CN101818382A - Electrostatic spinning device for preparing oriented carbon nanotube reinforced polymer-based nano fiber - Google Patents
Electrostatic spinning device for preparing oriented carbon nanotube reinforced polymer-based nano fiber Download PDFInfo
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- CN101818382A CN101818382A CN200910117705A CN200910117705A CN101818382A CN 101818382 A CN101818382 A CN 101818382A CN 200910117705 A CN200910117705 A CN 200910117705A CN 200910117705 A CN200910117705 A CN 200910117705A CN 101818382 A CN101818382 A CN 101818382A
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Abstract
The invention discloses an electrostatic spinning device for preparing an oriented carbon nanotube reinforced polymer-based nano fiber, and aims to realize highly oriented arrangement of CNTs (carbon nanotubes) in a polymer-based nano fiber to obtain the polymer-based nano fiber which has smooth surface appearance, no hole and uniformly-distributed diameter. The electrostatic spinning device comprises a liquid storage device 2, a quartz capillary orienting device connected below the liquid storage device 2, and a disc-shaped rotary collecting plate 5 and a motor M1 which are connected by a rotation shaft, wherein a high-voltage DC power supply 6 is correspondingly connected between the quartz capillary orienting device and the disc-shaped rotary collecting plate 5; one end of a quartz capillary tube 3 in the quartz capillary orienting device is connected with the liquid storage device 2; and a steel spinneret 4 into which thin copper wires 4a are embedded is arranged at the other end of the quartz capillary tube.
Description
Technical field
The present invention relates to prepare the device that CNT is used.
Background technology
CNT (CNTs) was found by Japanese scholar lijima in 1991, because it has performances such as very large draw ratio and good mechanics, electricity, calorifics, nanofiber strengthens body and conductive fiber adds material so can be used as, especially when CNTs high orientation in polymeric matrix was arranged, its above-mentioned performance will obtain more fully effectively performance.
Sundaray etc. have realized that by electrostatic spinning process CNTs tentatively aligns (Bibekananda Sundaray in the polymethyl methacrylate polymer-based nano fibers such as (PMMA), et al.APPLI-ED PHYSICS LETTERS.2006,88,143114), promptly by charged Polymer Solution or melt are flowed in electrostatic field and distortion, solidify through solvent evaporation or cooling then and obtain fibrous material, prepare nano-scale fiber.But the degree of aligning of the CNTs in the polymer-based nano fiber of its gained is not high; And in the electrostatic spinning process, low excessively when the concentration of solution or melt, when viscosity is too small, can make the surface topography of the polymer-based nano fiber that obtains rough, be prone to hole, beading structure and fiber and easily be sticked together, simultaneously the diameter skewness of the fiber of gained.
Summary of the invention
The objective of the invention is to realize the high orientation arrangement of CNTs in the polymer-based nano fiber, obtain the polymer-based nano fiber that smooth, no hole of surface topography and diameter are evenly distributed.
The technical scheme that the present invention addresses the above problem employing is: the electrostatic spinning apparatus of preparation oriented carbon nanotube reinforced polymer-based nano fiber, include device for storing liquid 2, be connected the quartz capillary bearing unit under the device for storing liquid 2, by the discoid rotation collecting board 5 and the motor M of rotating shaft connection
1, correspondence is connected with high-voltage DC power supply 6 between quartz capillary bearing unit and the discoid rotation collecting board 5, and quartz capillary 3 one ends in the quartz capillary bearing unit are connected with device for storing liquid 2, and the other end is equipped with the steel spinning head 4 that embeds thin copper wire 4a.
In the technical solution of the present invention: the length of described steel spinning head 4 is 30mm, the thick 100 μ m of the outer 4b of steel, the internal diameter 4c of steel spinning head 4 is slightly larger than the external diameter of quartz capillary 3, steel spinning head 4 is embedded with four thin copper wire 4a, on steel spinning head 4 outer walls of steel spinning head 4 and quartz capillary 3 junctions power supply access port 4d is arranged.
But in the technology solution of the present invention: the internal diameter of described quartz capillary 3 is that 200 μ m～300 μ m, length are 2m～5m, and quartz capillary 3 outer wrap have the polyamide coating layer of 50 μ m thickness.
In the technical solution of the present invention: described device for storing liquid 2 is provided with supercharging device 1.
In the technical solution of the present invention: described discoid rotation collecting board 5 thickness are 5mm, outside with the aluminium film, discoid rotation collecting board 5 is when work, the linear velocity at discoid rotation collecting board 5 edges is 5m/s～45m/s, and the distance between the steel spinning head 4 is 10cm～20cm.
