CN102817089A - Electrostatic spinning device with spinning nozzle capable of doing linear reciprocating motion - Google Patents
Electrostatic spinning device with spinning nozzle capable of doing linear reciprocating motion Download PDFInfo
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- CN102817089A CN102817089A CN2012100246572A CN201210024657A CN102817089A CN 102817089 A CN102817089 A CN 102817089A CN 2012100246572 A CN2012100246572 A CN 2012100246572A CN 201210024657 A CN201210024657 A CN 201210024657A CN 102817089 A CN102817089 A CN 102817089A
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Abstract
The invention belongs to the technical field of preparation of micro-nano fibers and relates to an electrostatic spinning device with a spinning nozzle capable of doing a linear reciprocatingmotion; a stainless steel needle head is fixed on an injector needle tube and is connected with the anode of a high-voltage direct-current power supply; the cathode of the high-voltage direct-current power supply is connected with an aluminum foil collector; the aluminum foil collector is fixed on a base of the device; the injector needle tube is fixed on one end of a linear motion rod; the linear motion rod runs through two parallel brackets and is capable of doing harmonic linear motion on the brackets; and the other end of the linear motion rod is connected with an organic glass plate by a crankshaft connection rod. The electrostatic spinning device has the advantages of multiple functions, concentrated spinning distribution and good ordering, small spinning distance, high yield, low working voltage, and the like.
Description
Technical field:
The invention belongs to the micro nanometer fiber preparing technical field; Relate to a kind of spinning nozzle linear reciprocating motion formula electrostatic spinning apparatus; Be used to prepare orderly arrangement, chi structure and twist structured micro nanometer fiber, as the material of nano photoelectric device, optics and the flexible device that can stretch.
Background technology:
At present; Electrostatic spinning technique is a kind ofly extensively paid close attention to, can be directly prepared the method for continuous fibers from polymer and composite solution or melt; Have advantages such as equipment is simple, cost is low, fiber yield is high, applied widely, gas and biology sensor, filter with separate, numerous areas such as Textile Engineering, medicament slow release, battery electrode material is with a wide range of applications.The principle of electrostatic spinning is: high voltage source provides high voltage; Between spinning nozzle and collecting board, set up a strong electrostatic field; Generally speaking, positive source is connected on the spinning nozzle, and negative pole is connected on (ground connection) on the collecting board; Operating voltage is generally the 10-30 kilovolt, and the spinning distance is generally 8-20 centimetre.Because the effect of high-voltage electrostatic field, spinning solution by polarized charged, are penetrated from spinning nozzle, by the fiber of electric field force slenderizing or generation splitting formation micro-nano-scale, be deposited on the collecting board at last then.The diameter and the experiment condition of fiber are closely related, generally between tens nanometers are to several microns.
The fiber of conventional electrostatic device for spinning preparation generally is a lack of alignment, and this has limited the application of electrospun fibers in some field.In recent years, the lot of domestic and international scientific research personnel is devoted to improve the conventional electrostatic spining technology to prepare the micro nanometer fiber of orderly arrangement architecture.At present, static textile technology and equipment relatively more commonly used have rotor (disk) collection, slit to collect or parallel pole collection, auxiliary external electric field or magnetic field collection, framework collection etc.For example, Chinese patent " electrostatic spinning apparatus " (application number: 200720067712.0) and " electrostatic spinning machine " (application number: what 200610125960.6) adopt is the collected in drums method; Chinese patent (application number: 200810102096.7) proposed the method that a kind of parallel pole gathering-device prepares ordered fiber; Document (Advanced Materials, 2007,19,3702-3706) then reported a kind of magnetoelectricity spinning technique that utilizes auxiliary magnetic field.In addition, Chinese patent " preparation facilities of a kind of orderly arrangement and chi structure the nanofiber " (patent No.: ZL201010184068.1) proposed the centrifugal electrostatic spinning technique that a kind of spinning nozzle rotatablely moves; Chinese patent (application number: 201110137420.0) also reported the preparation of a kind of improved framework collection electrostatic spinning technique arrangement and twisted wire structural fibers in order.But, more than these technical methods also come with some shortcomings: for example, the higher or spinning of operating voltage distance is bigger, and the orderly fiber arranged of preparation generally is linear structure, seldom has twist structured.And the distorted-structure fiber of arranging in order has application prospect at aspects such as the flexible electronic devices that can stretch.Particle is reciprocating motion on straight line, and its restoring force is directly proportional with displacement, and is in the opposite direction, is called simple harmonic motion; And simple harmonic motion can be regarded the motion of being done by projection on the particle vertical coordinate direction of principal axis of doing uniform circular motion as.Therefore in daily; Circular motion transforms through crankshaft-link rod can obtain linear reciprocating motion; This rectilinear motion is a kind of reciprocal simple harmonic oscillation in fact; It has had in mechanical systems such as lathe for machining, workshop streamline, automobile engine and various shaking platforms very widely uses, and is widely used in the classification or the sorting of powder such as metallurgical powder, chemical industry, fertilizer, abrasive material, medicine, grain and medium and small granularity material like common linear vibrating screen.
