CN109972292A - The method and system of material surface in-stiu coating Electrospun nano-fibers film - Google Patents
The method and system of material surface in-stiu coating Electrospun nano-fibers film Download PDFInfo
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- CN109972292A CN109972292A CN201910357947.0A CN201910357947A CN109972292A CN 109972292 A CN109972292 A CN 109972292A CN 201910357947 A CN201910357947 A CN 201910357947A CN 109972292 A CN109972292 A CN 109972292A
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- stiu coating
- collection device
- syringe
- axis direction
- electrostatic spinning
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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
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
-
- 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
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING 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
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-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
- D04H1/72—Non-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
- D04H1/728—Non-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
Abstract
The invention discloses a kind of method and system of material surface in-stiu coating Electrospun nano-fibers film.The system comprises syringe unit, HV generator unit and collection devices, the syringe unit, collection device are connected with the anode of HV generator unit, cathode respectively, the syringe unit and/or collection device are also connect with a driving with transmission device, and the driving is with transmission device at least to drive the syringe unit and/or collection device to move freely along preferential direction.The described method includes: making the electrostatic spinning liquid that Electrospun nano-fibers film be formed in situ in the material surface to in-stiu coating by electrostatic spinning technique by the control of HV generator unit, driving and transmission device and rotating device.The present invention can effectively realize different-thickness, porosity, different-diameter nano fiber diaphragm uniform in-stiu coating on the surface of the material, substantially reduce interface contact resistance.
Description
Technical field
The present invention relates to a kind of electrospinning devices in situ, and in particular to a kind of in-stiu coating electrostatic spinning on the surface of the material
The method and system of nano-fiber film belong to energy storage field and fibre supercapacitors field.
Background technique
Nanofiber is with a wide range of applications in multiple fields such as biomedicine, food, energy storage, machinery, environmental protection.It is quiet
Electrospun is because its manufacturing device is simple, cost of spinning is cheap, can spin the advantages that substance classes are various, technique is controllable, it has also become has
Effect prepares that organic, organic/inorganic is compound and one of the main path of inorganic nano-fiber.
Currently, a large amount of research work of industry is dedicated to the design of electrostatic spinning apparatus, the configuration of electrostatic spinning solution comes
Prepare different compositions, different-diameter size, different porosities, different physicochemical characteristics, structure-controllable, high quality Static Spinning
Nano fibrous membrane.The Chinese patent of Publication No. CN104018237A be related to a kind of electrostatic spinning membrane thicknesses regulating device and
Use the electrostatic spinning machine of the static spinning membrane thickness adjusting apparatus；The Chinese patent of Publication No. CN108893788A is related to one
Kind electrostatic spinning apparatus is held by the way that spinning injection apparatus is transformed to solve syringe needle existing for existing spininess electrostatic spinning technique
Easily occur blocking the technical problem low with production efficiency；The Chinese patent of Publication No. CN107829157A is related to a kind of Static Spinning
Silk technology, accordingly controls steering engine by PLC, so that the change of position multidimensional can be same with the change of nanofiber shape
Equipment is realized, the Electrospun nano-fibers film of high quality is obtained.
The high quality nano-fiber film obtained in the prior art based on different electrospinning devices, then according to actually answering
With cladding on the surface of the material, is applied in food packaging and fresh-keeping, high temperature filtration, efficient catalytic, bioengineered tissue, light manually
Electrical part, space flight equipment etc..But there are some problems in these prior arts, such as:Cladding electrostatic spinning manually
On the surface of the material, complex process, assembling is cumbersome, at high cost, time-consuming, assembles the rustic difficulty control come for nano-fiber film
System, electrostatic spinning nano fiber film flexibility are too poor (can only realize that the bill of materials bread to be coated covers)；The electrostatic of cladding
Spinning nano-fiber film and the material surface being wrapped by form poor nano-interface structural behaviour, such as Interfacial Adsorption
Difference, interface contact resistance are high, interfacial structure is unstable.
Summary of the invention
The main purpose of the present invention is to provide a kind of sides of material surface in-stiu coating Electrospun nano-fibers film
Method and system, with overcome the deficiencies in the prior art.
