The device of patterned Graphene film is prepared on electrospinning fibre network with czochralski method
Technical field
The utility model is related to the preparation field of composite nano-fiber membrane, specifically a kind of fine in electrospinning with czochralski method
The device of patterned Graphene film is prepared on dimension network.
Background technology
Graphene is star most dazzling in nano-carbon material field nearly ten years, and its unique two dimensional crystal structure is assigned
A series of its unique physicochemical characteristics is given.After being prepared from first passage experiment, it just causes domestic and foreign scholars
Extensive concern, research interest also from pay close attention to its unique physicochemical characteristics progressively to application fields such as microelectronics, biomedicines
Expand.
The film being made up of Graphene has that chemical stability is good, transparency is high, electric conductivity is strong, mechanical strength is big, biological
The series of advantages such as compatibility is good, has huge application prospect in numerous areas such as photoelectric cell, tissue cultures, just progressively into
It is study hotspot.
There are some researches show graphene film is to mesenchymal stem cells MSCs, NSC, multipotency induction stem cell etc.
Various cells of mamma animals have compatibility very high, it would be preferable to support cell sticks, breeds and breaks up.And pass through photoetching, electrospinning,
Patterned Graphene film surface obtained in the means such as micro Process contains abundant topological structure and microstructure, is expected to turn into new
Generation cell culture platform and organization bracket.
Some trials for preparing patterned Graphene film are had in the industry, but existing processes are still immature, there is film equal
Even property is poor, preparation technology complicated, be not easy to a series of defects such as large-scale production.
Utility model content
For above-mentioned deficiency of the prior art, the purpose of this utility model is to provide a kind of fine in electrospinning with czochralski method
Prepare the device of patterned Graphene film on dimension network, electrospinning used by the device is simple with lifting technical operation, into
This is cheap, easily controllable, gained graphene film it is uniform it is complete, be easy to carry out functional modification, and can be by controlling electrospinning fine
The pattern for tieing up network is patterned simply to be regulated and controled.
The technical scheme in the invention for solving the technical problem is:Made on electrospinning fibre network with czochralski method
The device of standby patterned Graphene film, including electrostatic spinning apparatus, pulling apparatus and the reduction apparatus being applied in combination, Static Spinning
Silk device, pulling apparatus and reduction apparatus are respectively positioned in locking device;
The electrostatic spinning apparatus include high pressure generator, micro pump, needle tubing and operating platform, under the operating platform
Side is provided with the lowering or hoisting gear of regulation operating platform height, and the table top of operating platform is provided with the aluminium-foil paper for carrying slide;It is described
Needle tubing is located at the surface of aluminium-foil paper, and needle tubing is connected with micro pump and is provided with shower nozzle in bottom;The high pressure generator is just
Pole is connected with the needle tubing, and the negative pole of high pressure generator is connected with the aluminium-foil paper;
The pulling apparatus include propulsion pump, connecting rod and device for storing liquid, and the connecting rod is longitudinally arranged and is connected with propulsion pump,
Device for storing liquid for top end opening groove and positioned at the underface of connecting rod;
The inner space of the reduction apparatus is divided into two-layer, and reduction apparatus inside is capable of achieving vacuum state.
Further technical scheme is:Described propulsion pump is connected after being inverted with the connecting rod.After propulsion pump is inverted, by
The pump housing is connected with connecting rod, compared with being connected with pushing ram, connects more firm, it is to avoid the rocking of pushing ram, and propulsion is also more
Plus stabilization, so that the movement of connecting rod is more accurate.
Further technical scheme is:Described locking device is openable plexiglass tent.Plexiglass tent can
Device is isolated from the outside, and does not influence the observation to the device course of work, in the preparatory stage of preparation work, can be by organic glass
Glass cover is opened, and adjusts the distance between height and connecting rod and device for storing liquid of operating platform etc., after the completion of preparation, device
In the course of work, device should be isolated from the outside using plexiglass tent.
To realize the effective support to advancing pump, further technical scheme is:It is flat that described propulsion pump is arranged on support
On platform.
