US20110049769A1 - Method for production of inorganic nanofibres through electrostatic spinning - Google Patents

Method for production of inorganic nanofibres through electrostatic spinning Download PDF

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Publication number
US20110049769A1
US20110049769A1 US12/991,000 US99100009A US2011049769A1 US 20110049769 A1 US20110049769 A1 US 20110049769A1 US 99100009 A US99100009 A US 99100009A US 2011049769 A1 US2011049769 A1 US 2011049769A1
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solution
spinning
alkoxide
vinylpyrrolidone
nanofibres
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Jiri Duchoslav
Lukas Rubacek
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/02—Heat treatment
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material

Definitions

  • the invention relates to a method for production of inorganic nanofibres through electrostatic spinning of solution, which contains alkoxide of metal or of semi-metal or of non-metal dissolved in a solvent system on basis of alcohol.
  • Inorganic materials feature a number of properties, thanks to which they are suitable for usage in many technical fields, e.g. in electrotechnics, medicine, industry, etc.
  • TiO 2 , SiO 2 , Al 2 O 3 , ZrO 2 and B 2 O 3 belong to the important inorganic substances.
  • Nanoparticles from inorganic material which may be produced through the above mentioned or other suitable method, could also be incorporated into a structure of nanofibres, which may be realised e.g. by adding the nanoparticles into polymer solution and consequent production of nanofibres from this solution. Presence of inorganic nanoparticles in polymer nanofibres renders specific properties to these nanofibres. Nevertheless the substantial portion of these nanoparticles is formed of polymer component.
  • the pure inorganic nanofibres are produced by discontinual methods of electrostatic spinning at usage of nozzle or needle spinning electrode, into which the solution is supplied, which may be represented by a precursor of given inorganic elements, or the polymer solution containing alkoxide of respective metal or non-metal as a source of inorganic basis of fibres.
  • the goal of the invention is to develop a continual production method of inorganic nanofibres through electrostatic spinning, which would remove disadvantages of the background art.
  • the goal of the invention has been achieved through a method for production of inorganic nanofibres according to the invention, whose principle consists in that, the alkoxide solution of metal or of semi-metal or non-metal is in a solvent system on basis of alcohol stabilised by chelating agent, which prevents hydrolysis of alkoxide, and after homogenizing is mixed with solution of poly(vinylpyrrolidone) in alcohol, after then the resultant solution is brought into electrostatic field, in which continually on long-term basis the electrostatic spinning is running, the result of which is production of organic-inorganic nanofibres, which are outside the spinning device calcinated after then in the air atmosphere at the temperature from 500° C. to 1300° C.
  • a concentrated acid which is according to the claim 3 preferably selected from the group of hydrochloric acid, nitric acid, phosphoric acid.
  • the chelating agent is composed of ⁇ -diketone, while the most suitable ⁇ -diketone seems to be acetylacetone, at whose usage the stabilisation of solution is permanent.
  • Alcohol in solution of poly(vinylpyrrolidone) is selected from the group of ethanol, 1-propanol, 2-propanol or their mixtures.
  • the poly(vinylpyrrolidone) has an average molecular weight within 1000000-1500000 g/mol and its weight concentration in solution is within the range from 4 to 9%, while the most preferred seems to be the poly(vinylpyrrolidone) having average molecular weight of 1300000 g/mol.
  • Alkoxide of metal is preferably selected from the group of titanium tetrabutoxide, titanium tetraisopropoxide, aluminium tri-sec-butoxide, aluminiumtriisopropoxide or zirconium tetraisopropoxide.
  • Alkoxide of semi-metal is preferably tetraethoxysilane or borium triethoxide.
  • the ratio of alkoxide and chelating agent in solution is within 1:0.8 to 1:2.2.
  • the alkoxide solution in electrostatic field is to be found on surface of active zone of the spinning mean of a spinning electrode.
  • the alkoxide solution is into electrostatic field for spinning transported by surface of the spinning electrode, which is preferably formed of rotating spinning electrode of an oblong shape, which extends by a section of its circumference into the solution being subjected to spinning.
  • the drawing represents in the FIG. 1 produced TiO 2 nanofibres, and in the FIG. 2 their XRD spectrum, the FIG. 3 represents Al 2 O 3 nanofibres and the FIG. 4 their XRD spectrum, the FIG. 5 represents B 2 O 3 nanofibres and the FIG. 6 their XRD spectrum, the FIG. 7 represents ZrO 2 nanofibres and the FIG. 8 their XRD spectrum.
  • Spinning solution for production of inorganic nanofibres contains as a source of inorganic basis an alkoxide of respective metal, semi-metal or non-metal, which is dissolved in a suitable solvent, e.g. in ethanol, 1 -propanol or 2-propanol.
  • a suitable solvent e.g. in ethanol, 1 -propanol or 2-propanol.
  • chelating agent is necessary to stabilise the solution of alkoxide, especially to prevent its hydrolysis.
  • the most suitable chelating agent is 6-diketone, e.g. acetylaceton.
  • Molecular ratio between alkoxide and chelating agent should be within the range from 1:0.8 to 1:2.2.