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes:
The embodiment of the invention provides a kind of system of material surface in-stiu coating Electrospun nano-fibers film, packets
Include the syringe unit, HV generator unit and collection device to contain electrostatic spinning liquid, the syringe unit
It is connected with the anode of HV generator unit, the collection device is connected with the cathode of HV generator unit, institute
It states syringe unit and/or the collection device to connect with a driving with transmission device, the driving and transmission device are to drive
Move freely the syringe unit and/or the collection device along preferential direction.
Among an embodiment, the collection device includes the material and rotating device to in-stiu coating, described to original
The material of position cladding is set on the rotating device, and is connected with the cathode of the HV generator unit.
Among an embodiment, the collection device includes electric conductor receiver, the material to in-stiu coating and rotation
Device, the electric conductor receiver are connected with the cathode of the HV generator unit, the material to in-stiu coating
It is set on the rotating device, and is fixed above the electric conductor receiver.
The embodiment of the invention also provides a kind of method of material surface in-stiu coating Electrospun nano-fibers film, it
It is to implement according to system above-mentioned comprising:
Syringe unit is provided, is loaded with electrostatic spinning liquid in the syringe unit；
By the control of HV generator unit, driving and transmission device and rotating device, make the electrostatic spinning
Electrospun nano-fibers film is formed in situ in the material surface to in-stiu coating by electrostatic spinning technique in liquid, obtains material
Surface in situ is coated with the composite material of Electrospun nano-fibers film.
Compared with prior art, the beneficial effect comprise that
1) more traditional electrospinning device is compared, novel electrospinning device in situ provided by the invention has very high
Flexibility: syringe unit and collection device realize left and right, front and back, up and down according to certain speed by driving and transmission device
Degree moves freely；The material of wanted in-stiu coating passes through rotating dress other than following collection device front and rear, left and right, moving up and down
The rotation of friction speed may be implemented in the control set；
2) group not only greatly reduces by in-stiu coating Electrospun nano-fibers film on the surface of the material in the present invention
It dresses up this, improve packaging efficiency, and assemble the component compact come, stabilization, have excellent performance, industry easy to accomplish
Change；
3) present invention uses the technology of preparing of material surface in-stiu coating Electrospun nano-fibers film, quiet by controlling
Electrospun liquid type, syringe needle size, electrostatic spinning distance, spinning rate, syringe and collection device relative moving speed, institute
The material rotation speed of in-stiu coating is wanted, effectively realizes different-thickness, porosity, different-diameter nano fiber diaphragm in material
The uniform in-stiu coating in surface, and real-time monitoring is carried out, the assembling of cladding bring is cumbersome, at high cost, time-consuming manually for solution, assembles
The relatively rough disadvantage difficult to control, electrostatic spinning nano fiber film flexibility difference of structure come；
4) present invention uses the technology of preparing of material surface in-stiu coating Electrospun nano-fibers film, spinning Nanowire
Dimension can very well, be uniformly adsorbed on the material surface to be coated, substantially reduce interface contact resistance；
5) technology of preparing of material surface in-stiu coating Electrospun nano-fibers film of the present invention, using very
Extensively, not only can be in fibrous material surface Electrospun nano-fibers film, while can be used for other topology materials
Electrospun nano-fibers film in situ, assemble come functional device can apply food packaging and fresh-keeping, high temperature filtration,
Efficient catalytic, bioengineered tissue, photoelectric device, space flight equipment etc..
Detailed description of the invention
It, below will be to required in embodiment or description of the prior art in order to illustrate more clearly of technical solution of the present invention
The attached drawing used is simply introduced, it should be apparent that, drawings discussed below is as just some implementations invented herein
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other accompanying drawings.
Fig. 1 is that a kind of material surface in-stiu coating Electrospun nano-fibers film is in an of the invention exemplary embodiments
The structural schematic diagram of system.
Fig. 2 is a kind of material surface in-stiu coating Electrospun nano-fibers film in another exemplary embodiments of the present invention
The structural schematic diagram of system.
Fig. 3 is long CNT fiber material surface in-stiu coating Static Spinning PAN nano-fiber film in the embodiment of the present invention 1
Low power scanning electron microscope (SEM) photograph.
Fig. 4 is long CNT fiber material surface in-stiu coating Static Spinning PAN nano-fiber film in the embodiment of the present invention 1
Magnified sweep electron microscope.
Fig. 5 is long CNT fiber material surface in-stiu coating Static Spinning PAN nano-fiber film in the embodiment of the present invention 1
FIB cutting section figure.