Further technical scheme is:The lowering or hoisting gear includes leading screw and nut sleeve, and it is flat that the leading screw is arranged on operation
At four angles of platform bottom surface, the nut sleeve is engaged with leading screw respectively, and the nut sleeve synchronous rotary drives the leading screw to do
Linear reciprocating motion.The height of operating platform is adjusted by screw transmission, accuracy is high, it is possible to achieve aluminium-foil paper and needle tubing
The adjustment of slight distance between shower nozzle.
A kind of selectable technical scheme is:The nut sleeve is driven by drive gear, two adjacent drivings
Travelling gear is provided between gear to realize drive gear synchronous rotary, bevel gear is passed through between active drive gear and rocking handle
Transmission mechanism is connected.
Another selectable technical scheme is:The nut sleeve is driven by driving worm gear, two adjacent drives
Transmission worm gear is provided between dynamic worm gear to realize driving worm gear synchronous rotary, worm gear is passed through between active drive worm gear and rocking handle
Worm mechanism is connected, and rocking handle is arranged on the end of worm screw.
Bevel gear transmission or worm-and-wheel gear change the transmission side of action during transmission is acted
To being easy to the operation of people.
Further technical scheme is:The vertical range between shower nozzle on the aluminium-foil paper and the needle tubing for 15~
20cm.Under the distance, the effect of electrostatic spinning is best.
Further technical scheme is:The needle tubing is made up of glass or plastics.
Further technical scheme is:The connecting rod is glass bar or teflon rod.
The beneficial effects of the utility model are:Preparation, the patterned oxide Graphene of electrospinning fibre network can be sequentially completed
The preparation of film and the preparation of patterned Graphene film, electrospinning used are simple to operate, with low cost, easily controllable, institute
It is simple, with low cost, easily controllable with lifting technical operation, it is easy to carry out functionalization by graphene film obtained by the present apparatus
Modification, and graphene film is smooth, uniform, can it is fully wrapped around live electrospinning fibre, can be passed through using device described in the utility model
Change the regulation and control of the pattern simple realization graphene film patterning of electrospinning fibre.
Brief description of the drawings
Fig. 1 is the structural representation of the utility model embodiment electrostatic spinning apparatus;
Fig. 2 is the structural representation of the utility model embodiment pulling apparatus;
Fig. 3 is the AFM 3D of the patterned oxide graphene film obtained by the utility model embodiment one
Figure;
Fig. 4 is the SEM of the patterned oxide graphene film obtained by the utility model embodiment two
Figure.
In figure:1 needle tubing, 2 shower nozzles, 3 slides, 4 aluminium-foil papers, 5 operating platforms, 6 high pressure generators, 7 first lucite
Cover, 8 propulsion pumps, 9 connecting rods, 10 second plexiglass tents, 11 device for storing liquid, 12 support platforms.
Specific embodiment
With reference to Figure of description and specific embodiment, the utility model will be further described:
Embodiment one:
The device of patterned Graphene film, including the electrostatic being applied in combination are prepared on electrospinning fibre network with czochralski method
Device for spinning, pulling apparatus and reduction apparatus, electrostatic spinning apparatus, pulling apparatus and reduction apparatus are respectively positioned in locking device.
As shown in figure 1, the electrostatic spinning apparatus include high pressure generator 6, micro pump, needle tubing 1 and operating platform 5, institute
The lower section for stating operating platform 5 is provided with the lowering or hoisting gear of the regulation height of operating platform 5, and the table top of operating platform 5 is provided with carrying and carries
The aluminium-foil paper 4 of slide 3;The needle tubing 1 is located at the surface of aluminium-foil paper 4, and needle tubing 1 is connected with micro pump and is provided with spray in bottom
First 2;The positive pole of the high pressure generator 6 is connected with the needle tubing 1, and the negative pole of high pressure generator 6 is connected with the aluminium-foil paper 4.
As shown in Fig. 2 the pulling apparatus include propulsion pump 8, connecting rod 9 and device for storing liquid 11, the connecting rod 9 is longitudinally arranged
And with propulsion pump 8 be connected, device for storing liquid 11 be top end opening groove and positioned at the underface of connecting rod 9.
