CN107699965B - Right-angled intersection stacks nanofiber array preparation method - Google Patents

Right-angled intersection stacks nanofiber array preparation method Download PDF

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Publication number
CN107699965B
CN107699965B CN201710801174.1A CN201710801174A CN107699965B CN 107699965 B CN107699965 B CN 107699965B CN 201710801174 A CN201710801174 A CN 201710801174A CN 107699965 B CN107699965 B CN 107699965B
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spinning
electrodes
nanofiber
angled intersection
stacks
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CN107699965A (en
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陈东
陈然
孙泽勇
孔琳琳
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Nanjing Beier Times Technology Co.,Ltd.
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Zhejiang University ZJU
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0076Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0092Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Nonwoven Fabrics (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

The invention discloses a kind of right-angled intersections to stack nanofiber array preparation method.This method realizes the preparation of the oriented nanofiber array of two dimension in conjunction with dedicated spinning substrate by electrostatic spinning apparatus spraying polymer solution.By changing the direction of an electric field of substrate, the direction of every layer of nanofiber array can control, so that preparing right-angled intersection stacks nanofiber;By the adjustment to solution parameter and operating parameter, the diameter of nanofiber and the density of every layer of nanofiber can control.

Description

Right-angled intersection stacks nanofiber array preparation method
Technical field
The present invention relates to electrostatic spinning fields, and the preparation side of nanofiber array is stacked more particularly, to a kind of right-angled intersection Method.
Background technique
In recent years, nanofiber has been to be concerned by more and more people, and nanofiber has large specific surface area, light-weight, machine The features such as tool performance is good, before there is wide application in fields such as filtering material, protective materials, biomedicine, micro-nano sensors Scape.The method for preparing nanofiber is varied, and method of electrostatic spinning prepares nanofiber with controllability is good, continuity is strong, can It prepares continuous nanofiber, the advantages that required equipment is simple, is to prepare nanofiber at present by the favor of numerous researchers Most efficient method.
To realize the industrial applications of Electrospun nano-fibers, it has to be possible to rapidly, continuously prepare uniform, desirable To the nanofiber of arrangement, but electrostatic spinning is typically only capable to obtain that random direction is curved, the continuous nonwoven mat structure of fiber, and Generally existing Beads;Spun fibre diameter is not of uniform size simultaneously;Non-polar polymer solution must be mixed in the solution Miscellaneous conducting nanoparticles.In recent years, some researchs are by changing receiver architecture, to change field distribution to obtain partial zones The directional fiber in domain, however its directional fiber preparative capacibility is still very limited, it is difficult to micro-nano is prepared between specific location point Fiber.
Summary of the invention
The purpose of the present invention is to provide the preparation methods that a kind of right-angled intersection stacks nanofiber array.Utilize Static Spinning Silk and dedicated spinning reception device, by changing direction of an electric field, realization quickly and efficiently prepares right-angled intersection and stacks nanofiber Array can more accurately control the diameter of nanofiber by the adjustment to solution parameter and operating parameter.
To achieve the above object, the present invention the following technical schemes are provided:
The present invention discloses a kind of right-angled intersection stacking nanofiber array preparation method, the specific steps of this method first It is as follows:
1) at room temperature, polymer is added in prepared solvent, is stirred to obtain spinning solution;
2) dedicated spinning reception substrate is mounted on electrostatic spinning apparatus, the dedicated spinning receive substrate by PCB substrate, two pairs of electrodes composition, two pairs of electrodes are arranged in PCB substrate and two pairs of electrodes are located at horizontal and vertical two Direction;And be grounded two electrodes of horizontal direction, two electrodes of vertical direction connect high voltage power supply;Then spinning nozzle is pacified Make the electrode of vertical some ground connection of face in its front end loaded on the height of spinning nozzle and position on bracket, is adjusted, after spinning nozzle End is connected by conduit with syringe pump, and spinning nozzle conductive part taps high-voltage DC power supply;
