CN101768797A - One-dimensional magnetic fiber material, preparation method thereof and use thereof - Google Patents
One-dimensional magnetic fiber material, preparation method thereof and use thereof Download PDFInfo
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- CN101768797A CN101768797A CN200810209829A CN200810209829A CN101768797A CN 101768797 A CN101768797 A CN 101768797A CN 200810209829 A CN200810209829 A CN 200810209829A CN 200810209829 A CN200810209829 A CN 200810209829A CN 101768797 A CN101768797 A CN 101768797A
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Abstract
The invention discloses a one-dimensional magnetic fiber material, a preparation method thereof and use thereof. Nano materials have marvelous performance and a variety of functional fibers can be prepared by combining the nano materials with special functions and fibrelike polymers. The material of the invention is comprised of a shell layer and a nuclear layer, wherein the average diameter of the magnetic conductor nano fiber material ranges from 100 to 450 nanometers; the shell layer is mainly made from poly(phenylene ethynylene) which is a p-type semiconductor polymer and is 30 to 150 nanometers thick; the nuclear layer is comprised of magnetic ferroferric oxide nanoparticles and a polyvinyl alcohol dispersion medium, and the particle size is 5 to 30 nanometers; the length of the magnetic nano fibers ranges from 10 micrometers to 10 centimeters; the weight content of the magnetic ferroferric oxide nanoparticles is 2 to 56 percent; and the weight content of the polyvinyl alcohol dispersion medium is 0 to 17 percent. The one-dimensional magnetic fiber material is used in fields of photoelectricity, medicament delivery, sensors and magnetic markers.
Description
Technical field:
The present invention relates to a kind of one-dimensional magnetic tri-iron tetroxide/p-phenylene vinylene's nano-fiber material and its production and application.
Background technology:
As far back as nineteen thirties, A.Fomhals has just reported in its patent and has utilized the high-voltage electrostatic field spining technology to prepare polymer nanofiber, but up near eighties of last century middle nineteen nineties, because the rapid intensification to nanosecond science and technology research makes the spinning this polymer composite fibrous spining technology of nano-scale for preparing in high-voltage electrostatic field evoke people to its great interest of furtheing investigate.Nobel chemistry Prize winner Mike Dare Mead professor seminars in 2000 have proposed the notion of Intelligent Composite nanofiber, have caused various countries scholars' extensive concern, and corresponding research work is also carried out immediately.
Nano material has a lot of peculiar performances, such as: nano material have special uvioresistant, absorb visible light and infrared ray, anti-aging, favorable conductive and electrostatic screen effect, strong antibacterial functions, stronger deodorizing function and adsorption capacity.By compound, can prepare various functional fibres nano material and fibrous polymer with specific function.Inorganic filler is dispersed in the organic polymer matrix with nano-scale formed Organic.In nano composite material, the size of decentralized photo at least in the one dimension direction less than 100nm.Calendar year 2001, the article of delivering on the Nature has proposed composite nano fiber potential application militarily, is about to some nano particle that poison gas is played catalyticing decomposition action and is compound to and removes to make military uniform in the fiber, and it is played a significant role in war.People such as Sudha Madhugiri adopt the electrospinning process of double syringe to prepare the composite nano fiber of electroluminescent macromolecule MEH-PPV and molecular sieve SBA-15, when the exciting light with identical wavelength excited, blue shift had taken place with pure high molecular comparing in the emission wavelength of composite nano fiber.People such as Frank Ko successfully are compound to the carbon nanotube bundles that is arranged in a row in the fiber, and this composite fibre has shown good mechanical performance, also can strengthen other fiber.When just can obtain the one-dimensional nano line that Single Walled Carbon Nanotube/carbon constitutes 1000 ℃ of calcination.
Summary of the invention:
The purpose of this invention is to provide a kind of paramagnetic tri-iron tetroxide/p-phenylene vinylene's nano-fiber material and its production and application that has.
Above-mentioned purpose realizes by following technical scheme:
One-dimensional magnetic fiber material, its composition comprises: shell, stratum nucleare, the average diameter of magnetic semiconductor nano-fiber material is 100-450nm, described shell is main material by p type semi-conducting polymer p-phenylene vinylene, thickness is 30-150nm, described stratum nucleare is made up of magnetic ferroferric oxide nano-particles and polyvinyl alcohol decentralized medium, particle size is 5-30nm, described magnetic Nano fibre length is 10 μ m-10cm, described magnetic ferroferric oxide nano-particles weight percentage is 2-56%, and described polyvinyl alcohol decentralized medium weight content is at 0--17%.
