CN106591966A - Electro-hydro dynamics preparation method for filament and particle parallel micro-nano structure - Google Patents
Electro-hydro dynamics preparation method for filament and particle parallel micro-nano structure Download PDFInfo
- Publication number
- CN106591966A CN106591966A CN201611021571.9A CN201611021571A CN106591966A CN 106591966 A CN106591966 A CN 106591966A CN 201611021571 A CN201611021571 A CN 201611021571A CN 106591966 A CN106591966 A CN 106591966A
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- Prior art keywords
- fluid
- grams
- nano structure
- preparation
- shower nozzle
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Classifications
-
- 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
-
- 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
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
-
- 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
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
-
- 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
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
-
- 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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Nonwoven Fabrics (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention relates to an electro-hydro dynamics preparation method for a filament and particle parallel micro-nano structure. The method prepares and combines nanofibers which are filaments, and microparticles which are particles by electro-hydro dynamics, and parallel structure characteristics are formed. The preparation process is simple, and is effective in a single process, and prepared filament and particle parallel structure product is clear in structure and uniform in distribution. The preparation method for a parallel micro-nano structure can provide an effective tool for development of various new functional materials.
Description
Technical field
The present invention relates to a kind of micro Nano material process technology, the electric current of more particularly to a kind of grain micro nano structure arranged side by side
Body dynamics preparation method.
Background technology
It is solid to prepare for energy, the interaction using it and fluid between that electrohydrodynamicss method adopts high-pressure electrostatic
Body material.The method mainly includes high-voltage electrostatic spinning technology (electrospinning）, high-voltage electrostatic spraying technology（EFI）And jet printing
Technology.Wherein high-voltage electrostatic spinning technology（Electrospinning）It is a kind of nano-fabrication technique of (top-down) from top to bottom, by outer
Added electric field power overcome shower nozzle tip drop surface tension of liquid and viscoelastic power and form jet, electrostatic repulsion, Coulomb force and
Under surface tension collective effect, the liquid jet after being atomized is drafted within a few tens of milliseconds by high frequency flexural, drawing, division
Thousands of times, the volatilization of Jing solvents or melt cooling obtain nano-scale fiber in receiving terminal.High-voltage electrostatic spraying technology is by work
Fluid applies certain voltage, it is divided atomization rapidly by electrostatic repulsion forces off field in high-pressure electrostatic and is produced huge table
Area, by the quick volatilization of the solvent in atomized drop solid particle is prepared.These electrohydrodynamicss technical processs
Simply, manipulate it is convenient, select that material ranges are extensive, controllability is strong, be considered as most possibly to realize continuous micro Nano material work
A kind of method that industry metaplasia is produced, prepares function micro Nano material and has good prospect using the technology.
There are numerous literature research electrospinnings to prepare nanofiber at present, while also there is numerous preparing with regard to EFI to gather
The report of compound microgranule, but seldom there is research to be combined the material structure feature of the two.Because electrospinning fibre is typically located
In nano-level, and EFI microgranule is more in micron level, therefore both combination can cause nano-fiber material and micro-
There is the synergism of structure of matter level in rice grain material, give micro-nano structure product better performance, complex function, or even
Them are promoted to produce new application of function.
The content of the invention
The present invention be directed to nanofiber and polymer particles combine the problem to form micro-nano structure, it is proposed that a kind of silk grain
The arranged side by side electrohydrodynamicss preparation method of micro nano structure, by for the nanofiber of " silk " and for " grain " micron particle electric current
Body dynamics are prepared and are combined together, and form parallel construction feature.
The technical scheme is that：A kind of electrohydrodynamicss preparation method of thread grain micro nano structure arranged side by side, specifically
Comprise the steps：
1）Build preparation facilitiess：There are two small one and large one capillary tubies arranged side by side in decentralized casing shower nozzle, little capillary tube is in big capillary
Guan Zhong, and tube wall is tangent, and fluid is hose connection partially by high resiliency silica gel in fixed syringe on first fluid syringe pump
Little capillary inlet in heart sleeve pipe shower nozzle；Fluid is directly connected to decentralized casing shower nozzle in the syringe that second fluid syringe pump is fixed
Big capillary inlet, high tension generator and decentralized casing shower nozzle connect, and decentralized casing spray outlet lower end is provided with a reception
Plate, receives the hardboard that flat board is aluminium foil parcel；
2）Polymer fluid of the configuration with favorable spinning quality, injects syringe fixed on first fluid syringe pump；
3）Configuration does not have the polymer fluid or small molecule fluid of spinning properties, injects note fixed on second fluid syringe pump
Emitter；
4）High tension generator is opened, the flow velocity of two kinds of fluids in controlling two syringe pumps to control decentralized casing shower nozzle, in high pressure
In the presence of electrostatic, decentralized casing spray outlet produces nanofiber and micron particle parallel construction product, by receiving flat board
Receive.