Specific embodiment
As previously mentioned, inventor is studied for a long period of time and largely practiced in view of the defect of the prior art, it is able to propose this
The technical solution of invention is related to a kind of technology of preparing of material surface in-stiu coating Electrospun nano-fibers diaphragm, purpose
It is exactly to realize electrostatic spinning nano film efficiently in situ in any material surface, prepares different composite materials, apply in difference
Field solves cladding bring manually and assembles the relatively rough difficult to control, electrostatic of structure that is cumbersome, at high cost, time-consuming, assembling
The disadvantage of spinning nano fibre film flexibility difference.It as follows will be further to works such as the technical solution, its implementation process and principles
It illustrates.
As the one aspect of technical solution of the present invention, involved in be a kind of material surface in-stiu coating electrostatic spinning
The system of nano-fiber film comprising to contain the syringe unit of electrostatic spinning liquid, HV generator unit and
Collection device, the syringe unit are connected with the anode of HV generator unit, the collection device and high-pressure electrostatic
The cathode of generator unit is connected, and the syringe unit and/or the collection device are connect with a driving with transmission device, institute
Driving and transmission device are stated to drive the syringe unit and/or the collection device to move freely along preferential direction.
Among an embodiment, the collection device includes the material and rotating device to in-stiu coating, described to original
The material of position cladding is set on the rotating device, and is connected with the cathode of the HV generator unit.
Further, the collection device is connected with a driving with transmission device, may be implemented centered on collection device
The x-axis (10~100mm/s) of point, y-axis direction (10~100mm/s), z-axis (10~100mm/s) are moved freely.This collection
The device situation conductive suitable for the material of wanted in-stiu coating.
Among an embodiment, the collection device includes electric conductor receiver, the material to in-stiu coating and rotation
Device, the electric conductor receiver are connected with the cathode of the HV generator unit, the material to in-stiu coating
It is set on the rotating device, and is fixed above the electric conductor receiver.
Further, the collection device is connected with a driving with transmission device, may be implemented centered on collection device
The x-axis (10~100mm/s) of point, y-axis direction (10~100mm/s), z-axis (10~100mm/s) are moved freely.This collection
The material conductivity that device is suitable for wanted in-stiu coating is very poor or the case where when without electric conductivity.
Among an embodiment, the syringe unit includes an at least syringe needle, the syringe needle
Diameter is that 0.10~0.50mm is controllable, and the spinning of different-diameter 50nm~600nm nanofiber may be implemented.
Further, the spray head quantity of the syringe unit can be regulated and controled according to demand, can be one, two
It is a, three, it is even more.
Further, the syringe unit is 50~150mm at a distance from the material surface to in-stiu coating.
Further, the rotating device can at least drive the material to in-stiu coating along axial-rotation.Two kinds
The material of the wanted in-stiu coating of different collection devices is all connected with rotating device, can not only follow collection device front and back, a left side
Right synchronizing moving, and by regulation rotating device, covering material can also carry out the rotation of friction speed.
Further, the preferential direction includes the x-axis direction put centered on the syringe unit or collection device
(i.e. following " left and right directions "), y-axis direction (i.e. following " front-rear directions ") or z-axis direction (i.e. following " upper and lower
To ").
Syringe unit is connected with driving with transmission device in the present invention, may be implemented to control according to certain speed, is preceding
Afterwards, unidirectional movement or different directions synchronizing moving up and down, collection device is connected with driving with transmission device, according to certain speed
Left and right, front and back, up and down unidirectional movement or different directions synchronizing moving may be implemented.
The present invention is filled by the driving in the driving and transmission device, syringe unit on regulation collection device with transmission
It sets, collection device and syringe unit or so, in the front-back direction relative motion may be implemented.Such as collection device does not move
It is dynamic, driving and the transmission device of syringe unit are adjusted, realizes that collection device and the opposite of syringe unit control, are upper and lower, preceding
After move；Or stationary nozzle, mobile collection device.
As the other side of technical solution of the present invention, involved in be a kind of material surface in-stiu coating Static Spinning
The method of silk nano-fiber film, it is implemented according to system above-mentioned comprising:
Syringe unit is provided, is loaded with electrostatic spinning liquid in the syringe unit；
By the control of HV generator unit, driving and transmission device and rotating device, make the electrostatic spinning
Electrospun nano-fibers film is formed in situ in the material surface to in-stiu coating by electrostatic spinning technique in liquid, obtains material
Surface in situ is coated with the composite material of Electrospun nano-fibers film.