Described one-dimensional magnetic fiber material, described p-phenylene vinylene is a p type semi-conducting polymer, and molecular weight is at 10000-100000, and the weight percent concentration of p-phenylene vinylene pioneer's aqueous solutions of polymers is 2-7%, described polyvinyl alcohol is n=1750 ± 50, and the concentration of the aqueous solution is 1-6%.
Described one-dimensional magnetic fiber material, the ferriferrous oxide nano-particle of described magnetic is with Fe
3+And Fe
2+Be 2 in molar ratio: 1-1: 1 to join the concentration for preparing be in the polyvinyl alcohol water solution of 1-6%, mechanical agitation, speed are 200-2000rpm, and the time is 1-6 hour, add the sodium hydrate aqueous solution that concentration is 2-8% again, the pH value of adjusting mixed liquor prepares for 11-13.
Described one-dimensional magnetic fiber material, described p-phenylene vinylene is a shell, and described polyvinyl alcohol/tri-iron tetroxide is a stratum nucleare, and the ratio of core-shell structure is controlled at 1 by micro syringe: 2-3: 1;
Described p-phenylene vinylene is a shell, and described tri-iron tetroxide is a stratum nucleare, and the ratio of core-shell structure is controlled at 2 by micro syringe: 1-10: 1;
Described tri-iron tetroxide is a shell, and described p-phenylene vinylene is a stratum nucleare, and the ratio of core-shell structure is controlled at 1 by micro syringe: 1-5: 1.
Described one-dimensional magnetic fiber material, described one-dimensional magnetic ferriferrous oxide nano fibrous material tri-iron tetroxide is formed, and diameter is at 100-300nm.
The preparation method of one-dimensional magnetic fiber material, employing be the high-voltage electrostatic spinning method, at ambient temperature, spinning voltage is 10-23kV, the distance between emission electrode and the collecting electrode is 8-40cm, the electrode platinum electrode.
One-dimensional magnetic fiber material is used for photoelectricity, drug delivery, sensor, magnetic mark aspect.
This technical scheme has following beneficial effect:
1. the present invention proposes with p type semi-conducting polymer p-phenylene vinylene, magnetic ferroferric oxide is the one-dimensional magnetic composite nano fiber that main component prepares shell-core structure, promptly utilizes dispersant to fill magnetic nano-particle in semi-conducting polymer.This structure has the outstanding characteristics in two aspects: (I) specific area that can adjust active layer easily by the form and the size of controlling fiber helps improving opto-electronic conversion or hole transport effect; (II) tri-iron tetroxide effect therein is to form inner conductor, and this helps transporting of carrier, particularly tri-iron tetroxide and the p-phenylene vinylene forms shell-shell-core composite structure, makes two kinds of materials form nano level contact, will be very favourable to transporting of hole.Novel one-dimensional magnetic nano material is expected to significantly improve the opto-electronic conversion performance of semi-conducting polymer material, thereby accelerates the practicalization of polymer semiconductor's opto-electronic conversion equal energy source transformation technology, also provides new material and method for the semiconductor film electrode.
2. the present invention utilizes the high-voltage electrostatic spinning technology to prepare a kind of magnetic ferroferric oxide/p-phenylene vinylene's nano-fiber material, and its average diameter is 100-450nm; Shell is main material by p type semi-conducting polymer p-phenylene vinylene, and thickness is 30-150nm, and stratum nucleare is made up of magnetic ferroferric oxide nano-particles and polyvinyl alcohol decentralized medium, and particle size is 5-30nm.Described magnetic Nano fibre length is 10 μ m-10cm, and described magnetic ferroferric oxide nano-particles weight percentage is 2-56%, and described polyvinyl alcohol decentralized medium weight content is below 17%.The doping of tri-iron tetroxide obviously increases the electrical conductivity of conducting polymer, has reduced the internal resistance of material, has prolonged the service life of semi-conducting polymer electrooptical device.