The step of nanofiber and micron particle parallel construction product 2）With 3）Two fluids is equipped with as follows：By 10 second
Base cellulose is put in 100 grams of ethanol, is made into not spinnable polymer fluid, by 7 grams of polyvinylpyrrolidones and 0.01 gram of Asia
Methyl blue is put in 100 grams of ethanol, is made into spinnable polymer fluid；
Step 4 after the allotment）Control is required：The flow of two fluids is 1.0 mL/h, receive flat board from spray outlet away from
From for 15 cm, the kV of high tension generator voltage 14, ambient temperature is 24 ± 2 DEG C, and ambient humidity is 55 ± 5%.
When the nanofiber and micron particle infrastructure product are polymer/lecithin silk grain micro nano structure product arranged side by side
Step 2）With 3）Two fluids is equipped with as follows：7 grams of polyvinylpyrrolidones and 0.01 gram of methylene blue are put into into 100 grams of ethanol
In, it is made into spinnable polymer fluid；20 grams of soybean lecithins are dissolved in 100 grams of dichloromethane, small molecule fluid is made into；
Step 4 after the allotment）Control is required：The flow of two fluids is 1.0 mL/h, receive flat board from spray outlet away from
From for 15 cm, the kV of high tension generator voltage 14, ambient temperature is 24 ± 2 DEG C, and ambient humidity is 55 ± 5%.
The beneficial effects of the present invention is：The electrohydrodynamicss preparation method of silk grain of the present invention micro nano structure arranged side by side,
Preparation process is simple, single step is effectively, the silk grain parallel construction product structure for preparing is clear, be evenly distributed.The micro-nano structure arranged side by side
Preparation method can provide effective tool for the exploitation of numerous new function materials.
Description of the drawings
Fig. 1 is silk grain micro nano structure schematic diagram arranged side by side；
Fig. 2 is the electrohydrodynamicss preparation method implementation figure of silk grain of the present invention micro nano structure arranged side by side；
Fig. 3 is decentralized casing shower nozzle schematic cross-section of the present invention；
Fig. 4 is the electrohydrodynamicss preparation process shooting figure of silk grain of the present invention micro nano structure arranged side by side；
Fig. 5 is the scanning electron microscope diagram of silk grain of the present invention micro nano structure arranged side by side；
Fig. 6 is the transmission electron microscope figure of silk grain of the present invention micro nano structure arranged side by side.
Specific embodiment
The silk grain micro nano structure arranged side by side of the present invention, as shown in figure 1, component 2 is " silk " nanofiber in figure, component 1 is
" grain " micron particle, both adheres to each other to form parallel construction feature.The architectural feature can integrate micro materials and receive
Common effect of rice material, it is also possible to integrate the common performance of granular materialss and fiber film material.
The assembling of electrohydrodynamicss preparation method device side by side：The electrohydrodynamic length of schooling of silk grain micro nano structure arranged side by side
Preparation Method implementation as shown in Fig. 2 including：High tension generator 1；Fluid syringe pump 2；Fluid syringe pump 3；Product receiver board 4；
Decentralized casing shower nozzle 5；High resiliency silica gel hose 6；Fluid injector 7 and fluid injector 8.There are two in decentralized casing shower nozzle 5
Small one and large one capillary tube arranged side by side, decentralized casing shower nozzle schematic cross-section as shown in Figure 3, little capillary tube in big capillary tube, and
And tube wall is tangent.Fluid connects decentralized casing spray by high resiliency silica gel hose 6 in fixed syringe 8 on fluid syringe pump 3
Little capillary inlet in 5；Fluid is directly connected to the big capillary tube of decentralized casing shower nozzle 5 in the syringe 7 that fluid syringe pump 2 is fixed
Entrance.High tension generator 1 and decentralized casing shower nozzle 5 connect.The exit lower end of decentralized casing shower nozzle 5 is provided with a receiver board 4, connects
It is closed flat the hardboard that plate 4 is aluminium foil parcel.
The allotment of two strands of working fluids：10 ethyl celluloses are put in 100 grams of ethanol, not spinnable polymer work is sprayed into
Make fluid, 7 grams of polyvinylpyrrolidones and 0.01 gram of methylene blue are put in 100 grams of ethanol, be sprayed into spinnable polymer flow
Body.