Among an embodiment, the electrostatic spinning liquid has diversity, including spinning presoma, solvent, proportion.
Further, according to actual needs, the spinning presoma can be organic material, inorganic material etc., for example, institute
Stating organic material can be appointing in Kynoar, polymethyl methacrylate, polyacrylonitrile, polyethylene, polycarbonate etc.
Meaning a combination of one or more, but not limited to this.In another example the inorganic material can be silica SiO2, dioxy
Change titanium TiO2Deng, but not limited to this.
Further, the solvent can selected from acetone, ethyl alcohol, n,N-Dimethylformamide, n,N-dimethylacetamide,
Any one in dimethyl sulfoxide, triethyl phosphate equal solvent or two or more combinations, but not limited to this.
Among an embodiment, the spinning voltage that the electrostatic spinning technique uses for 10~36kV, electrostatic spinning away from
From for 50~150mm, spinning rate is 500~1000 μ L/h, and the movement speed of syringe needle is 0~200mm/s.
It is whether conductive according to the material to in-stiu coating among an embodiment, the structure tool of collection device
There are two types of structures.When the material to in-stiu coating has certain electric conductivity, collection device is by the material to in-stiu coating, rotating dress
Composition is set, wherein the material installation to in-stiu coating is on the spinning device, directly as receiver, with HV generator list
The cathode of member is connected；If to in-stiu coating material do not have electric conductivity, collection device by conducting collector, to in-stiu coating
Material, rotating device composition, wherein material to in-stiu coating is mounted on rotating device, short distance is fixed on conduction together
The top of receiver, furthermore the collection device can also be used for superior electrical conductivity material surface in-stiu coating Electrospun nano-fibers
Film.
Among an embodiment, the material to in-stiu coating has a diversity, unlimited structure composition, length, big
Small, pattern (one-dimensional (fiber morphology), two-dimentional (sheet), three-dimensional (column), multidimensional topology material), as long as rotating dress can be passed through
The regulation set and spray head are installed on the spinning device at a distance from collection device, can be carried out electrostatic spinning in situ according to demand
The cladding of nano-fiber film (rather than just the electrostatic spinning nano fiber film of single side).
Further, the material to in-stiu coating is conductive or without electric conductivity.
Further, the material to in-stiu coating includes any in one-dimensional material, two-dimensional material, three-dimensional material etc.
A combination of one or more, but not limited to this.
Further, the pattern of the material to in-stiu coating includes any in threadiness, sheet and column etc.
A combination of one or more, but not limited to this.For example, the material to in-stiu coating can be CNT (carbon nanotube)
Fiber.
Among an embodiment, on collection device the quantity to the material of in-stiu coating can be one, two,
Three, it is even more.By regulation syringe needle quantity or to the material quantity of in-stiu coating, or pass through regulation spray head and receipts
Acquisition means realize left-right and front-back relative movement, to coat electrostatic spinning nano fiber film while realizing multiple materials.
Among an embodiment, which comprises make the syringe unit with transmission device by the driving
It is moved freely along preferential direction.
Further, the preferential direction includes that the x-axis direction put centered on the syringe unit is (i.e. following
" left and right directions "), y-axis direction (i.e. following " front-rear directions ") or z-axis direction (i.e. following " up and down directions ").
Further, the movement speed of the x-axis direction is 1~100mm/s, the movement speed in the y-axis direction is 5~
100mm/s, the movement speed in the z-axis direction are 5~100mm/s.
Among an embodiment, which comprises make the collection device edge with transmission device by the driving
Preferential direction moves freely.
Further, the preferential direction includes the x-axis direction (i.e. following " left side put centered on the collection device
Right direction "), y-axis direction (i.e. following " front-rear directions ") or z-axis direction (i.e. following " up and down directions ").
Further, the movement speed of the x-axis direction is 10~100mm/s, and the movement speed in the y-axis direction is 10
~100mm/s, the movement speed in the z-axis direction are 10~100mm/s.