3) spinning solution is fed by syringe pump, adjusts high-voltage DC power supply voltage, start spinning in the horizontal direction;
4) after horizontal direction spinning, then two electrodes of vertical direction are grounded, two electrodes of horizontal direction High voltage power supply is connect, then repeatedly step 3), in vertical direction spinning.
5) it repeats step 3) and stacks nanofiber array with right-angled intersection 4), finally can be obtained.
Preferably, polymer described in the polymer solute requires to be uniformly dissolved at room temperature, has certain glue Degree, such as polyoxyethylene (PEO), nylon (PA), polyurethane (PU), polylactic acid (PLLA), polystyrene (PS), polyvinyl alcohol (PVA), poly lactide-glycolide acid (PLGA), polylactide (PLA), polycaprolactone (PCL), Kynoar (PVDF), polymethyl methacrylate (PMMA), polyvinylpyrrolidone (PVP) etc. can be used single poly- according to functional requirement Object or mixed polymer are closed, natural polymer or inorganic matter can also be used.
Preferably, the viscosity of the spinning solution is 0.1~2.0Pas.
Preferably, the spinning process specifically: spinning receives a pair of electrodes ground connection in substrate, perpendicular direction Another pair electrode connect high potential, only this in ground connection is formed between electrode between movement electrode and at this electric field induction fiber To array.
Solvent requirement of the present invention can dissolve selected polymer solute, preferred to require at normal temperature easily quickly Volatilization.Dimethylformamide (DMF), tetrahydrofuran (THF) organic solvent can such as be selected.
In the step 3) and 4) in, pass through parameter (viscosity, surface tension, electric conductivity etc.) to spinning solution and behaviour Make parameter (voltage, the spacing of spray head and collecting board, spinning solution feed speed), controls the diameter and every layer of nanofiber of fiber Density.
The invention also discloses a kind of right-angled intersections that the method is prepared to stack nanofiber array.
Beneficial effects of the present invention are as follows:
(1) preparation that nanoscale criss-cross construction stacks nanofiber array may be implemented in the present invention, using cross Intersect to stack and form regular array, the new material with ordered micro-configuration can be prepared;
(2) equipment therefor of the present invention is simple and realizes automation, can at a high speed, continuously prepare right-angled intersection and stack nanometer Fiber array;
(3) structure of the invention parameter controllability is good, can control the diameter of fiber and the density of every layer of nanofiber, preparation The material of different function.
Detailed description of the invention
Fig. 1 is that right-angled intersection stacks nanofiber array structural schematic diagram.
Fig. 2 is electrostatic spinning apparatus structural schematic diagram.
Fig. 3 is dedicated spinning reception device structural schematic diagram.
In figure: 1, nanofiber, 2, copper electrode, 3, PCB substrate, 4, spinning nozzle, 5, high-voltage DC power supply.
Fig. 4 is that right-angled intersection stacks nanofiber array preparation process schematic diagram.
Specific embodiment
It names embodiment and illustrates the present invention, but the present invention is not limited to following embodiments.
Referring to attached drawing 1, nanofiber array is stacked using the method for the present invention preparation right-angled intersection, the specific steps are as follows:
1) present invention realizes that right-angled intersection stacks nanofiber array by solution injection and dedicated spinning reception device Preparation.As shown in Fig. 2, solution injection apparatus is made of spinning nozzle 4, high-voltage DC power supply 5;As shown in figure 3, spinning receives dress It sets and is made of copper electrode 2, PCB substrate 3, two pairs of copper electrode vertical distributions are in PCB substrate;
2) at room temperature, polymer is added in prepared solvent, is stirred to obtain spinning solution;
3) it is as shown in Figure 4 to stack nanofiber array preparation process for right-angled intersection.Two electrodes of horizontal direction are grounded, Two electrodes of vertical direction meet high potential U;Then spinning nozzle is installed on bracket, adjusts height and the position of spinning nozzle The electrode for making the vertical face left side ground in its front end is set, spinning nozzle rear end is connected by conduit with syringe pump, and spinning nozzle is led Electric part connects high-voltage DC power supply 5.
