle performance under electric current density-1 -1
| Embodiment 1 | Embodiment 2 | Comparative example 1 | Comparative example 2 | |
| Discharge capacity (mAh/g) | 938 | 940 | 924 | 925 |
Claims (5)
1. a double-layer nanometer fiber, it is characterised in that: fiber has inside and outside two-layer.
2. the preparation method of fiber as claimed in claim 1, it is characterised in that:
1) weigh respectively the high molecular weight polyacrylamide of 0.3 ~ 1.5g, the middle-molecular-weihydroxyethyl polyacrylamide of 0.78 ~ 1g, 0.4 ~
The low molecular weight polyacrylamide of 0.8g, and the precipitant of the slaine of 2 ~ 3mmol and 4 ~ 7mmol is added simultaneously to 28 ~ 39mL
Deionized water, puts it to magnetic agitation 6h in the thermostat water bath of 70 ~ 88 DEG C and makes it all dissolve, form transparent solution；
One or more in the nitrate of Mg, Al, Zn, Zr and Fe, sulfate, acetate, chloride and oxalates of slaine；
Selected from phosphoric acid, ammonium phosphate, ammonium dihydrogen phosphate, diammonium phosphate, ammonia, ammonium fluoride, ammonium carbonate, ammonium hydrogen carbonate in described precipitant
With one or more in oxalic acid；
2) by step 1) precursor solution joins in injection, in positive high voltage 17 ~ 20kV, the condition of negative high voltage-1.1 ~ 1.9kV
Under carry out electrostatic spinning, receive nanofiber with aluminium foil, syringe needle is adjusted to 13 ~ 18 cm with the distance receiving plate, and spinning liquid advances
Speed 1 ~ 1.5mL/h；
3) to step 2) nanofiber that obtains is positioned in 120 DEG C of baking ovens and is dried 5h；
4) by step 3) in the complex nanofiber that obtains of electrostatic spinning, under inert gas atmosphere first with 20 DEG C of min-1Fast
Heating rate to 380 DEG C, is incubated 1.5h, then with 2 DEG C of min-1Slow heating rate is to 550 DEG C and is incubated 4h, i.e. available by micro-
The nested nanofiber of little nano-particle composition；
Nanofiber a length of 5～15 μm obtained, is formed by inside and outside two layer nestings, is hollow-core construction between layers, outer layer
A diameter of 200～400 nm, a diameter of the 80 of internal layer～120nm, ectonexine spacing is 40～70 nm, layer wall thickness 20～30
nm。
3. preparation method as claimed in claim 2, it is characterised in that: noble gas is nitrogen.
4. preparation method as claimed in claim 2, it is characterised in that: slaine selected from the nitrate of Mg, Fe, sulfate and
One or more in oxalates；Selected from phosphoric acid, ammonium phosphate, ammonium dihydrogen phosphate, diammonium phosphate in described precipitant.
5. preparation method as claimed in claim 2, it is characterised in that: the fiber ectonexine wall prepared, all to contract, has
More than or equal to 130m2The specific surface area of/g.
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| CN201810284958.6A CN108301070A (en) | 2016-08-03 | 2016-08-03 | A kind of preparation method of double-layer nested nanofiber |
| CN201810594833.3A CN108728935A (en) | 2016-08-03 | 2016-08-03 | A kind of metal composite oxide nanofiber |
| CN201610628911.8A CN106222799B (en) | 2016-08-03 | 2016-08-03 | A kind of double-layer nested nanofiber and preparation method thereof |
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| CN201610628911.8A CN106222799B (en) | 2016-08-03 | 2016-08-03 | A kind of double-layer nested nanofiber and preparation method thereof |
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| CN201810284958.6A Division CN108301070A (en) | 2016-08-03 | 2016-08-03 | A kind of preparation method of double-layer nested nanofiber |
| CN201810594833.3A Division CN108728935A (en) | 2016-08-03 | 2016-08-03 | A kind of metal composite oxide nanofiber |
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| CN201810594833.3A Pending CN108728935A (en) | 2016-08-03 | 2016-08-03 | A kind of metal composite oxide nanofiber |
| CN201610628911.8A Active CN106222799B (en) | 2016-08-03 | 2016-08-03 | A kind of double-layer nested nanofiber and preparation method thereof |
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| CN106731229A (en) * | 2016-12-30 | 2017-05-31 | 东华大学 | Possesses electret nano-fiber air filter material of water-proof function and preparation method thereof |
| CN106731229B (en) * | 2016-12-30 | 2019-01-15 | 东华大学 | The electret nano-fiber air filter material and preparation method thereof for having water-proof function |
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| CN108728935A (en) | 2018-11-02 |
| CN108301070A (en) | 2018-07-20 |
| CN106222799B (en) | 2018-09-21 |
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