  • poly(vinylpyrrolidone) having molecular weight of 1300000 g/mol or viscosity number K-90, while its weight concentration towards a total weight of solution is from 4 to 9% by weight.
  • the process of electrostatic spinning depends on concentration, or more precisely on viscosity, surface tension and other parameters of alkoxide solution.
  • the exact composition of alkoxide solution depends on temperature and humidity of environment and parameters of electrostatic spinning, such as rotation and type of electrode, distance between electrodes and applied voltage.
  • the resultant solution of tetraethoxysilane was used for production of SiO 2 nanofibres by means of electrostatic spinning.
  • a device for electrostatic spinning of polymer solutions comprising a spinning electrode and against it arranged collecting electrode, while the spinning electrode comprised rotatably mounted spinning mean extending by a section of its circumference into a solution of tetraethoxysilane being present in a reservoir.
  • the rotating spinning mean thanks to its rotation, carried out the solution of tetraethoxysilane into a electrostatic field induced between the spinning electrode and the collecting electrode, while a portion of surface of rotating spinning mean being positioned against the collecting electrode represents an active spinning zone of the spinning mean.
  • the nanofibrous organic-inorganic layer was consequently calcinated in a furnace in air atmosphere at temperature from 600 to 800° C. at production of pure amorphous SiO 2 nanofibres.
  • TiO 2 nanofibres for preparation of solution the mixture of 250 g of ethanol and 29.4 g of acetylacetone was used, in which 100 g of titanium tetrabutoxide was dissolved. After homogenisation the obtained solution was carefully mixed with solution of 35.2 g of poly(vinylpyrrolidone) having molecular weight of 1300000 g/mol in 758.8 g of ethanol and after then acidified with concentrated hydrochloric acid. The resultant solution was subject to spinning through electrostatic spinning. The nanofibrous organic-inorganic layer was calcinated in furnace in air atmosphere at the temperature of 500° C. The crystallic form (structure) of resultant TiO 2 of inorganic nanofibres was purely of anatase.
  • the mixture of 150 g ethanol and 29.4 g of acetylacetone was used, in which 100 g of titanium tetrabutoxide was dissolved.
  • the obtained solution was mixed with solution of 35.2 g of poly(vinylpyrrolidone) having molecular weight of 1300000 g/mol in 272.1 g of ethanol, and after then acidified with concentrated hydrochloric acid.
  • the resultant solution was subject to spinning through electrostatic spinning.
  • the nanofibrous layer was calcinated at the temperature of 500° C. Crystallic form of resultant TiO 2 nanofibres was purely of anatase.
  • B 2 O 3 nanofibres For production of B 2 O 3 nanofibres the mixture of 500 g of ethanol and 68.6 g of acetylacetone was used, in which 100 g of borium triethoxide was dissolved. After homogenisation the obtained solution was mixed with solution of 71.5 g of poly(vinylpyrrolidone) having molecular weight of 1300000 g/mol in 1644.3 g of ethanol and after then acidified with concentrated hydrochloric acid. The resultant solution was subject to spinning through electrostatic spinning.
  • the nanofibrous layer was calcinated at the temperature of 500° C.
  • the resultant inorganic fibres showed B 2 O 3 crystallic structure with amorphous addition, which is witnessed by the picture represented in the FIG. 5 and XRD spectrum represented in the FIG. 6 .
  • Production of nanofibres from the above mentioned solutions of alkoxides is not limited only to the described electrostatic spinning device with rotating spinning electrode, but it is possible to use also other types of spinning electrodes, at which the solution of alkoxide in electrostatic field for spinning is to be found on surface of active spinning zone of a spinning mean of a spinning electrode.
  • Spinning of alkoxide solution runs successfully also on wire spinning electrodes according to the CZ PV 2007-485, at which the active spinning zone of the wire has during the spinning process a stable position towards the collecting electrode and alkoxide solution is to the active spinning zone of the wire supplied either by applying or by movement of the wire in direction of its length.
  • the solution of alkoxide in electrostatic field for spinning is to be found on surface of active zone of the wire of spinning mean.
  • the described solutions of alkoxides can of course be used also for discontinuous production of nanofibres at usage of nozzle or needle as a spinning electrode.
  • the mentioned method for production of nanofibres ensures a sufficient stability of the solution being subject to spinning for entire period of spinning, and it is a key aspect for continuous production of inorganic nanofibres.
  • Application of layers of inorganic nanofibres is important in many technical fields and industry, e.g. for production of composite materials, catalysts and electrochemical active elements.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Inorganic Fibers (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Nonwoven Fabrics (AREA)
US12/991,000 2008-05-06 2009-05-05 Method for production of inorganic nanofibres through electrostatic spinning Abandoned US20110049769A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
CZ20080277A CZ2008277A3 (cs) 2008-05-06 2008-05-06 Zpusob výroby anorganických nanovláken elektrostatickým zvláknováním
CZPV2008-277 2008-05-06
PCT/CZ2009/000065 WO2009135448A2 (en) 2008-05-06 2009-05-05 A method for production of inorganic nanofibres through electrostatic spinning