4) it adjusts high-voltage DC power supply voltage and high-voltage potential is provided, generate the electrode surface by being directed toward ground connection by spinning nozzle Electric field;Then spinning solution is fed to spinning nozzle by syringe pump, and take at spinning nozzle charge along electric field line to The right electrodes of ground connection are mobile, meanwhile, constantly volatilization causes solute to solidify to solvent in the sky, the nanofiber charged, In Nanofiber moves to the moment of right electrodes, since nanofiber charges, the electrode moment electrification contacted with nanofiber, So that electric field deflects, nanofiber is caused to move to the left;And so on, water can be formed between two electrodes in left and right Flat nanofiber array.
5) after horizontal direction spinning.Two electrodes of vertical direction are grounded again, two electrodes of horizontal direction High potential U is met, then repeatedly step 4), in vertical direction spinning.
6) it repeats step 4) and stacks nanofiber array with right-angled intersection 5), finally can be obtained.
Embodiment 1:
1) at room temperature, dimethylformamide (DMF) is mixed as solvent, so with tetrahydrofuran (THF) using mass ratio 1:1 Polyurethane (PU) particle, which is added in solvent, afterwards makes its mass fraction 20%-30%, then is obtained with magnetic stirrer 2 hours To spinning solution;
2) height and the position for adjusting spinning nozzle make the electrode of the vertical face left side ground in its front end, spinning nozzle rear end It is connected by conduit with syringe pump, spinning nozzle conductive part taps high-voltage DC power supply 5;Then by two electrodes of horizontal direction Ground connection, two electrodes of vertical direction meet high potential U, about 1-3KV,
3) adjusting high-voltage DC power supply is 10-15KV or so, is then fed by syringe pump with the speed of 0.2-0.8ml/h Spinning solution, solution take charge at spinning nozzle and move along electric field line to the right electrodes of ground connection, meanwhile, solvent is in the sky Constantly volatilization causes solute to solidify, and the nanofiber charged moves to the moment of right electrodes in nanofiber, due to Nanofiber electrification, the electrode moment electrification contacted with nanofiber, so that electric field deflects, leads to nanofiber to the left It is mobile;
4) after every layer of spinning 1min, switch direction of an electric field: two electrodes of vertical direction being grounded, two of horizontal direction Electrode meets high potential U, carries out spinning in vertical direction.
5) step (4) and (5) are repeated, is superimposed 120 layers, obtain the polyurethane nanofiber array of right-angled intersection stacking, institute The diameter for obtaining fiber is about 1um, and the spacing between fiber is 5-10um.
Embodiment 2:
1) at room temperature, dimethylformamide (DMF) is mixed as solvent, so with tetrahydrofuran (THF) using mass ratio 1:1 Poly lactide-glycolide acid (PLGA), which is added in solvent, afterwards makes its mass fraction 25%-35%, then uses electromagnetic agitation Device stirs 2 hours and obtains spinning solution;
2) height and the position for adjusting spinning nozzle make the electrode of the vertical face left side ground in its front end, spinning nozzle rear end It is connected by conduit with syringe pump, spinning nozzle conductive part taps high-voltage DC power supply 5;Then by two electrodes of horizontal direction Ground connection, two electrodes of vertical direction meet high potential U, about 1-3KV,
3) adjusting high-voltage DC power supply is 10-15KV or so, is then fed by syringe pump with the speed of 0.2-0.8ml/h Spinning solution, solution take charge at spinning nozzle and move along electric field line to the right electrodes of ground connection, meanwhile, solvent is in the sky Constantly volatilization causes solute to solidify, and the nanofiber charged moves to the moment of right electrodes in nanofiber, due to Nanofiber electrification, the electrode moment electrification contacted with nanofiber, so that electric field deflects, leads to nanofiber to the left It is mobile;
4) after every layer of spinning 2min, switch direction of an electric field: two electrodes of vertical direction being grounded, two of horizontal direction Electrode meets high potential U, carries out spinning in vertical direction.
5) repeat step 4) and 5), be superimposed 120 layers, obtain right-angled intersection and stack nanofiber array, gained fiber it is straight Diameter is about 2um, and the spacing between fiber is 2-6um.

