CN104358029B - A kind of method and device that micro-nano corrugated structure is prepared using electrostatic spinning - Google Patents

A kind of method and device that micro-nano corrugated structure is prepared using electrostatic spinning Download PDF

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Publication number
CN104358029B
CN104358029B CN201410555068.6A CN201410555068A CN104358029B CN 104358029 B CN104358029 B CN 104358029B CN 201410555068 A CN201410555068 A CN 201410555068A CN 104358029 B CN104358029 B CN 104358029B
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China
Prior art keywords
metallic nozzle
collecting board
electrospun polymer
polymer solution
high pressure
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CN201410555068.6A
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Chinese (zh)
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CN104358029A (en
Inventor
布宁斌
尹周平
黄永安
丁亚江
王小梅
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Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • 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
    • D01D5/0015Electro-spinning characterised by the initial state of the material
    • D01D5/0023Electro-spinning characterised by the initial state of the material the material being a polymer melt

Abstract

The invention discloses a kind of method and device that micro-nano corrugated structure is prepared using electrostatic spinning, this method includes:Prepare electrospun polymer solution;Metallic nozzle is kept certain distance with collecting board, avoid the occurrence of " whip moves " behavior;Control electrospun polymer solution to be flowed out with certain flow speed, while from high pressure generator to voltage is applied between Metallic Nozzle At The Ingot and collecting board, make electrospun polymer solution powered and form jet, and ensure that jet is straight jet;Metallic nozzle is rotated, drives fluidic spaces to rotate;Drive collecting board collecting board is moved in one direction by mobile platform simultaneously, ripple struction is formed on base material.The present invention can effectively solve the problem that by the way that for example mode of jet etc. is improved to its critical process step and control the problem of difficult when electrostatic spinning prepares ripple struction, reach simplified preparation technology and realize the technique effect of micro-nano ripple controllable growth.