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US (1) US20110049769A1 (zh)
EP (1) EP2276880A2 (zh)
JP (1) JP2011520045A (zh)
KR (1) KR20100135975A (zh)
CN (1) CN102084044A (zh)
AU (1) AU2009243816A1 (zh)
BR (1) BRPI0912221A2 (zh)
CA (1) CA2723471A1 (zh)
CZ (1) CZ2008277A3 (zh)
IL (1) IL209135A0 (zh)
RU (1) RU2010147892A (zh)
WO (1) WO2009135448A2 (zh)

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US20110089595A1 (en) * 2003-06-19 2011-04-21 Eastman Chemical Company Water-dispersible and multicomponent fibers from sulfopolyesters
US8216953B2 (en) 2003-06-19 2012-07-10 Eastman Chemical Company Water-dispersible and multicomponent fibers from sulfopolyesters
US8840757B2 (en) 2012-01-31 2014-09-23 Eastman Chemical Company Processes to produce short cut microfibers
US9273417B2 (en) 2010-10-21 2016-03-01 Eastman Chemical Company Wet-Laid process to produce a bound nonwoven article
US9303357B2 (en) 2013-04-19 2016-04-05 Eastman Chemical Company Paper and nonwoven articles comprising synthetic microfiber binders
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US9598802B2 (en) 2013-12-17 2017-03-21 Eastman Chemical Company Ultrafiltration process for producing a sulfopolyester concentrate
US9605126B2 (en) 2013-12-17 2017-03-28 Eastman Chemical Company Ultrafiltration process for the recovery of concentrated sulfopolyester dispersion
WO2017186201A1 (en) 2016-04-26 2017-11-02 Pardam, S.R.O. Precursor fibers intended for preparation of silica fibers, method of manufacture thereof, method of modification thereof, use of silica fibers
CN110004519A (zh) * 2019-04-16 2019-07-12 天津工业大学 一种可生产"毛毛虫"状多尺度氧化铝纤维的静电纺丝液
EP3604640A4 (en) * 2017-03-30 2021-01-13 JNC Corporation METAL TITANATE FIBER PRODUCTION METHOD
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US11141506B2 (en) * 2018-04-03 2021-10-12 Peking University School And Hospital Of Stomatology Electrified composite membrane with extracellular matrix electrical topology characteristics, and preparation method thereof
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EP2276880A2 (en) 2011-01-26
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KR20100135975A (ko) 2010-12-27
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