The enforcement of electrohydrodynamicss preparation method side by side：Above two working fluid is respectively charged into into corresponding syringe
In, it is fixed on corresponding syringe pump according to embodiment 1, connect decentralized casing shower nozzle and HV generator.
Implement electrohydrodynamic method arranged side by side according to following technological parameter：The flow of two fluids is 1.0 mL/
H, receiver board is 15 cm, the kV of voltage 14 with a distance from spinning nozzle.Ambient temperature is (24 ± 2) DEG C, and ambient humidity is 55 ± 5%.
Product wraps up cardboard and is collected by the aluminium foil being grounded.In the above operating condition, in situ amplification is carried out to electro-spinning process to clap
Take the photograph, be as a result illustrated in figure 4 a typical electrohydrodynamicss process, i.e., stretch from taylor cone, straight jet to high frequency
Range of instability.Under the instruction of indicator methylene blue, the compound taylor cone of parallel construction is clear and legible.
The analysis and characterization of silk grain micro nano structure arranged side by side：Using field scanning Electronic Speculum to micro-nano prepared by embodiment 3
Structure carries out being observed after the metal spraying of surface, as a result as shown in Figure 5.Prepared silk grain micro nano structure arranged side by side is evenly distributed.Wherein
Fiber while good linear condition is presented, a diameter of 74 ± 9 nm, granule rounded state on one side, a diameter of 2.1 ± 0.4
m.Prepared structure is observed using high-resolution projection electron microscope, as a result as shown in fig. 6, micron particle and Nanowire
Dimension close adhesion is together.
The preparation of polymer/lecithin silk grain micro nano structure arranged side by side：By 7 grams of polyvinylpyrrolidones and 0.01 gram of methylene
Base indigo plant is put in 100 grams of ethanol, is sprayed into spinnable polymer fluid.20 grams of soybean lecithins are dissolved in into 100 grams of dichloromethane
In, it is made into working fluid（This is small molecule fluid）.In being loaded into corresponding syringe, it is fixed to accordingly according to embodiment 1
Syringe pump on, connect decentralized casing shower nozzle and HV generator.Implement electric current arranged side by side according to following technological parameter
Body dynamic method：The flow of two fluids is 1.0 mL/h, and receiver board is 15 cm, the kV of voltage 14 with a distance from spinning nozzle.Ring
Border temperature is (24 ± 2) DEG C, and ambient humidity is 55 ± 5%.Product wraps up cardboard and is collected by the aluminium foil being grounded, you can system
Obtain polymer/lecithin silk grain micro nano structure product arranged side by side.
Feature of the present invention is the parallel construction mixed by nanofiber and micron particle automatic uniform in preparation process and
Into；One side micron particle in parallel construction is bonded on the nanofiber of another side, and both are collectively forming a complete product；
The structure adopts decentralized casing and prepares for shower nozzle implements electrohydrodynamicss technique；Side by side one is with good in two fluids
The polymer solution of good spinning properties, another stock is the polymer solution or small molecule solution without spinning properties.Silk grain is simultaneously
Array structure is received using aluminium foil flat board.
Claims (3)
1. the electrohydrodynamicss preparation method of a kind of grain micro nano structure arranged side by side, it is characterised in that specifically include following step
Suddenly：
1）Build preparation facilitiess：There are two small one and large one capillary tubies arranged side by side in decentralized casing shower nozzle, little capillary tube is in big capillary
Guan Zhong, and tube wall is tangent, and fluid is hose connection partially by high resiliency silica gel in fixed syringe on first fluid syringe pump
Little capillary inlet in heart sleeve pipe shower nozzle；Fluid is directly connected to decentralized casing shower nozzle in the syringe that second fluid syringe pump is fixed
Big capillary inlet, high tension generator and decentralized casing shower nozzle connect, and decentralized casing spray outlet lower end is provided with a reception
Plate, receives the hardboard that flat board is aluminium foil parcel；
2）Polymer fluid of the configuration with favorable spinning quality, injects syringe fixed on first fluid syringe pump；
3）Configuration does not have the polymer fluid or small molecule fluid of spinning properties, injects note fixed on second fluid syringe pump
Emitter；
4）High tension generator is opened, the flow velocity of two kinds of fluids in controlling two syringe pumps to control decentralized casing shower nozzle, in high pressure
In the presence of electrostatic, decentralized casing spray outlet produces nanofiber and micron particle parallel construction product, by receiving flat board
Receive.