In the technical solution of the present invention: the positive pole of described high-voltage DC power supply 6 is connected with the power supply access port 4d of steel spinning head 4 with lead, and the negative pole of high-voltage DC power supply 6 is connected with discoid rotation collecting board 5 with lead.
In the technical solution of invention: the diameter of described thin copper wire 4a is 20 μ m, holding row level with both hands at the spinning nozzle of steel spinning head 4 arranges, is separated from each other, and stretch out the spinning nozzle 2mm of steel spinning head 4, thin copper wire 4a stretches out and is fixed on the outer wall of steel spinning head 4 at the other end relative with the spinning nozzle end of steel spinning head 4, connects with the power supply access port 4d of steel spinning head 4.
Compared with prior art, the present invention has following characteristics:
1. the present invention adopts the combination physical field that electric field and flow field form in the electrostatic spinning process, has improved CNTs degree of orientation in the polymer-based nano fiber.
Promptly between the device for storing liquid 2 of electrostatic spinning apparatus and power supply 6, add the quartz capillary bearing unit of overlength, make electrostatic spinning solution or melt pass through quartz capillary 3 parts with the form of Poiseuille stream, the flow velocity height of capillary center is low near capillary wall place flow velocity.In this process, because the existence of current gradient, make CNTs only when longshore current line direction is arranged, suffered rotating torque just equals zero.Simultaneously, according to finding the solution the analysis of Fokker-Planck equation, the flow process of current gradient field is long more, and CNTs longshore current speed direction orientation advantage is obvious more.It is 2m-5m that the present invention selects length for use, during the quartz capillary 3 of internal diameter 200 μ m-300 μ m, can guarantee that before carrying out electrostatic spinning CNTs has obtained certain orientation advantage in advance, thereby improve its degree of orientation in end product.
2. the present invention is in the electrostatic spinning process, and a. utilizes thin copper wire to make near the electric field line of spinning nozzle more concentrated, reduces to spray the critical voltage of silk; B. utilize the capillarity between spinning solution or melt and copper wire, make taylor cone result from the thin copper wire tip, reduce actual spinning head bore and taylor cone bottom surface diameter, strengthen composite nano fiber to obtain thinner CNTs.
Description of drawings
Fig. 1 is a modified electrostatic spinning device structure schematic diagram, Fig. 2 is for embedding the spinning head structural representation that thin copper wire is arranged, Fig. 3 is the sectional view of quartz capillary, Fig. 4 is for embedding the sectional view of the steel spinning head AB face that thin copper wire is arranged among Fig. 2, Fig. 5 is the SEM photo of CNTs/PMMA polymer-based nano fiber, and Fig. 6 is the TEM photo of CNTs/PMMA polymer-based nano fiber.
The specific embodiment
Fig. 1 is expression the present invention, promptly prepare the structural representation that aligned carbon nanotube strengthens the electrostatic spinning apparatus of polymer-based nano fiber, as shown in Figure 1, the present invention includes: device for storing liquid 2, be connected the quartz capillary bearing unit under the device for storing liquid 2, by the discoid rotation collecting board 5 and the motor M of rotating shaft connection
1, correspondence is connected with high-voltage DC power supply 6 between quartz capillary bearing unit and the discoid rotation collecting board 5, and quartz capillary 3 one ends in the quartz capillary bearing unit are connected with device for storing liquid 2, and the other end is equipped with the steel spinning head 4 that embeds thin copper wire 4a.
Fig. 2 is the structural representation that embeds the steel spinning head 4 that thin copper wire 4a is arranged among Fig. 1, Fig. 4 is the sectional view that embeds the steel spinning head 4A-B face that thin copper wire 4a is arranged among Fig. 2, as shown in Figure 2, the length of described steel spinning head 4 is the external diameter that 30mm, internal diameter 4c are slightly larger than quartz capillary 3, on steel spinning head 4 outer walls of steel spinning head 4 and quartz capillary 3 junctions power supply access port 4d is arranged; Steel spinning head 4 is embedded with four thin copper wire 4a, and stretches out the spinning nozzle 2mm of steel spinning head 4; Thin copper wire 4a stretches out and is fixed on the outer wall of steel spinning head 4 at the other end relative with the spinning nozzle end of steel spinning head 4, connects with the power supply access port 4d of steel spinning head 4.Thick 100 μ m of the outer 4b of steel as shown in Figure 4, the diameter of thin copper wire 4a is 20 μ m, and holds row level with both hands at the spinning nozzle of steel spinning head 4 and arrange, be separated from each other.