3. the present invention utilizes polyvinyl alcohol to stop the reunion of ferriferrous oxide nano-particle as dispersant, and the diameter that has improved nanofiber simultaneously distributes, and makes the composite fibre diameter that obtains distribute narrower.In addition, the polyvinyl alcohol dissolubility is good, helps washing and removes, thereby further improve the specific area of composite fibre, strengthens the assimilation effect to light, improves the utilization ratio of opto-electronic device to light.
4. the present invention promptly when the size of magnet is suitable with the feature physical length, will present the magnetic property of abnormality because the feature physical length relevant with magnetic is in nanometer scale just.The compound various features of taking into account magnetic material and conducting polymer composite of magnetic nano-particle and semi-conducting polymer, has significant performance at aspects such as light, electricity, magnetic, therefore, the prepared one-dimensional ferroferric oxide magnetic nano fibrous material of the present invention has potential application at aspects such as chemical industry, information material, photoelectronics.
5. the magnetic ferroferric oxide nano-particles among the present invention has good light, electricity, sound and magnetic property, tri-iron tetroxide/p-phenylene vinylene's the composite nano fiber that utilizes the high-voltage electrostatic spinning technology to prepare one dimension has promptly obtained stable magnetic nano-particle, and make the physical length of particle be in nanometer scale just, when the size of magnetic was suitable with the feature physical length, it will present unusual magnetic property.In addition, semi-conducting polymer contacts with the nanoscale of magnetic nano-particle, obviously improved the transmission performance of semi-conducting material, therefore, tri-iron tetroxide/p-phenylene vinylene's composite nano fiber has application at aspects such as chemical industry, information material, photoelectric material and bioengineering.
Description of drawings:
The specific embodiment of the present invention:
Embodiment 1:
The used spinning solution of prepared one dimension p-phenylene vinylene/polyvinyl alcohol/ferroferric oxide magnetic nano fibrous material (seeing accompanying drawing 1) is by p-phenylene vinylene pioneer's polymer 1, Fe in the present embodiment
3+And Fe
2+Solution 2, polyvinyl alcohol 3 and NaOH are prepared by following amount: p-phenylene vinylene pioneer's polymer solution (4%) 30mL, Fe
3+And Fe
2+The mol ratio of two kinds of particles in solution 2: 1.2 is with the pH=11-13 of sodium hydroxide solution adjustment solution.The weight percent concentration of polyvinyl alcohol water solution is 1-6%,
With p-phenylene vinylene is shell, and polyvinyl alcohol/tri-iron tetroxide is that stratum nucleare prepares the one-dimensional magnetic nano-fiber material, and its preparation process is as follows:
A. the preparation of spinning solution: get polyvinyl alcohol (4%) 100mL that has dissolved, place the 250mL four-hole bottle, logical nitrogen is warming up to 80 ℃, and mechanical agitation (more than the 600rpm) 15 minutes adds the Fe of 4mL 1M respectively
3+The Fe of solution and 2.4mL 1M
2+Behind the solution, constant temperature stirred 20 minutes.With micro-injection pump dropping sodium aqueous solution in system, adjust the pH value of solution value to 11-13, continue heating after 1-5 hour, cooling.
B. the preparation of one-dimensional magnetic nano-fiber material: get above-mentioned polyvinyl alcohol/tri-iron tetroxide solution 36mL and place the 50mL syringe.Get 30mL p-phenylene vinylene pioneer polymer solution and place an other 50mL syringe.Respectively two syringes are fixed on the micro-injection pump, syringe needle bushing type syringe needle, platinum electrode is connected to the syringe nozzle place, and the electrostatic generator of the living positive high voltage of practicing midwifery, utilize the flow injection pump to control the flow velocity of shell and stratum nucleare solution respectively, realization is to the control of shell and stratum nucleare content, and flow velocity is 20-120mL/H; Shower nozzle is 10-50cm to the distance of collecting electrode; Spinning voltage is 10-23kV; Environment temperature is 25 ℃; Relative air humidity is 30-60%; The electrostatic generator of the collecting electrode ground connection or the living negative high voltage of practicing midwifery, negative material are mainly aluminium foil, quartz plate, copper mesh, ito glass etc.Elder generation's open flow syringe pump when treating that the shower nozzle place has liquid to flow out, is opened HV generator, and regulation voltage carries out electrostatic spinning to appropriate value.The one-dimensional magnetic nano-fiber material that obtains slowly is warming up to 80 ℃, constant temperature 2-3H under the high pure nitrogen protection; continue to be warming up to 220 ℃; behind the constant temperature 0.5H, slowly cool to room temperature, promptly obtain p-phenylene vinylene of the present invention/Fe 3 O 4 magnetic core-shell structure composite nano-fiber material.