The inner space of the reduction apparatus is divided into the glass evacuated drier of two-layer, and reduction apparatus inside is capable of achieving vacuum
State.Operationally, hydrazine hydrate solution is located at the ground floor of reduction apparatus to reduction apparatus, and graphene oxide film is located at also original-pack
The second layer put, in whole reduction process, reduction apparatus are in vacuum state.
Electrostatic spinning apparatus, pulling apparatus and reduction apparatus are located on same workbench, in the present embodiment, electrostatic spinning
The first plexiglass tent 7 is covered with outside device, the outside of pulling apparatus is covered with the second plexiglass tent 10, also can be by electrostatic spinning
Device, pulling apparatus and reduction apparatus are covered in an openable plexiglass tent for entirety.Plexiglass tent will can be filled
Put and be isolated from the outside, and do not influence the observation to the device course of work, in the preparatory stage of preparation work, can be by plexiglass tent
Open, adjust the distance between height and connecting rod and device for storing liquid of operating platform etc., after the completion of preparation, device work
During, device should be isolated from the outside using plexiglass tent.
Described propulsion pump 8 is connected after being inverted with the connecting rod 9.After propulsion pump 8 is inverted, it is connected with connecting rod 9 by the pump housing
Connect, compared with being connected with pushing ram, connect more firm, it is to avoid the rocking of pushing ram, propulsion is also more stablized, so that even
The movement of bar 9 is more accurate.
To realize the effective support to advancing pump 8, described propulsion pump 8 is arranged in support platform 12.
The lowering or hoisting gear includes leading screw and nut sleeve, and the leading screw is arranged at four angles of operating platform bottom surface, institute
State nut sleeve to be engaged with leading screw respectively, the nut sleeve synchronous rotary drives the leading screw to do linear reciprocating motion.By silk
Thick stick transmission adjusts the height of operating platform, and accuracy is high, it is possible to achieve slight distance between aluminium-foil paper and the shower nozzle of needle tubing
Adjustment.
The nut sleeve is driven by drive gear, be provided between two adjacent drive gears travelling gear with
Drive gear synchronous rotary is realized, is connected by bevel gear transmission between active drive gear and rocking handle.
The vertical range between shower nozzle 2 on the aluminium-foil paper 4 and the needle tubing 1 is 15cm, and the needle tubing 1 is by glass system
Into the connecting rod 9 is glass bar.
The method for preparing patterned Graphene film using the device of the present embodiment is as follows:
Step (1):Weigh 0.02 gram of graphene oxide to be dissolved in 20 milliliters of ultra-pure waters, obtain uniformly within ultrasonically treated 2 hours
1.0 milligrams every milliliter of graphene oxide water solution.
Step (2):Weigh 1.5 grams of polyacrylonitrile to be dissolved in 10 milliliters of DMFs, in 55 degrees Celsius of temperature
Under degree, magnetic agitation is kept 12 hours with 300 rpms of rotating speed, obtain the N of 0.15 gram every milliliter of polyacrylonitrile, N- diformazans
Base formamide solution.
Step (3):The concentrated sulfuric acid and 9 milliliter 30% of hydrogen peroxide for measuring 21 milliliter 8% are configured to Piranha solution, by glass
Glass slide 3 is inserted after wherein etching 2 hours, is cleaned with ultra-pure water with ethanol successively after taking-up.
Step (4):It is solution that the toluene and 1 milliliter of 3- aminopropyl triethoxysilanes for measuring 29 milliliters are matched somebody with somebody, by anthropophagy
Slide 3 after fish solution etches is inserted and wherein processed 30 minutes, is cleaned with toluene, ethanol and ultra-pure water successively after taking-up.
Step (5):With with the DMF solution of polyacrylonitrile be raw material, with pretreated load glass
Piece 3 is carrier, carries out electrostatic spinning, and electrospinning parameters used are as follows:The material of needle tubing 1 is the glass needle tubing of disposable 1ml, by high pressure
The voltage of generator 6 is adjusted to 15kV, receives distance:Aluminium-foil paper 4 is with the vertical range of the shower nozzle 2 of needle tubing 1 on operating platform 5
15cm, goes out flow quantity for 1.0mL/h, and the size of aluminium-foil paper 4 is 20cm2。
Step (6):It is molten in obtained graphene oxide with the obtained slide for being covered with electrospinning fibre network of step (5)
In liquid, graphene oxide film is prepared using the method for lifting plated film, connecting rod used 9 is glass bar, and pull rate is controlled to 500
Nanometer is per second.