Summary of the invention:
The objective of the invention is to overcome the shortcoming that prior art exists; Seek to design the feasibility equipment that proposes the multiple special appearance structure micro-nano of a kind of novel preparation rice fiber; Be spinning nozzle linear reciprocating motion formula electrostatic spinning apparatus, linear structure micro nanometer fiber, chi structure fiber and the orderly distorted-structure fiber of arranging that this device adopts less spinning distance and lower operating voltage can successfully prepare orderly arrangement.
To achieve these goals, agent structure of the present invention comprises speed regulator, poly (methyl methacrylate) plate, dc brushless motor, crankshaft-link rod, rectilinear motion bar, support, syringe needle tube, stainless steel syringe needle, high-voltage DC power supply, aluminium foil collector and base; Hollow stainless steel syringe needle after the tip polishes is fixed on the medical syringe needle tube; The stainless steel syringe needle links to each other with the positive pole of high-voltage DC power supply; The negative pole of high-voltage DC power supply links to each other with the aluminium foil collector that aluminium foil is posted on the surface, and the aluminium foil collector is fixed on the base of device; Syringe needle tube is fixed in an end of rectilinear motion bar (length is 20 centimetres); The rectilinear motion bar is through two arranged side by side being fixed on the support on the base; The rectilinear motion bar can be done the simple harmonic quantity rectilinear motion on support; The other end of rectilinear motion bar links to each other with the poly (methyl methacrylate) plate that is fixed in dc brushless motor (length is 5.7 centimetres) through crankshaft-link rod, and speed regulator is used to control the rotating speed of dc brushless motor, and the rotating speed of dc brushless motor is read by the scale on the speed regulator; Dc brushless motor and speed regulator all are fixed on the base, the linear reciprocating motion part of the syringe needle tube that the formation spinning is used; When collecting fiber sheet glass is placed on the midpoint of stainless steel syringe needle distance that moving linearly passes through, the fastest according to the characteristics of simple harmonic motion in local stainless steel syringe needle movement velocity near mid point, and the acceleration minimum, be beneficial to the collection of spinning fibre.
When the present invention is used for arranging the preparation of linear structure fiber in order; Earlier add precursor solution in syringe needle tube in spinning; The distance of regulating between stainless steel syringe needle and the aluminium foil collector is 1-2 centimetre; On the aluminium foil collector, put slide, take clean, a dry paper to cover on the slide; Connect high-voltage DC power supply, regulation voltage is the 1.7-2.5 kilovolt, gives spinning needle tubing stopper pressure a little, and solution is slowly flowed out under the pressure of gravity and stopper, and static syringe needle begins spinning; After treating that spinning is stable; Connect the power supply of dc brushless motor, regulate the knob of speed regulator, making its rotating speed is about 200rpm; When near the stainless pin head straight reciprocating motion speed the mid point was suitable with stainless steel syringe needle spinning speed, electrospinning fibre was deposited on the aluminium foil collector with orderly fashion; Remove the paper that covers on slide, the collection of fiber sample picks up counting simultaneously on the beginning slide, after about 15 seconds, closes high-voltage DC power supply earlier, and the disable motor power supply can obtain orderly electrospinning fibre arranged in a straight line on the slide at this moment again.
