CN206279382U - The device of patterned Graphene film is prepared on electrospinning fibre network with czochralski method - Google Patents

The device of patterned Graphene film is prepared on electrospinning fibre network with czochralski method Download PDF

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Publication number
CN206279382U
CN206279382U CN201621124411.2U CN201621124411U CN206279382U CN 206279382 U CN206279382 U CN 206279382U CN 201621124411 U CN201621124411 U CN 201621124411U CN 206279382 U CN206279382 U CN 206279382U
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Prior art keywords
graphene film
czochralski method
fibre network
electrospinning fibre
patterned graphene
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CN201621124411.2U
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Chinese (zh)
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冯章启
王婷
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Nanjing Daniu New Material Technology Co ltd
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Suzhou New Silk Mstar Technology Ltd
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Abstract

The utility model discloses a kind of device for preparing patterned Graphene film on electrospinning fibre network with czochralski method, belong to the preparation field of composite nano-fiber membrane, its structure includes the electrostatic spinning apparatus, pulling apparatus and the reduction apparatus that are applied in combination, and electrostatic spinning apparatus, 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, and the pulling apparatus include propulsion pump, connecting rod and device for storing liquid, and the inner space of the reduction apparatus is divided into two-layer, and reduction apparatus inside is capable of achieving vacuum state.Ingenious reasonable, the used electrospinning of device of the present utility model is simple, with low cost, easily controllable with lifting technical operation, gained graphene film is uniform complete, be easy to carry out functional modification, and can simply be regulated and controled by controlling the pattern of electrospinning fibre network to be patterned, it is that the further research and development of graphene film and application create condition.

Description

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.

Claims (10)

1. the device of patterned Graphene film is prepared on electrospinning fibre network with czochralski method, it is characterized in that, including combination make Electrostatic spinning apparatus, pulling apparatus and reduction apparatus, electrostatic spinning apparatus, pulling apparatus and reduction apparatus are respectively positioned on closing In device;
The electrostatic spinning apparatus include high pressure generator, micro pump, needle tubing and operating platform, are set below the operating platform There is the lowering or hoisting gear of regulation operating platform height, the table top of operating platform is provided with the aluminium-foil paper for carrying slide;The needle tubing Positioned at the surface of aluminium-foil paper, needle tubing is connected with micro pump and is provided with shower nozzle in bottom;The positive pole of the high pressure generator with The needle tubing is connected, 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, liquid storage Device 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.
2. the device for preparing patterned Graphene film on electrospinning fibre network with czochralski method according to claim 1, It is characterized in that, described propulsion pump is connected after being inverted with the connecting rod.
3. the device for preparing patterned Graphene film on electrospinning fibre network with czochralski method according to claim 1, It is characterized in that, described locking device is openable plexiglass tent.
4. the device for preparing patterned Graphene film on electrospinning fibre network with czochralski method according to claim 1, It is characterized in that, described propulsion pump is arranged in support platform.
5. the device for preparing patterned Graphene film on electrospinning fibre network with czochralski method according to claim 1, It is characterized in that, 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.
6. the device for preparing patterned Graphene film on electrospinning fibre network with czochralski method according to claim 5, It is characterized in that, the nut sleeve is driven by drive gear, and travelling gear is provided between two adjacent drive gears To realize drive gear synchronous rotary, it is connected by bevel gear transmission between active drive gear and rocking handle.
7. the device for preparing patterned Graphene film on electrospinning fibre network with czochralski method according to claim 5, It is characterized in that, the nut sleeve is driven by driving worm gear, and transmission worm gear is provided between two adjacent driving worm gears To realize driving worm gear synchronous rotary, be connected by worm-and-wheel gear between active drive worm gear and rocking handle, rocking handle is installed In the end of worm screw.
8. the device for preparing patterned Graphene film on electrospinning fibre network with czochralski method according to claim 1, It is characterized in that, the vertical range between shower nozzle on the aluminium-foil paper and the needle tubing is 15~20cm.
9. the device for preparing patterned Graphene film on electrospinning fibre network with czochralski method according to claim 1, It is characterized in that, the needle tubing is made up of glass or plastics.
10. the device for preparing patterned Graphene film on electrospinning fibre network with czochralski method according to claim 1, It is characterized in that, the connecting rod is glass bar or teflon rod.
CN201621124411.2U 2016-10-14 2016-10-14 The device of patterned Graphene film is prepared on electrospinning fibre network with czochralski method Expired - Fee Related CN206279382U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107937996A (en) * 2017-12-25 2018-04-20 大连民族大学 The environment control method of electrospinning fibre sample collection device

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107937996A (en) * 2017-12-25 2018-04-20 大连民族大学 The environment control method of electrospinning fibre sample collection device
CN107937996B (en) * 2017-12-25 2019-07-19 大连民族大学 The environment control method of electrospinning fibre sample collection device

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