Fig. 3 is the sectional view of quartz capillary 4a among Fig. 2, is that a kind of internal diameter is the high suppleness quartz capillary of the polyamide of 200 μ m～300 μ m, outer wrap 50 μ m thickness.
Figure 5 shows that the SEM photo of gained CNTs/PMMA polymer-based nano fiber.
Figure 6 shows that the TEM photo of gained CNTs/PMMA polymer-based nano fiber.
Steel spinning head of the present invention (4) by lead link to each other with high-voltage DC power supply 6 positive terminals, discoid rotation collecting board 5 links to each other with high-voltage DC power supply 6 negative pole ends by lead, when high-voltage DC power supply 6 is opened, between steel spinning head 6 and discoid rotation collecting board 5, produce static electric field.
After producing static electric field, supercharging device 1 provides pressure to make spinning solution or melt-flow in the device for storing liquid 2 have a Flow Field Distribution and CNTs to be subjected to the rotating torque effect when quartz capillary 3 in the flow field, promptly in the flow field the suffered rotating torque of CNTs be proportional to CNTs and streamline angle sine value square, and the spatial orientation of CNTs in the flow field distributes and obeys the Fokker-Planck equation, thereby makes CNTs obtain the spatial orientation advantage in advance before electrostatic spinning.
Discoid rotation collecting board 5 of the present invention, employing be the wide and outside narrow collecting board with the aluminium film of 5mm, with the electric field in the further constraint spinning zone, realize the oriented and ordered collection of composite nano fiber.
The linear velocity on surface was that 5m/s～45m/s is adjustable when discoid rotation collecting board 5 of the present invention was worked.When the beginning electrostatic spinning, by different motor M
1Selection, the evaporation rate of solvent or melt is complementary when making the linear velocity on discoid rotation collecting board 5 surfaces and jet deposition, and then obtains being wrapped in the fiber that aligns at disk border place.
Distance between discoid rotation collecting board 5 of the present invention and the steel spinning head 4 is 10cm～20cm, when electrostatic spinning, by regulating the distance between discoid rotation collecting board 5 and the steel spinning head 4, make selected flux or melt when jet deposits, can under corresponding electric field action power, obtain enough aerial running times, the abundant volatilization of final acquisition moulding, the nanofiber that the high orientation that smooth, no hole of pattern and diameter are evenly distributed is arranged.
Provide below and utilize above-mentioned improvement electrostatic spinning apparatus to prepare the method embodiment that high orientation CNTs strengthens composite nano fiber:
After Single Walled Carbon Nanotube (SWNTs) purification, getting the 0.1g product adds in the 33ml dimethyl formamide (DMF), ultrasonic dispersion 1 hour, add 2g polymethyl methacrylate (PMMA then, mean molecule quantity is greater than 1000000) particle, dispersed with stirring is injected the device for storing liquid of the said equipment after 48 hours, the internal diameter of flowing through is 200 μ m-300 μ m, length is that the quartz capillary of 2m～5m is to the steel spinning head, regulate the about 15kV of high-voltage DC power supply voltage value, opening motor makes the linear velocity on discoid rotation collecting board surface reach 5m/s-45m/s, the diameter of discoid rotation collecting board is 140mm, and distance is 10cm between spinning head and collecting board, carries out spinning with the constant flow rate of 2mL/h, can get diameter at last less than 100nm, ganoid ultra-long nano fiber, as Fig. 5, shown in Figure 6.
Claims (7)
1. the electrostatic spinning apparatus of preparation oriented carbon nanotube reinforced polymer-based nano fiber includes device for storing liquid (2), is connected the quartz capillary bearing unit under the device for storing liquid (2), by the discoid rotation collecting board (5) and the motor (M of rotating shaft connection
1), correspondence is connected with high-voltage DC power supply (6) between quartz capillary bearing unit and the discoid rotation collecting board (5), it is characterized in that: quartz capillary (3) one ends in the described quartz capillary bearing unit are connected with device for storing liquid (2), and the other end is equipped with the steel spinning head (4) that embeds thin copper wire (4a).
2. the electrostatic spinning apparatus of preparation oriented carbon nanotube reinforced polymer-based nano fiber according to claim 1, it is characterized in that: the length of described steel spinning head (4) is the thick 100 μ m of 30mm, steel skin (4b), the internal diameter (4c) of steel spinning head (4) is slightly larger than the external diameter of quartz capillary (3), steel spinning head (4) is embedded with four thin copper wires (4a), on steel spinning head (4) outer wall of steel spinning head (4) and quartz capillary (3) junction power supply access port (4d) is arranged.