The present invention is used for the preparation of chi structure fiber: substrate is placed on the aluminium foil collector collects spinning fibre; And after the spinning first time is accomplished, it is horizontally rotated 90 degree (or other angle) and carry out spinning again, obtain the square fiber mesh array that right-angled intersection or other angles intersect the most at last; If select suitable material; For example, ground floor is the organic or inorganic semiconductor nano fiber of n type, and the second layer is the organic or inorganic semiconductor fiber of p type; On substrate, just be assembled into the p-n junction array of Nano grade like this, aspect nano electron device, have very big application prospect.
The present invention is used for arranging in order the preparation of distorted-structure fiber: if under the constant situation of spinning distance, increase operating voltage; Can make the spinning solution polarization be with more multi-charge; The electric field force that charged jet receives in spinning process can be bigger, and the movement velocity when electrospinning fibre arrives collecting board can increase; When the fiber of high-speed motion bumps against on the collecting board staticly when getting off, the recoil strength of bump can make not completely crued as yet linear pattern fiber form distorted-structure; Spin on the liquid jet electrically charged amount increase can increase the bending or the moving unstability of whip of jet, cause the formation of distorted-structure fiber; According to above analysis, arrange in order in the linear structure fiber process, if operating voltage is brought up to the 3.0-4.0 kilovolt from the 1.7-2.5 kilovolt, the twist structured fiber of on collecting board, being arranged in order in preparation; The distorted-structure fiber can stretch in preparation and be with a wide range of applications aspect the flexible electronic device.
The present invention has compared with prior art that function is many, weaving distribute to be concentrated and order number, advantage such as the weaving distance is little, yield rate is high and operating voltage is low; Be used to prepare the fiber of orderly linear structure, chi structure and orderly three kinds of appearance structure of distorted-structure; Under the electric field force effect, spinning fibre is concentrated and is distributed in (wide about 5-10 millimeter) on the needle point moving direction, and the orderly degree of alignment of fiber is high; Work down in little spinning distance, thereby reduce in the fiber dropping process environment instability the influence of the fiber degree of order; Because prepared fiber only is distributed in the small space, has reduced fiber and has been scattered in other local probabilities, the ordered fiber yield rate is improved; Because the spinning distance is less, operating voltage can be reduced in 4 kilovolts, has improved the security of experiment.
Fig. 1 is the structural principle sketch map of apparatus of the present invention.
Fig. 2 is the scanning electron microscope sem photo of the orderly arrangement linear structure PVP fiber of the present invention's preparation.
Fig. 3 is the optical microscope photograph of the chi structure PVP fiber of the present invention's preparation.
Fig. 4 is the SEM photo of the orderly arrangement distorted-structure PVP fiber of the present invention's preparation.
The specific embodiment:
Below in conjunction with accompanying drawing and through embodiment the present invention is further specified.
The agent structure of present embodiment comprises speed regulator 1, poly (methyl methacrylate) plate 2, dc brushless motor 3, crankshaft-link rod 4, rectilinear motion bar 5, support 6, syringe needle tube 7, stainless steel syringe needle 8, high-voltage DC power supply 9, aluminium foil collector 10 and base 11; Hollow stainless steel syringe needle 8 after the tip polished is fixed on the medical syringe needle tube 7; Stainless steel syringe needle 8 links to each other with the positive pole of high-voltage DC power supply 9; The negative pole of high-voltage DC power supply 9 links to each other with the aluminium foil collector 10 that aluminium foil is posted on the surface, and the aluminium foil collector is fixed on the base 11 of device; Syringe needle tube 7 is fixed in an end of rectilinear motion bar 5 (length is 20 centimetres); Rectilinear motion bar 5 is through two arranged side by side being fixed on the support 6 on the base 11; Rectilinear motion bar 5 can be done the simple harmonic quantity rectilinear motion on support 6; The other end of rectilinear motion bar 5 links to each other with the poly (methyl methacrylate) plate that is fixed in dc brushless motor 32 (length is 5.7 centimetres) through crankshaft-link rod 4, and speed regulator 1 is used to control the rotating speed of dc brushless motor 3, and the rotating speed of dc brushless motor 3 is read by the scale on the speed regulator; Dc brushless motor 3 all is fixed on the base 11 with speed regulator 1, the linear reciprocating motion part of the syringe needle tube 7 that the formation spinning is used; When collecting fiber sheet glass is placed on the midpoint of stainless steel syringe needle 8 distances that moving linearly passes through, the fastest according to the characteristics of simple harmonic motion in local stainless steel syringe needle 8 movement velocitys near mid point, and the acceleration minimum, be beneficial to the collection of spinning fibre.