Step (7):The slide of graphene oxide film will be coated with to insert in glass evacuated drier, 2~3 are instilled and dripped
Vacuumized after closing hydrazine, reductase 12 takes out after 4 hours.
In the present embodiment, final obtained patterned oxide graphene film can be wrapped as shown in figure 3, smooth, uniform completely
Wrap electrospinning fibre.
Embodiment two:
The present embodiment is repeated no more with the identical feature of embodiment one, and the present embodiment feature different from embodiment one exists
In:The nut sleeve is driven by driving worm gear, and transmission worm gear is provided between two adjacent driving worm gears to realize
Worm gear synchronous rotary is driven, is connected by worm-and-wheel gear between active drive worm gear and rocking handle, rocking handle is arranged on worm screw
End.
The vertical range between shower nozzle on the aluminium-foil paper and the needle tubing is 20cm, and the needle tubing is made of plastics,
The connecting rod is teflon rod.
The method for preparing patterned Graphene film using the device of the present embodiment is as follows:
Step (1):Weigh 0.03 gram of graphene oxide to be dissolved in 20 milliliters of ultra-pure waters, obtain uniformly within ultrasonically treated 3 hours
1.5 milligrams every milliliter of graphene oxide water solution.
Step (2):Weigh 1.8 grams of polyacrylonitrile to be dissolved in 10 milliliters of DMFs, in 55 degrees Celsius of temperature
Under degree, magnetic agitation is kept 14 hours with 400 rpms of rotating speed, obtain the N of 0.18 gram every milliliter of polyacrylonitrile, N- diformazans
Base formamide solution.
Step (3):The concentrated sulfuric acid and 9 milliliter 30% of hydrogen peroxide for measuring 21 milliliter 8% are configured to Piranha solution, by glass
Glass slide 3 is inserted after wherein etching 2 hours, is cleaned with ultra-pure water with ethanol successively after taking-up.
Step (4):It is solution that the toluene and 1 milliliter of 3- aminopropyl triethoxysilanes for measuring 29 milliliters are matched somebody with somebody, by anthropophagy
Slide 3 after fish solution etches is inserted and wherein processed 30 minutes, is cleaned with toluene, ethanol and ultra-pure water successively after taking-up.
Step (5):With with the DMF solution of polyacrylonitrile be raw material, with pretreated load glass
Piece 3 is carrier, carries out electrostatic spinning, and electrospinning parameters used are as follows:The material of needle tubing 1 is the plastics needle tubing of disposable 1ml, pressure high
The raw voltage of device 6 is adjusted to 15kV, receives distance:Aluminium-foil paper 4 and the vertical range of the shower nozzle 2 of needle tubing 1 are 20cm on operating platform 5,
Go out flow quantity for 2.0mL/h, the size of aluminium-foil paper 4 is 30cm2。
Step (6):With the obtained slide for being covered with electrospinning fibre network in step (5), in obtained graphene oxide
In solution, graphene oxide film is prepared using the method for lifting plated film, connecting rod used 9 is teflon rod, pull rate
Be controlled to 250 nanometers it is per second.
Step (7):The slide of graphene oxide film will be coated with to insert in glass evacuated drier, 2~3 are instilled and dripped
Vacuumized after closing hydrazine, reduction is taken out after 48 hours.
In the present embodiment, final obtained patterned oxide graphene film can be wrapped as shown in figure 4, smooth, uniform completely
Wrap electrospinning fibre.
In the utility model, the lowering or hoisting gear of the lifting of control operation platform 5 is not limited to leading screw and nut described in embodiment
Set, can also be using other lowering or hoisting gears such as hydraulic cylinder, cylinder, electric pushrod, linear electric motors.
Preferred embodiment of the present utility model is the foregoing is only, is not whole embodiments of the present utility model,
Be not used to limit the utility model, all any modifications within spirit of the present utility model and principle, made, equivalent,
Improve etc., should be included within protection domain of the present utility model.
In addition to technical characteristic described in specification, remaining technical characteristic is technology known to those skilled in the art.