CN105274734A - Method for preparing three-dimensional micro-nano fiber membrane based on ice balls as templates - Google Patents
Method for preparing three-dimensional micro-nano fiber membrane based on ice balls as templates Download PDFInfo
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- CN105274734A CN105274734A CN201510852061.5A CN201510852061A CN105274734A CN 105274734 A CN105274734 A CN 105274734A CN 201510852061 A CN201510852061 A CN 201510852061A CN 105274734 A CN105274734 A CN 105274734A
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- electrospun
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- ice hockey
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Abstract
The invention discloses a method for preparing a three-dimensional micro-nano fiber membrane based on ice balls as templates. The method includes the steps that super-hydrophobic aluminum foil is placed on a refrigeration plate, water is dripped onto the super-hydrophobic aluminum foil to be coagulated into the ice balls, then electrostatic spinning is performed at a normal temperature with the aluminum foil as a collection device and the ice balls as the templates, and the three-dimensional micro-nano fiber membrane is obtained. According to the method, compared with metal templates, the ice balls serving as the templates are easier to control and lower in manufacturing cost; more importantly, it is not needed to remove the templates one by one manually after spinning is completed, it is only needed to place the three-dimensional micro-nano fiber membrane at a room temperature for certain time, and then the ice balls can disappear automatically, so that the whole process of preparing the three-dimensional micro-nano fiber membrane is simplified; besides, the ice balls are good in biocompatibility and free of metal residues and do not interfere with an electrostatic spinning electric field.
Description
Technical field
The invention belongs to electricity spinning fibre field of material technology, being specifically related to a kind of is template with ice hockey, utilizes electrostatic spinning technique to prepare the method for three-dimensional Electrospun material.
Background technology
In recent years, at home and abroad scientific and technical research field is always quite concerned to utilize electrostatic spinning technique to prepare micro nanometer fiber material.Electrostatic spinning technique is simple, easy to operate because of itself device, in prepared by one-dimensional micro-nanometer material, possess obvious advantage.The micro nanometer fiber of preparation has the features such as large L/D ratio, high surface energy and high porosity, is thus all subject to very big high praise in fields such as physics, chemistry, biomedicine and textile industries.Three-dimensional micro-nano structure is prepared from one-dimensional micro-nanometer fiber basis, compared to one-dimensional micro-nanometer fiber, three-dimensional micro-nano structure has space support effect, and this just determines three-dimensional micro-nano structure material has and apply widely in biomedicine etc.The method preparing three-dimensional micro-nano structure has multiple, but process more complicated, wherein normal using metallic object as fiber collecting pole, make fiber laydown on it, thus obtain micro nanometer fiber film, but easily produce metal residues with metal as template, and electric interfering field.
Summary of the invention
Technical problem to be solved by this invention is to overcome the shortcoming existed using metal as Template preparation three-dimensional micro-nano fiber, provide a kind of simple to operate, cost is low, template easily except, without the method preparing three-dimensional micro-nano tunica fibrosa of metal residual.
Solving the problems of the technologies described above adopted technical scheme is: loaded in Electrospun syringe by Electrospun solution, Electrospun spinning head is connected with high voltage source; Superhydrophobic aluminum foil is placed on cold plate, and on superhydrophobic aluminum foil, drip water droplet make it form ice hockey, then using this aluminium foil as gathering-device, and to be connected with low-voltage ground end, be that template carries out electrostatic spinning process at normal temperatures with ice hockey, obtain three-dimensional micro-nano tunica fibrosa.
The size of above-mentioned ice hockey is preferably 1.0 ~ 2.5mm.
Above-mentioned Electrospun solution can be the solution of prior art any one applicable electrostatic spinning process disclosed, the flow that electrostatic spinning process preferably controls Electrospun solution is 0.5 ~ 1.5mL/h, distance between Electrospun spinning head and gathering-device is 9 ~ 12cm, Electrospun voltage is 5 ~ 8kV, relative humidity lower than 15%, the temperature of cold plate is lower than-1 DEG C.
Beneficial effect of the present invention:
1, the present invention take ice hockey as template, opposing metallic template, ice hockey more easily controls and cost of manufacture is low, do not need after what is more important spinning completes manually to remove template one by one, only three-dimensional micro-nano tunica fibrosa at room temperature need be placed a period of time, ice hockey can be died away, thus simplifies the whole process of preparation three-dimensional micro-nano tunica fibrosa.
2, the present invention is that its bio-compatibility of template is good with ice hockey, there is not metal residual.
3, the present invention take ice hockey as the electric field that template is not disturbed electrospinning device and produced.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of three-dimensional micro-nano tunica fibrosa prepared by embodiment 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of the convex surface of three-dimensional micro-nano tunica fibrosa prepared by embodiment 1.
Fig. 3 is the scanning electron microscope (SEM) photograph of the concave surface of three-dimensional micro-nano tunica fibrosa prepared by embodiment 1.
Fig. 4 is the scanning electron microscope (SEM) photograph of three-dimensional micro-nano tunica fibrosa prepared by embodiment 2.