The selected spinning precursor solution of present embodiment is that mass percent is polyvinylpyrrolidone (PVP) solution of 13wt%; Elder generation's weighing 1.3 gram PVP (molecular weight 1300000) join under magnetic agitation in the 8.7 gram absolute ethyl alcohols; The room temperature lower magnetic force stirred 5 hours; Static then half an hour, get final product the 13wt%PVP electrostatic spinning precursor solution of homogeneous transparent.
Embodiment 1: the preparation of arranging linear structure PVP fiber in order: extract 1 milliliter of left and right sides PVP precursor solution with Dispette and inject spinning with in the syringe needle tube 7; High-voltage DC power supply 9 positive poles connect stainless steel syringe needle 8, and negative pole connects aluminium foil collector 10, and the distance of regulating stainless steel syringe needle 8 and 1 aluminium foil collector 10 is 1 centimetre; On collector, put slide; Take clean, a dry paper to cover on the slide, connect, make its switch be in " ON " state high-voltage DC power supply 9; Regulation voltage is 1.8 kilovolts, and static syringe needle begins spinning; Connect the power supply of dc brushless motor 3, the knob of rotation speed regulator 1, making rotating speed is 200rpm; Static syringe needle begins to do reciprocal rectilinear motion, treat stabilization of speed in a few second after, take away the paper that is covered on the cover glass fast; And pick up counting, after 15 seconds, close high-voltage DC power supply 9; Make its switch part in " OFF " state, close the power supply of dc brushless motor 3 again, electricity spins end; Get the sample of collecting on the slide, observe with scanning electron microscope sem, the result is as shown in Figure 2, from figure, can see that the pattern of spinning fibre is good, and the depth of parallelism of arrangement is higher, and spun fibre diameter is about the 1.5-3 micron under this condition, and thickness is more even.
Embodiment 2: the preparation of chi structure PVP fiber: the PVP fiber for preparing orderly arrangement earlier according to the step among the embodiment 1; Then the sample half-twist of collecting being repeated electricity again with same condition and step spins once; Obtain the PVP fiber of chi structure, the optical microscope photograph of its sample is as shown in Figure 3.
Embodiment 3: the preparation of arranging distorted-structure PVP fiber in order: the voltage of regulating among the embodiment 1 is 3.5 kilovolts; Other step is constant; Arranged twist structured PVP fiber at last in order, the SEM photo of its sample is as shown in Figure 4, can find out that the fiber that makes is distorted-structure and arranges in order; But because the distribution of vimentin filament on two-dimentional yardstick causes existing between the fiber mutual crossover phenomenon.
Claims (4)
1. a spinning nozzle linear reciprocating motion formula electrostatic spinning apparatus is characterized in that comprising speed regulator, poly (methyl methacrylate) plate, dc brushless motor, crankshaft-link rod, rectilinear motion bar, support, syringe needle tube, stainless steel syringe needle, high-voltage DC power supply, aluminium foil collector and base; Hollow stainless steel syringe needle after the tip polishes is fixed on the medical syringe needle tube; The stainless steel syringe needle links to each other with the positive pole of high-voltage DC power supply; The negative pole of high-voltage DC power supply links to each other with the aluminium foil collector that aluminium foil is posted on the surface, and the aluminium foil collector is fixed on the base of device; Syringe needle tube is fixed in rectilinear motion bar one end; The rectilinear motion bar is through two arranged side by side being fixed on the support on the base; The rectilinear motion bar can be done the simple harmonic quantity rectilinear motion on support; The other end of rectilinear motion bar links to each other with the poly (methyl methacrylate) plate that is fixed in dc brushless motor through crankshaft-link rod, and speed regulator is used to control the rotating speed of dc brushless motor, and the rotating speed of dc brushless motor is read by the scale on the speed regulator; Dc brushless motor and speed regulator all are fixed on the base, the linear reciprocating motion part of the syringe needle tube that the formation spinning is used; When collecting fiber sheet glass is placed on the midpoint of stainless steel syringe needle distance that moving linearly passes through, the fastest according to the characteristics of simple harmonic motion in local stainless steel syringe needle movement velocity near mid point, and the acceleration minimum, be beneficial to the collection of spinning fibre.