Description

A kind of method and device that micro-nano corrugated structure is prepared using electrostatic spinning
Technical field
The invention belongs to micro-nano corrugated structure technical field, and micro-nano is prepared using electrostatic spinning more particularly, to one kind The method and device of ripple struction.
Background technology
Electrostatic spinning is a kind of technology of simple manufacture nanofiber, is currently widely used for the production of non-woven fabrics, leads to Often it is applied in terms of filtering, biological tissue.Because nanofiber has the performances such as good light, electricity, magnetic, it is in electronics device Part is more widely applied.Wherein, using the flexible electronic device of buckling structure, the extensive concern of people is obtained.
First propose buckling structure be Huang and Rogers etc. (Hanqing Jiang et al, PNAS. 2007, 104,15607;Dahl-Young Khang, Hanqing jiang, Young Huang, John A.Rogers, 2006, A Stretchable Form of Single-Crystal Silicon for High-Performance Electronics On Rubber Substrates, Science), they are in order to connect the isolated island element manufactured on flexible substrates, using one kind Nanobelt and the buckling structure (i.e. ripple struction) of elastic base plate generation are as interconnection wire.Preparation method is first to use traditional light Quarter, means generated very thin monocrystalline silicon zone on silicon substrate, then monocrystalline silicon zone were transferred to the elastic rubber of pre-stretching (i.e. prestrain) In gum base materials, then remove the prestrain of elastic caoutchouc base material, silicon ribbon is squeezed immediately, generation rule, periodically, can draw The ripple struction stretched.The manufacture method principle is simple, and flexible design, controllability is strong, can by adjust nanobelt material parameter, Section, size etc., are realized in plane or out-of-plane various flexings.Although manufacture craft principle is simple, above-mentioned preparation technology Process is complicated, time-consuming, and prepared by the ripple struction that can not once complete on elastic base plate, and need the costlinesses such as litho machine to set It is standby.
Duan etc. (Duan, Y., Huang, Y., Yin, Z., Bu, N., & Dong, W. (2014) Non-wrinkled, highly stretchable piezoelectric devices by electrohydrodynamic direct- Writing.Nanoscale, 6 (6), 3289-3295) above-mentioned technique is copied, using Electrospun direct write straight line PVDF fibers pre- On the elastic PDMS elastic base plates of strain, corresponding buckling structure is also obtain, and the piezoelectric property of the structure is surveyed Examination.But it is this linear structure is transferred on the elastic caoutchouc substrate of prestrain, then release substrate, form buckling structure, Inevitably introduce residual stress.
For existing ripple struction preparation method complex operation, obtained ripple struction residual stress is big the problem of, at present The method for being used to prepare ripple struction in the prior art is mainly to use directly to prepare by " whip moves " effect in electrostatic spinning The mode of ripple struction.Patent CN102162176A propose it is a kind of using electrostatic spinning prepare ripple struction preparation principle and Method and its device, using " whip moves " behavior in a kind of electrostatic spinning, routing motion platform is direct on flexible elastomeric substrates Realize that ripple struction manufactures, high polymer nanometer fiber can be made to obtain wave structure under the stretched condition of base material, have and prepare Technique is simple, and figure is accurate, the features such as high duplication and high controllability.
However, further investigations have shown that, although above-mentioned existing solution can solve ripple struction to a certain extent The problem of residual stress is big in preparation process, but still following technical problem be present:Due to " whip moves " in electrostatic spinning OK It is related with composite factors such as the density of solution, surface tension, electrical conductivity, dielectric constants for itself, it is the one kind of Electrospun in itself Characteristic, because influence factor is numerous, mechanism is complicated, cause " whip moves " behavior of most fibers disorderly and unsystematic, the fiber of deposition Mostly random, irregular non-woven fabrics form;In addition, to realize " whip moves " behavior, different solutions system need to be directed to, to a variety of Technological parameter (such as voltage, jet length, flow) is adjusted, and state modulator is more difficult, can only be joined in specific technique Under several, reliable and stable " whip moves " could be obtained, thus it is this prepare micro-nano corrugated structure method it is often less efficient, actual Operability is poor.
The content of the invention
The defects of for prior art, micro-nano ripple knot is prepared using electrostatic spinning it is an object of the invention to provide one kind The method and device of structure, wherein by the way that for example generation mechanism of mode of jet, ripple struction etc. is carried out to its critical process step Improve, can effectively solve the problem that control the problem of difficult when electrostatic spinning prepares ripple struction compared with prior art, reach actively Control spinning ripple struction, simplify preparation technology and finally realize the technique effect of micro-nano ripple controllable growth.
To achieve the above object, according to one aspect of the present invention, there is provided one kind prepares micro-nano ripple using electrostatic spinning The method of line structure, it is characterised in that comprise the following steps:
(1) electrospun polymer solution is prepared, then adds the electrospun polymer to the syringe of syringe pump Solution, and the electrospun polymer solution is full of the metallic nozzle being connected with high pressure generator positive pole;
(2) metallic cathode collecting board being connected with high pressure generator earth polar is placed below the metallic nozzle, described Base material is placed on collecting board, the metallic nozzle is kept certain distance with the collecting board, whip is avoided the occurrence of and moves behavior;
(3) control the electrospun polymer solution to be flowed out with certain flow speed, while occurred by the high pressure Device applies voltage between the Metallic Nozzle At The Ingot and the collecting board, makes the electrospun polymer solution powered and formed to penetrate Stream;
(4) metallic nozzle is rotated by certain rotating speed, and drive the jet rotary;Driven simultaneously by mobile platform The collecting board makes the collecting board move in one direction, so as to form ripple struction on the substrate.
As present invention further optimization, the electrospun polymer is polyethylene glycol oxide, and the electrostatic spinning is high Molecular solution is weight percentage concentration as 8% polyethylene oxide solutions, and solvent is deionized water.