Fig. 5 is the scanning electron microscope (SEM) photograph of the convex surface of three-dimensional micro-nano tunica fibrosa prepared by embodiment 2.
Fig. 6 is the scanning electron microscope (SEM) photograph of the concave surface of three-dimensional micro-nano tunica fibrosa prepared by embodiment 2.
Fig. 7 is with the scanning electron microscope (SEM) photograph of the ice hockey of the different size three-dimensional micro-nano tunica fibrosa that is Template preparation in embodiment 3.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in more detail, but protection scope of the present invention is not limited only to these embodiments.
Superhydrophobic aluminum foil below in embodiment is prepared according to literature method, concrete grammar was: by the aluminium foil of 4cm × 4cm in deionized water, ethanol, chloroform and acetone ultrasonic 2 minutes successively, then by aluminium foil soaking at room temperature 4 minutes in the aqueous hydrochloric acid solution of 2.5mol/L, after clean by washed with de-ionized water, boil 20 minutes in deionized water, finally use N
2drying, obtains the aluminium foil cleaned up; Be the diallyl dimethyl ammoniumchloride (1.0mg/mL of 200000 ~ 350000 successively at molecular weight by the aluminium foil cleaned up, solvent is the 1.0mol/LNaCl aqueous solution), molecular weight be 70000 poly-tetraphenyl ethylene sodium sulfonate (1.0mg/mL, solvent is the 1.0mol/LNaCl aqueous solution), molecular weight be 200000 ~ 350000 diallyl dimethyl ammoniumchloride (1.0mg/mL, solvent is the 1.0mol/LNaCl aqueous solution) respectively in solution to soak 20 minutes, carry out layer assembly, wherein each soak after all clean by washed with de-ionized water and use N
2dry; Last to soak 3 minutes in 0.1mol/L perfluoro caprylic acid sodium water solution, and by washed with de-ionized water clean and N
2drying, obtains superhydrophobic aluminum foil.
Embodiment 1
By 1.5g molecular weight be 70000 ~ 90000 the polycaprolactone volume ratio that adds 10mL chloroform and methyl alcohol be in the mixed liquor of 7:1, be mixed with Electrospun solution, loaded in Electrospun syringe by Electrospun solution, Electrospun spinning head is connected with high voltage source; Superhydrophobic aluminum foil is placed on cold plate, and the water droplet dripping multiple 2 μ L on superhydrophobic aluminum foil makes it form ice hockey, then using this aluminium foil as gathering-device, and be connected with low-voltage ground end, be that template carries out electrostatic spinning process at normal temperatures with ice hockey, the flow controlling Electrospun solution is 1mL/h, distance between Electrospun spinning head and gathering-device is 10.5cm, Electrospun voltage is 6.97kV, relative humidity is 11%, the temperature of cold plate is-5 DEG C, obtains three-dimensional micro-nano tunica fibrosa.Adopt the tunica fibrosa (as Fig. 1 ~ 3) that scanning electron microscopic observation obtains, the as can be seen from Figure 1 uniform diameter of fiber.From Fig. 2 and 3, in electrostatic spinning process, fiber laydown can obtain three-dimensional micro-nano tunica fibrosa in ice hockey template, and Fig. 2 and 3 is respectively convex surface and the concave surface of three-dimensional micro-nano tunica fibrosa.
Embodiment 2
By 1g molecular weight be 70000 ~ 90000 polycaprolactone add in 10mL hexafluoroisopropanol, be mixed with Electrospun solution, loaded in Electrospun syringe by Electrospun solution, Electrospun spinning head is connected with high voltage source; Superhydrophobic aluminum foil is placed on cold plate, and the water droplet dripping multiple 2 μ L on superhydrophobic aluminum foil makes it form ice hockey, then using this aluminium foil as gathering-device, and be connected with low-voltage ground end, be that template carries out electrostatic spinning process at normal temperatures with ice hockey, the flow controlling Electrospun solution is 1mL/h, distance between Electrospun spinning head and gathering-device is 10.5cm, Electrospun voltage is 5.13KV, relative humidity is 14.1%, the temperature of cold plate lower than-4 DEG C, obtain three-dimensional micro-nano tunica fibrosa.Adopt the tunica fibrosa (as Fig. 4 ~ 6) that obtains of scanning electron microscopic observation, as seen from Figure 4, the fibre diameter in the tunica fibrosa of acquisition evenly and thinner, illustrates that this tunica fibrosa has higher surface energy.From Fig. 5 and 6, in electrostatic spinning process, be that template can obtain three-dimensional micro-nano tunica fibrosa with ice hockey.Fig. 5 and 6 is respectively convex surface and the concave surface of three-dimensional micro-nano tunica fibrosa.