Among an embodiment, freely moving relatively for certain orientation is may be implemented in the syringe unit and collection device
Dynamic, further relative moving speed is 0~200mm/s, may include that the x-axis direction put centered on collection device is (opposite
Movement speed is 0-200mm/s), y-axis direction (0-200mm/s).The present invention is by the driving and biography on regulation collection device
Dynamic device, the driving on syringe and transmission device, may be implemented collection device and syringe unit or so, in the front-back direction phase
To movement.Such as collection device does not move, and adjusts driving and the transmission device of syringe unit, realizes collection device and note
The opposite left and right of emitter unit, upper and lower, back-and-forth motion；Or the spray head of fixed syringe unit, mobile collection device.
Among an embodiment, the material of the wanted in-stiu coating of two kinds of different collection devices all with rotating device phase
Even, around can not only following collection device, front and back synchronizing moving, but also by regulation rotating device, material can be with
Carry out the rotation of friction speed.
Further, the revolving speed of the material to in-stiu coating be 0~500rpm, preferably 1~500rpm, it is especially excellent
It is selected as 1~250rpm.
Among an embodiment, the Electrospun nano-fibers film includes three formed by complex root nanofiber
Tie up porous structure.
Further, the Electrospun nano-fibers film with a thickness of 500nm~10 μm, the hole of contained hole
Diameter is 0.1~5 μm, and porosity is 10%~80%.
Further, the diameter of the nanofiber is 50nm~600nm.
In conclusion the present invention passes through control 10~36kV of electrostatic spinning voltage, electrostatic spinning liquid type, syringe needle size
0.10~0.50mm, 50~150mm of electrostatic spinning distance, 500~1000 μ L/h of spinning rate, spray head movement speed 0~
200mm/s, material 1~250rpm of velocity of rotation to in-stiu coating, may be implemented different-thickness 500nm~100 μm, different holes
0.1 μm~5 μm of diameter, different composed structure, different porosities nanofiber uniformly quickly and effectively in-stiu coating in material table
Face.
For the structure of the system of material surface in-stiu coating Electrospun nano-fibers film of the invention, according to being wanted
Whether the material of in-stiu coating is conductive, and used system is divided into two kinds.
Among some more specifically case study on implementation, when the material to in-stiu coating (is hereafter also referred to as and " wants in situ
The material of cladding ") it is conductive when, used system include syringe unit (preferably syringe), high-pressure electrostatic hair
Raw device unit (preferably HV generator), collection device, as shown in Figure 1.Wherein, the syringe be equipped with driving with
Transmission device, can according to actual needs, according to certain speed realize left and right (1~100mm/s), front and back (5~100mm/s) or
Freely up and down move (5~100mm/s)；The collection device is equipped with driving and transmission device, can be according to certain speed
Left and right (10~100mm/s), (10~100mm/s) and front and back (10~100mm/s) is mobile up and down.In addition, collection device by
Material, the rotating device composition of wanted in-stiu coating, the material of in-stiu coating are installed on the spinning device, with high-pressure electrostatic
The cathode of generator is connected, and directly as receiver, by controlling rotating device, the material of in-stiu coating is received in addition to following
Around acquisition means, except upper and lower synchronizing moving, additionally it is possible to realize the rotation (preferably 1~250rpm) of friction speed.It is logical
Cross 10~36kV of control electrostatic spinning voltage, electrostatic spinning liquid type, 0.10~0.5mm of syringe needle size, electrostatic spinning distance 50
~150mm, 500~1000 μ L/h of spinning rate, syringe and collection device 0~200mm/s of relative moving speed, want former
Material 0~500rpm of rotation speed of position cladding, may be implemented different-thickness 500nm~100 μm, 0.1 μm~5 μ of different pore size
M, different composed structures, different porosities (10%~80%) nanofiber uniformly quickly and effectively in-stiu coating in material table
Face.