Embodiment 2:
The spinning solution of the preparation one-dimensional magnetic nano-fiber material (seeing accompanying drawing 2) of present embodiment is by p-phenylene vinylene pioneer's polymer, Fe
3+And Fe
2+Solution, polyvinyl alcohol are prepared by following composition: p-phenylene vinylene pioneer's polymer solution (4%) 30mL, Fe
3+And Fe
2+The mol ratio of two kinds of ions in solution 2: 1.2 is with the pH=11-13 of sodium hydroxide solution adjustment solution.The weight percent concentration of polyvinyl alcohol water solution is 2%.Polyvinyl alcohol/tri-iron tetroxide solution according to mode one preparation is removed polyvinyl alcohol through washing, and centrifugation, precipitation is transferred in the 30mL p-phenylene vinylene pioneer polymer solution, mechanical agitation, and ultrasonic dispersion is after 30 minutes, carry out high-voltage electrostatic spinning, its method of operating is identical with specific embodiment 1.
Embodiment 3:
The spinning solution of the preparation one-dimensional magnetic nano-fiber material of present embodiment is by p-phenylene vinylene pioneer's polymer, Fe
3+And Fe
2+Solution, polyvinyl alcohol are prepared by following composition: p-phenylene vinylene pioneer's polymer solution (4%) 30mL, Fe
3+And Fe
2+The mol ratio of two kinds of ions in solution 2: 1.5 is with the pH=11-13 of sodium hydroxide solution adjustment solution.The weight percent concentration of polyvinyl alcohol water solution is 4%.Its method of operating is identical with specific embodiment 1.
Embodiment 4:
The spinning solution of the preparation one-dimensional magnetic nano-fiber material of present embodiment is by p-phenylene vinylene pioneer's polymer, Fe
3+And Fe
2+Solution, polyvinyl alcohol are prepared by following composition: p-phenylene vinylene pioneer's polymer solution (4%) 30mL, Fe
3+And Fe
2+The mol ratio of two kinds of ions in solution 2: 1.1 is with the pH=11-13 of sodium hydroxide solution adjustment solution.The weight percent concentration of polyvinyl alcohol water solution is 2%.Its method of operating is identical with specific embodiment 1.
Embodiment 5:
The spinning solution of the preparation one-dimensional magnetic nano-fiber material of present embodiment is by p-phenylene vinylene pioneer's polymer, Fe
3+And Fe
2+Solution, polyvinyl alcohol are prepared by following composition: p-phenylene vinylene pioneer's polymer solution (2%) 30mL, Fe
3+And Fe
2+The mol ratio of two kinds of ions in solution 2: 1.2, weight percent concentration is 2% polyvinyl alcohol water solution 20mL, in room temperature, nitrogen protection was stirred 12 hours down with above-mentioned solution, adjusted the pH=11-13 of solution with sodium hydroxide solution.Its method of operating is identical with specific embodiment 1.
Embodiment 6:
The spinning solution of the preparation one-dimensional magnetic nano-fiber material of present embodiment is by Fe
3+And Fe
2+Solution, polyvinyl alcohol are prepared by following composition: Fe
3+And Fe
2+The mol ratio of two kinds of ions in solution 2: 1.3, weight percent concentration is 3.5% polyvinyl alcohol water solution 100mL, in room temperature, nitrogen protection was stirred 12 hours down with above-mentioned solution, adjusted the pH=11-13 of solution with sodium hydroxide solution.The method of operating of its spinning is identical with specific embodiment 1.Polyvinyl alcohol/tri-iron tetroxide the composite nano fiber that obtains placed carry out sintering in the high temperature furnace, temperature is controlled at below 500 ℃, removes polyvinyl alcohol, promptly obtains product of the present invention-ferroferric oxide magnetic nano fiber.
Embodiment 7:
One-dimensional magnetic tri-iron tetroxide/p-phenylene vinylene's nano-fiber material is used for photoelectricity, drug delivery, sensor, magnetic mark aspect.