As present invention further optimization, metallic nozzle and the distance of the collecting board are described in the step (2) 1-2mm。
As present invention further optimization, the voltage applied in the step (3) is 1.5kV.
As present invention further optimization, the rotating speed of metallic nozzle described in the step (4) is 60 revs/min;It is described The movement velocity of collecting board is less than or equal to 160mm/s.
By the contemplated above technical scheme of the present invention, compared with prior art, due to being revolved using active control jet The mode turned, can obtain the preparation technology of simplified micro-nano corrugated structure and realize the beneficial effect of micro-nano ripple controllable growth. Metallic nozzle and the distance of collecting board are 1-2mm, in this number range, can effectively be avoided " whip moves " in spinning process Occur.The rotation of metallic nozzle can cause to disturb to the electric field environment of electrostatic spinning to a certain extent, make electric field more complicated, And the polarization performance of spinning polymer in spinning process can be influenceed, this is very not there is situation about finely requiring to spun structure Profit;The present invention is by controlling the rotary speed of metallic nozzle in a suitable interval range in actual spinning process It is interior, and coordinate and apply suitable substrate motion speed, influence of the electric field fluctuation to spinning result was both controlled, and can passes through metal The rotary speed of nozzle and the cooperation of substrate motion speed, can obtaining preferable ripple struction pattern, (such as buckling structure is bent Curvature etc.).
According to another aspect of the present invention, there is provided a kind of device that micro-nano corrugated structure is prepared using electrostatic spinning, It is characterised in that it includes injection flow pump 1, syringe, solution conduit 2, rotating mechanism 3, metallic nozzle 4, high pressure generator 5, Base material 6, metal collection plate 7, motion platform 8, wherein the injected current amount pump 1 is connected with the rear end of the syringe, it is described molten Fluid catheter 2 connects the front end of the syringe and the metallic nozzle 4;The metallic nozzle 4 is fixed on the rotating mechanism 3 On, the rotating mechanism 3 can drive the metallic nozzle 4 to rotate;The base material 6 is located on the metal collection plate 7, described Metal collection plate 7 is located on the motion platform 8, and the motion platform 8 can drive the metal collection plate 7 to move;It is described The positive pole of high pressure generator 5 is connected with the metallic nozzle 4, the earth polar of the high pressure generator 5 and the phase of metal collection plate 7 Even;For the metallic nozzle 4 positioned at the top of base material 6, distance of the metal collection plate 7 away from the metallic nozzle 4 is 1- 2mm。
By the contemplated above technical scheme of the present invention, compared with prior art, by by metallic nozzle and collecting board Distance be arranged to 1-2mm, can effectively avoid the generation of " whip moves " in spinning process;And use rotating mechanism active control Metallic nozzle rotation, so as to drive electrostatic spinning jet rotary, the preparation technology of simplified micro-nano corrugated structure and real can be obtained The beneficial effect of existing micro-nano ripple controllable growth.
Brief description of the drawings
Fig. 1 is the schematic diagram of electrostatic spinning apparatus, wherein 1 is an injection flow pump for carrying syringe, 2 lead for solution Pipe, 3 be rotating mechanism, and 4 be metallic nozzle, and 5 be high pressure generator, and 6 be base material, and 7 be metal collection plate, and 8 be motion platform;
The pattern formed when Fig. 2 is spinning under friction speed on base material.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and It is not used in the restriction present invention.
Embodiment 1
The polyethylene glycol oxide spinning solution that weight percent concentration is 8% is configured, is poured into syringe, is promoted in syringe pump Under, solution flows into metallic nozzle 4 along solution conduit 2;Metallic Nozzle At The Ingot 4 is connected with the positive pole of high pressure generator 5, is also secured to On rotating mechanism 3, it can be driven and rotated by the mechanism;Metal collection plate 5 is 1mm apart from the distance of metallic nozzle 4, metal collection plate 7 are fixed on motion platform 8, are placed with base material 6 thereon, are here PET film;4 a diameter of 0.16mm of metallic nozzle, flow Speed is 500nL/min;Apply voltage 1.5kV, make the electrospun polymer solution powered and form jet, and jet is in Move along a straight line (i.e. straight jet, avoiding " whip moves " behavior);Rotating mechanism 3 drives jet to rotate, rotating mechanism 3 Rotating speed is 60 revs/min, and motion platform 8 drives base material 6 to be moved in one direction with fixed speed (i.e. substrate transport speed), enters Row Electrospun.Above-mentioned straight jet is by making metallic nozzle and substrate keep closely realizing.Fig. 2 is respectively from top to bottom Spinning pattern when substrate transport speed is 10mm/s, 80mm/s, 160mm/s and 240mm/s, respectively phone cable architecture, draw 8 word structures, sinusoidal structured and the linear structure opened;It can be seen that when substrate transport speed is less than 160mm/s, electrostatic spinning can obtain To micro-nano corrugated structure, and the different range of flexion of buckling structure can be realized, such as phone cable architecture, the 8 word structures pulled open, sinusoidal knot Structure etc..
Embodiment 2
The polyethylene glycol oxide spinning solution that weight percent concentration is 8% is configured, is poured into syringe, is promoted in syringe pump Under, solution flows into metallic nozzle 4 along solution conduit 2;Metallic Nozzle At The Ingot 4 is connected with the positive pole of high pressure generator 5, is also secured to On rotating mechanism 3, it can be driven and rotated by the mechanism;Metal collection plate 5 is 2mm apart from the distance of metallic nozzle 4, metal collection plate 7 are fixed on motion platform 8, are placed with base material 6 thereon, are here PET film;Apply voltage 1.5kV, make the Static Spinning Silk Polymer Solution is powered and forms jet, and jet linearly moves and (i.e. straight jet, avoids " whip moves " behavior);Rotation Mechanism 3 drives jet to rotate, and the rotating speed of rotating mechanism 3 is 60 revs/min, and motion platform 8 drives base material 6 with fixed speed Degree (i.e. substrate transport speed) moves in one direction, carries out Electrospun.
Above example only provides explanation step, wherein concentration, voltage, nozzle inside diameter, flow speed, motion platform speed Suitable numerical value can be selected according to experimental conditions.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., all should be included Within protection scope of the present invention.