Among other more specifically case study on implementation, when the material to in-stiu coating (is hereafter also referred to as and " wants former
The material of position cladding ") electric conductivity is very poor or when without electric conductivity, used system include syringe, HV generator,
Collection device, as shown in Figure 2.Wherein, the syringe be equipped with driving and transmission device, can according to actual needs, according to
Certain speed realizes left and right (1~100mm/s), front and back (5~100mm/s) or (5~100mm/s) is moved freely up and down；It is described
Collection device be equipped with driving and transmission device, can according to certain speed or so (10~100mm/s), up and down (10~
100mm/s) and front and back (10~100mm/s) is mobile.In addition, collection device is by electric conductor receiver, wanted in-stiu coating
Material, rotating device composition, wherein electric conductor receiver is connected with HV generator cathode, the material of in-stiu coating
It is mounted on the top for being fixed on conducting collector of rotating device short distance together, by controlling rotating device, to be wrapped in situ
The material covered is around following collection device, other than upper and lower synchronizing moving, additionally it is possible to realize the rotation of friction speed
(preferably 1~250rpm).By control 10~36kV of electrostatic spinning voltage, electrostatic spinning liquid type, syringe needle size 0.10~
0.5mm, it 50~150mm of electrostatic spinning distance, 500~1000 μ L/h of spinning rate, 0~100mm/s of spray head movement speed, is wanted
Different-thickness 500nm~100 μm, different pore size 0.1 μm~5 may be implemented in material 1~500rpm of velocity of rotation of in-stiu coating
μm, the nanofibers of different composed structure, different porosities (10%~80%) uniformly quickly and effectively in-stiu coating in material
Surface.The system equally can also be used to conductive material surface in-stiu coating Electrospun nano-fibers film.
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out detailed retouch
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, those of ordinary skill in the art's every other implementation obtained without making creative work
Example, shall fall within the protection scope of the present invention.
Embodiment 1
The present embodiment coats electrostatic spinning PAN (poly- third by taking CNT (carbon nanotube) fibrous material as an example, in its surface in situ
Alkene nitrile) nano-fiber film, the specific steps are as follows:
Since CNT (carbon nanotube) fibrous material electric conductivity is preferable, so the system that the present embodiment uses Fig. 1, CNT fiber
Material is receiver, is connected with HV generator cathode, is mounted on the rotating device in collection device, and Static Spinning is regulated and controled
Flight lead is from for 100mm.Electrostatic spinning liquid by presoma PAN (polyacrylonitrile), solvent DMF (N,N-dimethylformamide) according to
5% matches；During electrostatic spinning, electrostatic spinning voltage is 15.0kV, and control syringe needle (one) diameter is
0.15mm, syringe and collection device relative to moving left and right speed by the rotation speed of 50mm/s, the material for wanting in-stiu coating
Degree is 250rpm to realize long CNT fiber (length 35cm) surface in situ uniform fold Static Spinning PAN nano-fiber film.Wherein
The diameter of Static Spinning PAN nanofiber is 190-200nm, and the thickness of film is about 5 μm.
Fig. 3, Fig. 4 and Fig. 5 are respectively CNT manufactured in the present embodiment (carbon nanotube) fibrous material surface in-stiu coating electrostatic
Low power scanning electron microscope (SEM) photograph, high power scanning electron microscope (SEM) photograph and the section of FIB (focused ion beam) cutting of spinning PAN nano-fiber film
Figure.
Embodiment 2
The present embodiment coats electrostatic spinning PAN (poly- third by taking CNT (carbon nanotube) fibrous material as an example, in its surface in situ
Alkene nitrile) nano-fiber film, the specific steps are as follows:
Since CNT (carbon nanotube) fibrous material electric conductivity is preferable, so the system that the present embodiment uses Fig. 1, CNT fiber
Material is receiver, is connected with HV generator cathode, is mounted on the rotating device in collection device, and Static Spinning is regulated and controled
Flight lead is from for 50mm.Electrostatic spinning liquid is by presoma PAN (polyacrylonitrile), solvent DMF (N,N-dimethylformamide) according to 5%
Match；During electrostatic spinning, electrostatic spinning voltage is 10.0kV, and spinning rate is 500 μ L/h, controls syringe needle
Head (one) diameter is moved left and right speed and is 200mm/s, wants in-stiu coating by the opposite of 0.15mm, syringe and collection device
The rotation speed of material be that 500rpm realizes that long CNT fiber (length 35cm) surface in situ uniform fold Static Spinning PAN receives
Rice fiber membrane.Wherein the diameter of Static Spinning PAN nanofiber is 190-200nm, and the thickness of film is about 8 μm.