Claims (10)
1. one-dimensional magnetic fiber material, its composition comprises: shell, stratum nucleare, it is characterized in that: the average diameter of magnetic semiconductor nano-fiber material is 100-450nm, described shell is main material by p type semi-conducting polymer p-phenylene vinylene, thickness is 30-150nm, described stratum nucleare is made up of magnetic ferroferric oxide nano-particles and polyvinyl alcohol decentralized medium, particle size is 5-30nm, described magnetic Nano fibre length is 10 μ m-10cm, described magnetic ferroferric oxide nano-particles weight percentage is 2-56%, and described polyvinyl alcohol decentralized medium weight content is at 0--17%.
2. according to right 1 described one-dimensional magnetic fiber material, it is characterized in that: described p-phenylene vinylene is p type semi-conducting polymer, molecular weight is at 10000-100000, the weight percent concentration of p-phenylene vinylene pioneer's aqueous solutions of polymers is 2-7%, described polyvinyl alcohol is n=1750 ± 50, and the concentration of the aqueous solution is 1-6%.
3. one-dimensional magnetic fiber material according to claim 1 and 2 is characterized in that: the ferriferrous oxide nano-particle of described magnetic is with Fe
3+And Fe
2+Be 2 in molar ratio: 1-1: 1 to join the concentration for preparing be in the polyvinyl alcohol water solution of 1-6%, mechanical agitation, speed are 200-2000rpm, and the time is 1-6 hour, add the sodium hydrate aqueous solution that concentration is 2-8% again, the pH value of adjusting mixed liquor prepares for 11-13.
4. one-dimensional magnetic fiber material according to claim 1 and 2 is characterized in that: described p-phenylene vinylene is a shell, and described polyvinyl alcohol/tri-iron tetroxide is a stratum nucleare, and the ratio of core-shell structure is controlled at 1 by micro syringe: 2-3: 1;
Described p-phenylene vinylene is a shell, and described tri-iron tetroxide is a stratum nucleare, and the ratio of core-shell structure is controlled at 2 by micro syringe: 1-10: 1;
Described tri-iron tetroxide is a shell, and described p-phenylene vinylene is a stratum nucleare, and the ratio of core-shell structure is controlled at 1 by micro syringe: 1-5: 1.
5. one-dimensional magnetic fiber material according to claim 3 is characterized in that: described p-phenylene vinylene is a shell, and described polyvinyl alcohol/tri-iron tetroxide is a stratum nucleare, and the ratio of core-shell structure is controlled at 1 by micro syringe: 2-3: 1;
Described p-phenylene vinylene is a shell, and described tri-iron tetroxide is a stratum nucleare, and the ratio of core-shell structure is controlled at 2 by micro syringe: 1-10: 1;
Described tri-iron tetroxide is a shell, and described p-phenylene vinylene is a stratum nucleare, and the ratio of core-shell structure is controlled at 1 by micro syringe: 1-5: 1.
6. according to claim 1 or 2 or 5 described one-dimensional magnetic fiber materials, it is characterized in that: described one-dimensional magnetic ferriferrous oxide nano fibrous material tri-iron tetroxide is formed, and diameter is at 100-300nm.
7. one-dimensional magnetic fiber material according to claim 3 is characterized in that: described one-dimensional magnetic ferriferrous oxide nano fibrous material tri-iron tetroxide is formed, and diameter is at 100-300nm.
8. one-dimensional magnetic fiber material according to claim 4 is characterized in that: described one-dimensional magnetic ferriferrous oxide nano fibrous material tri-iron tetroxide is formed, and diameter is at 100-300nm.
9. the preparation method of an one-dimensional magnetic fiber material is characterized in that: employing be the high-voltage electrostatic spinning method, at ambient temperature, spinning voltage is 10-23kV, the distance between emission electrode and the collecting electrode is 8-40cm, the electrode platinum electrode.
10. an one-dimensional magnetic fiber material is used for photoelectricity, drug delivery, sensor, magnetic mark aspect.
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| CN101649501B (en) * | 2009-09-09 | 2012-07-25 | 大连交通大学 | Magnetic composite nano fiber and preparation method thereof |
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| CN101649501B (en) * | 2009-09-09 | 2012-07-25 | 大连交通大学 | Magnetic composite nano fiber and preparation method thereof |
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| CN111663198B (en) * | 2020-06-19 | 2021-07-30 | 华中科技大学 | Micro-nano magnetic fiber and preparation method thereof |
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