Embodiment 3
By 1g molecular weight be 70000 ~ 90000 polycaprolactone add in 10mL hexafluoroisopropanol, be mixed with Electrospun solution, loaded in Electrospun syringe by Electrospun solution, Electrospun spinning head is connected with high voltage source; Superhydrophobic aluminum foil is placed on cold plate, and on superhydrophobic aluminum foil, drip multiple 1 μ L, 3 μ L, the water droplet of 3.5 μ L makes it form ice hockey, then using this aluminium foil as gathering-device, and be connected with low-voltage ground end, be that template carries out electrostatic spinning process at normal temperatures with ice hockey, the flow controlling Electrospun solution is 1mL/h, distance between Electrospun spinning head and gathering-device is 11cm, Electrospun voltage is 5.32kV, relative humidity is 9.6%, the temperature of cold plate is-5 DEG C, obtains three-dimensional micro-nano tunica fibrosa.As seen from Figure 7, there is by using the ice hockey of different size to obtain the three-dimensional micro-nano tunica fibrosa of different-diameter spheroid.
Claims (3)
1. be a method for Template preparation three-dimensional micro-nano tunica fibrosa based on ice hockey, it is characterized in that: loaded in Electrospun syringe by Electrospun solution, Electrospun spinning head is connected with high voltage source; Superhydrophobic aluminum foil is placed on cold plate, and on superhydrophobic aluminum foil, drip water droplet make it form ice hockey, then using this aluminium foil as gathering-device, and to be connected with low-voltage ground end, be that template carries out electrostatic spinning process at normal temperatures with ice hockey, obtain three-dimensional micro-nano tunica fibrosa.
2. according to claim 1 is the method for Template preparation three-dimensional micro-nano tunica fibrosa based on ice hockey, it is characterized in that: the size of described ice hockey is 1.0 ~ 2.5mm.
3. according to claim 1 and 2 is the method for Template preparation three-dimensional micro-nano tunica fibrosa based on ice hockey, it is characterized in that: the flow of described electrostatic spinning process control Electrospun solution is 0.5 ~ 1.5mL/h, distance between Electrospun spinning head and gathering-device is 9 ~ 12cm, Electrospun voltage is 5 ~ 8kV, relative humidity lower than 15%, the temperature of cold plate is lower than-1 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510852061.5A CN105274734B (en) | 2015-11-27 | 2015-11-27 | A kind of is the method that template is prepared three-D micro-nano rice tunica fibrosa based on ice hockey |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510852061.5A CN105274734B (en) | 2015-11-27 | 2015-11-27 | A kind of is the method that template is prepared three-D micro-nano rice tunica fibrosa based on ice hockey |
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| CN105274734A true CN105274734A (en) | 2016-01-27 |
| CN105274734B CN105274734B (en) | 2017-03-15 |
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| CN201510852061.5A Expired - Fee Related CN105274734B (en) | 2015-11-27 | 2015-11-27 | A kind of is the method that template is prepared three-D micro-nano rice tunica fibrosa based on ice hockey |
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Citations (6)
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| US6495258B1 (en) * | 2000-09-20 | 2002-12-17 | Auburn University | Structures with high number density of carbon nanotubes and 3-dimensional distribution |
| CN101423984A (en) * | 2008-12-04 | 2009-05-06 | 上海大学 | Ice surface collection method of polymer fiber electrostatic imitated silk and apparatus thereof |
| US20100093093A1 (en) * | 2006-12-05 | 2010-04-15 | Nanyang Technological University | Manufacturing three-dimensional scaffolds using electrospinning at low temperatures |
| CN102453965A (en) * | 2011-01-20 | 2012-05-16 | 中国科学技术大学 | Method and device for preparing nanofibers |
| WO2014063013A1 (en) * | 2012-10-18 | 2014-04-24 | The University Of Akron | Apparatus and method for electrospinning a nanofiber coating on surfaces of poorly conductive three-dimensional objects |
| KR101387886B1 (en) * | 2013-05-20 | 2014-04-24 | 한림대학교 산학협력단 | Method of fabricating a scaffold capable of controlling the thickness and pore size thereof, the scaffold fabricated thereby, and a fabricating equipment used therefor |
-
2015
- 2015-11-27 CN CN201510852061.5A patent/CN105274734B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6495258B1 (en) * | 2000-09-20 | 2002-12-17 | Auburn University | Structures with high number density of carbon nanotubes and 3-dimensional distribution |
| US20100093093A1 (en) * | 2006-12-05 | 2010-04-15 | Nanyang Technological University | Manufacturing three-dimensional scaffolds using electrospinning at low temperatures |
| CN101423984A (en) * | 2008-12-04 | 2009-05-06 | 上海大学 | Ice surface collection method of polymer fiber electrostatic imitated silk and apparatus thereof |
| CN102453965A (en) * | 2011-01-20 | 2012-05-16 | 中国科学技术大学 | Method and device for preparing nanofibers |
| WO2014063013A1 (en) * | 2012-10-18 | 2014-04-24 | The University Of Akron | Apparatus and method for electrospinning a nanofiber coating on surfaces of poorly conductive three-dimensional objects |
| KR101387886B1 (en) * | 2013-05-20 | 2014-04-24 | 한림대학교 산학협력단 | Method of fabricating a scaffold capable of controlling the thickness and pore size thereof, the scaffold fabricated thereby, and a fabricating equipment used therefor |
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