Embodiment 3
The present embodiment coats electrostatic spinning PAN (poly- third by taking CNT (carbon nanotube) fibrous material as an example, in its surface in situ
Alkene nitrile) nano-fiber film, the specific steps are as follows:
Since CNT (carbon nanotube) fibrous material electric conductivity is preferable, so the system that the present embodiment uses Fig. 1, CNT fiber
Material is receiver, is connected with HV generator cathode, is mounted on the rotating device in collection device, and Static Spinning is regulated and controled
Flight lead is from for 150mm.Electrostatic spinning liquid by presoma PAN (polyacrylonitrile), solvent DMF (N,N-dimethylformamide) according to
5% matches；During electrostatic spinning, electrostatic spinning voltage is 36.0kV, and spinning rate is 800 μ L/h, control injection
Device syringe needle (one) diameter is 50mm/s, is wanted in situ by the opposite speed that moves left and right of 0.10mm, syringe and collection device
The rotation speed of the material of cladding is 1rpm to realize long CNT fiber (length 35cm) surface in situ uniform fold Static Spinning PAN
Nano-fiber film.Wherein the diameter of Static Spinning PAN nanofiber is 190-200nm, and the thickness of film is about 2 μm.
Embodiment 4
The present embodiment coats electrostatic spinning PAN (polyacrylonitrile) nanometer by taking nylon fiber material as an example, in its surface in situ
Fiber membrane, the specific steps are as follows:
Since nylon fiber electric conductivity is excessively poor, so the system that the present embodiment uses Fig. 2, nylon fiber and rotating device
The 2mm above electric conductor receiver, wherein conducting collector is connected with HV generator cathode, regulates and controls electrostatic spinning distance
For 100mm.Electrostatic spinning liquid is matched by presoma PAN (polyacrylonitrile), solvent DMF (N,N-dimethylformamide) according to 5%
Than forming；During electrostatic spinning, electrostatic spinning voltage is 25.0kV, and spinning rate is 1000 μ L/h, controls syringe needle
(one) diameter is moved left and right speed and is 50mm/s, wants in-stiu coating by the opposite of 0.50mm, syringe and nylon fiber
The rotation speed of nylon fiber is 250rpm, to realize long nylon fiber (length 35cm) surface in situ uniform fold Static Spinning
PAN nano-fiber film.Wherein the diameter of Static Spinning PAN nanofiber is 190-200nm, and the thickness of film is about 5 μm.
In conclusion the present invention uses material surface in-stiu coating electrostatic spinning by above-mentioned technical proposal of the invention
The technology of preparing of nano-fiber film, by control electrostatic spinning liquid type, syringe needle size, electrostatic spinning distance, spinning rate,
The material rotation speed of the relative moving speed of syringe and collection device, wanted in-stiu coating, come effectively realize different-thickness,
Porosity, different-diameter nano fiber diaphragm uniform in-stiu coating on the surface of the material, and real-time monitoring is carried out, solve cladding manually
Bring assembles relatively rough difficult to control, the electrostatic spinning nano fiber film spirit of structure that is cumbersome, at high cost, time-consuming, assembling
The shortcomings that poor activity；Spinning nanofiber can very well, be uniformly adsorbed on the material surface to be coated, substantially reduce interface
Contact resistance.
It should be noted that, in this document, the terms "include", "comprise" or its any other variant are intended to non-row
His property includes, so that the process, method, article or equipment for including a series of elements not only includes those elements, and
And further include other elements that are not explicitly listed, or further include for this process, method, article or equipment institute it is intrinsic
Element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that including institute
State in the process, method, article or equipment of element that there is also other identical elements.
It should be appreciated that the technical concepts and features of above-described embodiment only to illustrate the invention, its object is to allow be familiar with this
The personage of item technology cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all
Equivalent change or modification made by Spirit Essence according to the present invention, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of system of material surface in-stiu coating Electrospun nano-fibers film comprising to contain electrostatic spinning liquid
Syringe unit, HV generator unit and collection device, the syringe unit and HV generator unit
Anode be connected, the collection device is connected with the cathode of HV generator unit, it is characterised in that: the syringe list
The first and/or described collection device is connect with a driving with transmission device, and the driving and transmission device are to drive the injection
Device unit and/or the collection device are moved freely along preferential direction.
2. system according to claim 1, it is characterised in that: the collection device includes the material and rotation to in-stiu coating
Rotary device, the material to in-stiu coating are set on the rotating device, and with the HV generator unit
Cathode is connected.