Claims (5)

1. a kind of right-angled intersection stacks nanofiber array preparation method, specific step is as follows for this method:
1) at room temperature, polymer is added in prepared solvent, is stirred to obtain spinning solution;
2) spinning reception substrate is mounted on electrostatic spinning apparatus, the spinning receives substrate by PCB substrate, two pairs of electrodes Composition, two pairs of electrodes are arranged in PCB substrate and two pairs of electrodes are located at horizontal and vertical directions;And by horizontal direction Two electrodes ground connection, two electrodes of vertical direction connect high voltage power supply;Then spinning nozzle is installed on bracket, adjusts and spins Height and the position of silk spray head make the electrode of vertical some ground connection of face in its front end, and spinning nozzle rear end passes through conduit and syringe pump It is connected, spinning nozzle conductive part taps high-voltage DC power supply;
3) spinning solution is fed by syringe pump, adjusts high-voltage DC power supply voltage, start spinning in the horizontal direction;
4) after horizontal direction spinning, then by two electrodes ground connection of vertical direction, two electrodes of horizontal direction connect height Voltage source, then repeatedly step 3), in vertical direction spinning;
5) step 3) and 4) is repeated, right-angled intersection finally can be obtained and stack nanofiber array.
2. right-angled intersection according to claim 1 stacks nanofiber array preparation method, it is characterised in that: described is poly- Conjunction object solute is polyoxyethylene, nylon, polyurethane, polylactic acid, polystyrene, polyvinyl alcohol, poly lactic-co-glycolic acid copolymerization One of object, polylactide, polycaprolactone, Kynoar, polymethyl methacrylate, polyvinylpyrrolidone are more Kind.
3. right-angled intersection according to claim 1 stacks nanofiber array preparation method, it is characterised in that: the spinning The viscosity of silk solution is 0.1 ~ 2.0Pas.
4. right-angled intersection according to claim 1 stacks nanofiber array preparation method, it is characterised in that: the spinning Silk process specifically: spinning receives a pair of electrodes ground connection in substrate, and another pair electrode in perpendicular direction connects high potential, electricity Induction fiber only ground connection this between movement electrode and at this between forming oriented array electrode.
5. the right-angled intersection that any one of claim 1-4 the method is prepared stacks nanofiber array.
CN201710801174.1A 2017-09-07 2017-09-07 Right-angled intersection stacks nanofiber array preparation method Active CN107699965B (en)

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CN109449357A (en) * 2018-11-06 2019-03-08 苏州华骞时代新能源科技有限公司 A kind of lithium battery diaphragm, preparation method and electrostatic spinning apparatus
CN111041566B (en) * 2019-03-22 2021-11-02 大连民族大学 Combined electrostatic spinning experimental device based on gravity stepped electric field

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CN101538746A (en) * 2008-03-17 2009-09-23 国家纳米科学中心 Principle and novel method for preparing orientation-controllable electrostatic spinning nano polymer fibers
CN201520821U (en) * 2009-09-27 2010-07-07 上海大学 Device for preparing spatial ordered electrostatic spinning nanofibers
EP2045375B1 (en) * 2007-10-02 2011-03-16 Stem Cell Technology Company Apparatus and method for electrospinning 2D- or 3D-structures of micro- or nano-fibrous materials
CN102234848A (en) * 2011-07-05 2011-11-09 东华大学 Device and method for collecting oriented nano fibers by using parallel metal plates
CN103996813A (en) * 2014-05-28 2014-08-20 天津工业大学 Preparation method and device of bi-directional reinforced electrostatic spinning lithium ion battery diaphragm
CN106498514A (en) * 2017-01-05 2017-03-15 大连理工大学 A kind of electrospinning process for preparing orientated nano fibers

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US20100327494A1 (en) * 2009-06-22 2010-12-30 University Of South Carolina Electrospun Fibrous Three-Dimensional Scaffolds with Well-Defined Pore Geometry

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2045375B1 (en) * 2007-10-02 2011-03-16 Stem Cell Technology Company Apparatus and method for electrospinning 2D- or 3D-structures of micro- or nano-fibrous materials
CN101538746A (en) * 2008-03-17 2009-09-23 国家纳米科学中心 Principle and novel method for preparing orientation-controllable electrostatic spinning nano polymer fibers
CN201520821U (en) * 2009-09-27 2010-07-07 上海大学 Device for preparing spatial ordered electrostatic spinning nanofibers
CN102234848A (en) * 2011-07-05 2011-11-09 东华大学 Device and method for collecting oriented nano fibers by using parallel metal plates
CN103996813A (en) * 2014-05-28 2014-08-20 天津工业大学 Preparation method and device of bi-directional reinforced electrostatic spinning lithium ion battery diaphragm
CN106498514A (en) * 2017-01-05 2017-03-15 大连理工大学 A kind of electrospinning process for preparing orientated nano fibers

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