Claims (2)

  1. A kind of 1. method that micro-nano corrugated structure is prepared using electrostatic spinning, it is characterised in that comprise the following steps:
    (1) electrospun polymer solution is prepared, then adds the electrospun polymer solution to the syringe of syringe pump, And the electrospun polymer solution is set to be full of the metallic nozzle being connected with high pressure generator positive pole;
    (2) metallic cathode collecting board being connected with high pressure generator earth polar is placed below the metallic nozzle, in the collection Base material is placed on plate, the metallic nozzle is kept certain distance with the collecting board, whip is avoided the occurrence of and moves behavior;The metal The distance of nozzle and the collecting board is 1-2mm;
    (3) control the electrospun polymer solution to be flowed out with certain flow speed, at the same from the high pressure generator to Apply voltage between the Metallic Nozzle At The Ingot and the collecting board, make the electrospun polymer solution powered and form jet;
    (4) metallic nozzle is rotated by certain rotating speed, and drive the jet rotary;Simultaneously as described in driving mobile platform Collecting board makes the collecting board move in one direction, so as to form ripple struction on the substrate;
    Wherein, the electrospun polymer is polyethylene glycol oxide, and the electrospun polymer solution is weight percentage dense The polyethylene oxide solutions for 8% are spent, solvent is deionized water;
    The voltage applied in the step (3) is 1.5kV;
    The rotating speed of metallic nozzle described in the step (4) is 60 revs/min;The movement velocity of the collecting board be less than or equal to 160mm/s。
  2. 2. a kind of device that micro-nano corrugated structure is prepared using electrostatic spinning, it is characterised in that including injection flow pump (1), note Emitter, solution conduit (2), rotating mechanism (3), metallic nozzle (4), high pressure generator (5), base material (6), metal collection plate (7), Motion platform (8), wherein the injected current amount pump (1) is connected with the rear end of the syringe, the solution conduit (2) connects institute State front end and the metallic nozzle (4) of syringe;The metallic nozzle (4) is fixed on the rotating mechanism (3), the rotation Rotation mechanism (3) can drive the metallic nozzle (4) to rotate;The base material (6) is located on the metal collection plate (7), described Metal collection plate (7) is located on the motion platform (8), and the motion platform (8) can drive the metal collection plate (7) to transport It is dynamic;The positive pole of the high pressure generator (5) is connected with the metallic nozzle (4), the earth polar of the high pressure generator (5) with it is described Metal collection plate (7) is connected, and the high pressure generator (5) is used for the voltage for applying 1.5kV to the metallic nozzle (4);It is described Metallic nozzle (4) is located above the base material (6), and the distance of the metal collection plate (7) away from the metallic nozzle (4) is 1- 2mm;The metallic nozzle (4) is used to rotate with 60 revs/min of rotating speed;The collecting board is used for less than or equal to 160mm/s's Movement velocity moves;
    In addition, the syringe is used to accommodate electrospun polymer solution, the electrospun polymer is polyethylene glycol oxide, The electrospun polymer solution is weight percentage concentration as 8% polyethylene oxide solutions, and solvent is deionized water.
CN201410555068.6A 2014-10-17 2014-10-17 A kind of method and device that micro-nano corrugated structure is prepared using electrostatic spinning Expired - Fee Related CN104358029B (en)

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CN103966682A (en) * 2014-05-22 2014-08-06 苏州东茂纺织实业有限公司 Radial-direction control device for fuse wire
CN104909333B (en) * 2015-04-17 2017-03-01 广东工业大学 Micro-nano corrugated structure manufacture device and method
CN104808271B (en) * 2015-04-17 2017-06-27 广东工业大学 The grating manufacture method of rheology direct write is induced based on hot induced electric field
US10138574B2 (en) * 2016-10-17 2018-11-27 Fanavaran Nano-Meghyas Company (Ltd) Blowing-assisted electrospinning
CN106847707B (en) * 2017-01-18 2019-08-30 华中科技大学 A method of extending island bridge structure is prepared based on electrofluid Printing techniques
CN111389472B (en) * 2020-03-23 2021-08-17 南京工业职业技术学院 Device and method for preparing electrospinning direct-writing multilayer microfluidic chip
CN111501112B (en) * 2020-04-29 2021-12-24 陕西工业职业技术学院 Device and method for preparing logic channel microfluidic chip
CN113308768B (en) * 2021-06-22 2022-06-21 青岛科技大学 Electrostatic spinning superfine fiber twisting device and method

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CN103998667B (en) * 2011-12-21 2018-02-02 纳幕尔杜邦公司 The method of web of the tiling from centrifugal type spinning technology
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