2. the electrohydrodynamicss preparation method of silk grain micro nano structure arranged side by side according to claim 1, it is characterised in that institute
The step of stating nanofiber and micron particle parallel construction product 2）With 3）Two fluids is equipped with as follows：10 ethyl celluloses are put
In entering 100 grams of ethanol, not spinnable polymer fluid is made into, 7 grams of polyvinylpyrrolidones and 0.01 gram of methylene blue are put into
In 100 grams of ethanol, spinnable polymer fluid is made into；
Step 4 after the allotment）Control is required：The flow of two fluids is 1.0 mL/h, receive flat board from spray outlet away from
From for 15 cm, the kV of high tension generator voltage 14, ambient temperature is 24 ± 2 DEG C, and ambient humidity is 55 ± 5%.
3. the electrohydrodynamicss preparation method of silk grain micro nano structure arranged side by side according to claim 1, it is characterised in that institute
State step 2 when nanofiber and micron particle infrastructure product are polymer/lecithin silk grain micro nano structure product arranged side by side）With 3）
Two fluids is equipped with as follows：7 grams of polyvinylpyrrolidones and 0.01 gram of methylene blue are put in 100 grams of ethanol, being made into spin
Polymer fluid；20 grams of soybean lecithins are dissolved in 100 grams of dichloromethane, small molecule fluid is made into；
Step 4 after the allotment）Control is required：The flow of two fluids is 1.0 mL/h, receive flat board from spray outlet away from
From for 15 cm, the kV of high tension generator voltage 14, ambient temperature is 24 ± 2 DEG C, and ambient humidity is 55 ± 5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611021571.9A CN106591966B (en) | 2016-11-21 | 2016-11-21 | Electrohydrodynamic preparation method of silk particle parallel micro-nano structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611021571.9A CN106591966B (en) | 2016-11-21 | 2016-11-21 | Electrohydrodynamic preparation method of silk particle parallel micro-nano structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106591966A true CN106591966A (en) | 2017-04-26 |
| CN106591966B CN106591966B (en) | 2020-11-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611021571.9A Active CN106591966B (en) | 2016-11-21 | 2016-11-21 | Electrohydrodynamic preparation method of silk particle parallel micro-nano structure |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2004427A1 (en) * | 1968-03-21 | 1969-11-21 | Kanegafuchi Boseki | |
| CN101638828A (en) * | 2009-08-20 | 2010-02-03 | 东华大学 | Method for preparing amphiphilic composite nanometer film by using high pressure electrostatic spinning |
| CN101979726A (en) * | 2010-11-08 | 2011-02-23 | 东华大学 | Solvent circulation electrostatic spinning device |
| CN101994162A (en) * | 2010-12-10 | 2011-03-30 | 江南大学 | Microfluid electrostatic spinning device |
| CN102051693A (en) * | 2011-01-20 | 2011-05-11 | 东华大学 | Split type composite electrostatic spinning device |
| CN102824641A (en) * | 2012-09-07 | 2012-12-19 | 东华大学 | Two-phase drug-release multilayer drug-loaded nanofiber mat and preparation method thereof |
| CN104611773A (en) * | 2015-01-19 | 2015-05-13 | 上海理工大学 | Eccentric sleeve type parallel spinning head and application thereof |
-
2016
- 2016-11-21 CN CN201611021571.9A patent/CN106591966B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2004427A1 (en) * | 1968-03-21 | 1969-11-21 | Kanegafuchi Boseki | |
| CN101638828A (en) * | 2009-08-20 | 2010-02-03 | 东华大学 | Method for preparing amphiphilic composite nanometer film by using high pressure electrostatic spinning |
| CN101979726A (en) * | 2010-11-08 | 2011-02-23 | 东华大学 | Solvent circulation electrostatic spinning device |
| CN101994162A (en) * | 2010-12-10 | 2011-03-30 | 江南大学 | Microfluid electrostatic spinning device |
| CN102051693A (en) * | 2011-01-20 | 2011-05-11 | 东华大学 | Split type composite electrostatic spinning device |
| CN102824641A (en) * | 2012-09-07 | 2012-12-19 | 东华大学 | Two-phase drug-release multilayer drug-loaded nanofiber mat and preparation method thereof |
| CN104611773A (en) * | 2015-01-19 | 2015-05-13 | 上海理工大学 | Eccentric sleeve type parallel spinning head and application thereof |
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| CN106591966B (en) | 2020-11-24 |
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