3. system according to claim 1, it is characterised in that: the collection device includes electric conductor receiver, to original position
The material and rotating device of cladding, the electric conductor receiver is connected with the cathode of the HV generator unit, described
Material to in-stiu coating is set on the rotating device, and is fixed above the electric conductor receiver.
4. system according to claim 2 or 3, it is characterised in that: the syringe unit includes at least one syringe
Syringe needle, the diameter of the syringe needle are 0.10~0.50mm；
And/or the syringe unit is 50~150mm at a distance from the material surface to in-stiu coating；
And/or the rotating device can at least drive the material to in-stiu coating along axial-rotation；
And/or the preferential direction includes the x-axis direction put centered on the syringe unit or collection device, y-axis direction
Or z-axis direction.
5. a kind of method of material surface in-stiu coating Electrospun nano-fibers film, it is appointed according in claim 1-4
System described in one and implement, characterized by comprising:
Syringe unit is provided, is loaded with electrostatic spinning liquid in the syringe unit；
By the control of HV generator unit, driving and transmission device and rotating device, keep the electrostatic spinning liquid logical
It crosses electrostatic spinning technique and Electrospun nano-fibers film is formed in situ in the material surface to in-stiu coating, obtain material surface
In-stiu coating has the composite material of Electrospun nano-fibers film.
6. according to the method described in claim 5, it is characterized by: the electrostatic spinning liquid includes spinning presoma and solvent；
Preferably, the spinning presoma includes organic material and/or inorganic material；Especially preferred, the organic material includes poly-
Vinylidene, polymethyl methacrylate, polyacrylonitrile, polyethylene, any one or two or more groups in polycarbonate
It closes；Especially preferred, the inorganic material includes silica and/or titanium dioxide；Preferably, the solvent include acetone,
Ethyl alcohol, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, dimethyl sulfoxide, in triethyl phosphate any one or two
Kind or more combination；
And/or the spinning voltage that the electrostatic spinning technique uses is 10~36kV, electrostatic spinning distance is 50~150mm, is spun
Silk rate is 500~1000 μ L/h, and the movement speed of syringe needle is 0~200mm/s.
7. according to the method described in claim 5, it is characterized by: the material to in-stiu coating is conductive or nothing is led
Electrically；Preferably, the material to in-stiu coating include one-dimensional material, two-dimensional material, in three-dimensional material any one or
Two or more combination, it is preferred that the pattern of the material to in-stiu coating includes any in threadiness, sheet and column
A combination of one or more, especially preferred, the material to in-stiu coating is carbon nano-tube fibre；
And/or the quantity of the material to in-stiu coating is at more than one.
8. according to the method described in claim 5, it is characterised by comprising: making the injection with transmission device by the driving
Device unit is moved freely along preferential direction；Preferably, the preferential direction includes the x-axis put centered on the syringe unit
Direction, y-axis direction or z-axis direction；Especially preferred, the movement speed of the x-axis direction is 1~100mm/s, the y-axis side
To movement speed be 5~100mm/s, the movement speed in the z-axis direction is 5~100mm/s；
And/or, which comprises the collection device is moved freely along preferential direction with transmission device by the driving
It is dynamic；Preferably, the preferential direction includes the x-axis direction put centered on the collection device, y-axis direction or z-axis direction；Especially
It is preferred, and the movement speed of the x-axis direction is 10~100mm/s, and the movement speed in the y-axis direction is 10~100mm/
S, the movement speed in the z-axis direction are 10~100mm/s.
9. according to the method described in claim 8, it is characterized by: the relative movement speed of the syringe unit and collection device
Degree is 0~200mm/s；And/or the revolving speed of the material to in-stiu coating be 0~500rpm, preferably 1~500rpm, especially
It is preferably 1~250rpm.
10. according to the method described in claim 5, it is characterized by: the Electrospun nano-fibers film includes by plural number
The three-dimensional porous structure that root nanofiber is formed；Preferably, the Electrospun nano-fibers film with a thickness of 500nm
~100 μm, the aperture of contained hole is 0.1~5 μm, and porosity is 10%~80%；Preferably, the diameter of the nanofiber
For 50nm~600nm.
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| CN112354709A (en) * | 2020-10-18 | 2021-02-12 | 中国人民解放军陆军工程大学 | Efficient preparation device for nano composite material |
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