2. a kind of spinning nozzle linear reciprocating motion formula electrostatic spinning apparatus according to claim 1; When it is characterized in that being used for arranging the preparation of linear structure fiber in order; Earlier add precursor solution in syringe needle tube in spinning; The distance of regulating between stainless steel syringe needle and the aluminium foil collector is 1-2 centimetre, on the aluminium foil collector, puts slide, takes clean, a dry paper to cover on the slide; Connect high-voltage DC power supply, regulation voltage is the 1.7-2.5 kilovolt, gives spinning needle tubing stopper pressure a little, and solution is slowly flowed out under the pressure of gravity and stopper, and static syringe needle begins spinning; After treating that spinning is stable; Connect the power supply of dc brushless motor, regulate the knob of speed regulator, making its rotating speed is 200rpm; When near the stainless pin head straight reciprocating motion speed the mid point was suitable with stainless steel syringe needle spinning speed, electrospinning fibre was deposited on the aluminium foil collector with orderly fashion; Remove the paper that covers on slide, the collection of fiber sample picks up counting simultaneously on the beginning slide, after 15 seconds, closes high-voltage DC power supply earlier, and the disable motor power supply can obtain orderly electrospinning fibre arranged in a straight line on the slide at this moment again.
3. a kind of spinning nozzle linear reciprocating motion formula electrostatic spinning apparatus according to claim 1; It is characterized in that being used for the preparation of chi structure fiber: substrate is placed on the aluminium foil collector collects spinning fibre; And after first time spinning is accomplished, it is horizontally rotated 90 degree or other angle is carried out spinning again, obtain the square fiber mesh array that right-angled intersection or other angles intersect the most at last; Selecting ground floor is n type organic or inorganic semiconductor nano fiber, and the second layer is a p type organic or inorganic semiconductor fiber, on substrate, is assembled into the p-n junction array of Nano grade.
4. a kind of spinning nozzle linear reciprocating motion formula electrostatic spinning apparatus according to claim 1; It is characterized in that being used for arranging in order the preparation of distorted-structure fiber: under the constant situation of spinning distance, increase operating voltage; Make the spinning solution polarization be with electric charge; The electric field force that charged jet receives in spinning process, the movement velocity when electrospinning fibre arrives collecting board increases; The fiber of high-speed motion bumps against on the collecting board when static, and the recoil strength of bump makes not completely crued as yet linear pattern fiber form distorted-structure; On the spinning solution jet electrically charged amount increase the bending or the moving unstability of whip that can increase jet, cause the formation of distorted-structure fiber; Arrange in order in the linear structure fiber process in preparation, operating voltage is brought up to the 3.0-4.0 kilovolt from the 1.7-2.5 kilovolt, the twist structured fiber of on collecting board, being arranged in order; The distorted-structure fiber is used for preparing the flexible electronic device that can stretch.
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| CN104120546A (en) * | 2014-08-08 | 2014-10-29 | 青岛大学 | Preparation method for flexible stretching device of two-dimensional reticular structure |
| CN104711685A (en) * | 2015-02-08 | 2015-06-17 | 福建师范大学 | Multifunctional electrostatic spinning equipment |
| CN104711685B (en) * | 2015-02-08 | 2017-01-25 | 福建师范大学 | Multifunctional electrostatic spinning equipment |
| CN104695031A (en) * | 2015-02-12 | 2015-06-10 | 青岛博纳生物科技有限公司 | Electrostatic spinning device |
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