3. the electrostatic spinning apparatus of preparation oriented carbon nanotube reinforced polymer-based nano fiber according to claim 1, it is characterized in that: the internal diameter of described quartz capillary (3) is that 200 μ m～300 μ m, length are 2m～5m, and quartz capillary (3) outer wrap has the polyamide coating layer of 50 μ m thickness.
4. the electrostatic spinning apparatus of preparation oriented carbon nanotube reinforced polymer-based nano fiber according to claim 1 is characterized in that: described device for storing liquid (2) is provided with supercharging device (1).
5. the electrostatic spinning apparatus of preparation oriented carbon nanotube reinforced polymer-based nano fiber according to claim 1, it is characterized in that: described discoid rotation collecting board (5) thickness is 5mm, outside with the aluminium film, discoid rotation collecting board (5) is when work, its surperficial linear velocity is 5m/s～45m/s, and the distance between the steel spinning head (4) is 10cm～20cm.
6. the electrostatic spinning apparatus of preparation oriented carbon nanotube reinforced polymer-based nano fiber according to claim 1, it is characterized in that: the positive pole of described high-voltage DC power supply (6) is connected with the power supply access port (4d) of steel spinning head (4) with lead, and the negative pole of high-voltage DC power supply (6) is connected with discoid rotation collecting board (5) with lead.
7. a kind of electrostatic spinning apparatus for preparing oriented carbon nanotube reinforced polymer-based nano fiber according to claim 2, it is characterized in that: the diameter of described thin copper wire (4a) is 20 μ m, holding row level with both hands at the spinning nozzle of steel spinning head (4) arranges, is separated from each other, and stretch out the spinning nozzle 2mm of steel spinning head (4), thin copper wire (4a) stretches out and is fixed on the outer wall of steel spinning head (4) at the other end relative with the spinning nozzle end of steel spinning head (4), with power supply access port (4d) connection of steel spinning head (4).
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| CN200910117705A CN101818382A (en) | 2009-12-09 | 2009-12-09 | Electrostatic spinning device for preparing oriented carbon nanotube reinforced polymer-based nano fiber |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102794952A (en) * | 2012-06-28 | 2012-11-28 | 北京化工大学常州先进材料研究院 | Preparation method of CFRP (Carbon Fiber Reinforced Plastics) composite material with height orientation MWNTs and synchronously reinforced and toughened by hybrid nanofiber |
| CN104818536A (en) * | 2015-04-03 | 2015-08-05 | 西安交通大学 | Directional arranged electrostatic spinning fiber preparation apparatus and preparation method |
| CN105506858A (en) * | 2016-01-26 | 2016-04-20 | 东北林业大学 | Method for preparing cellulose-reinforced nano-composite fiber membrane by electrostatic spinning |
| CN106854779A (en) * | 2016-12-15 | 2017-06-16 | 华南理工大学 | A kind of carbon nano-tube oriented enhanced carbon fibre composite and preparation method thereof |
-
2009
- 2009-12-09 CN CN200910117705A patent/CN101818382A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102794952A (en) * | 2012-06-28 | 2012-11-28 | 北京化工大学常州先进材料研究院 | Preparation method of CFRP (Carbon Fiber Reinforced Plastics) composite material with height orientation MWNTs and synchronously reinforced and toughened by hybrid nanofiber |
| CN102794952B (en) * | 2012-06-28 | 2015-02-18 | 北京化工大学常州先进材料研究院 | Preparation method of CFRP (Carbon Fiber Reinforced Plastics) composite material with height orientation MWNTs and synchronously reinforced and toughened by hybrid nanofiber |
| CN104818536A (en) * | 2015-04-03 | 2015-08-05 | 西安交通大学 | Directional arranged electrostatic spinning fiber preparation apparatus and preparation method |
| CN104818536B (en) * | 2015-04-03 | 2017-06-06 | 西安交通大学 | A kind of electrospun fibers preparation facilities for aligning and preparation method |
| CN105506858A (en) * | 2016-01-26 | 2016-04-20 | 东北林业大学 | Method for preparing cellulose-reinforced nano-composite fiber membrane by electrostatic spinning |
| CN105506858B (en) * | 2016-01-26 | 2017-11-14 | 东北林业大学 | The method that electrostatic spinning prepares cellulose enhancing nano-composite fiber film |
| CN106854779A (en) * | 2016-12-15 | 2017-06-16 | 华南理工大学 | A kind of carbon nano-tube oriented enhanced carbon fibre composite and preparation method thereof |
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Open date: 20100901 |