WO2018034625A1 - Randomly distributed and/or vertically/horizontally grown carbon nanotubes on polymeric nanofibers and their composites - Google Patents
Randomly distributed and/or vertically/horizontally grown carbon nanotubes on polymeric nanofibers and their composites Download PDFInfo
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- WO2018034625A1 WO2018034625A1 PCT/TR2016/050289 TR2016050289W WO2018034625A1 WO 2018034625 A1 WO2018034625 A1 WO 2018034625A1 TR 2016050289 W TR2016050289 W TR 2016050289W WO 2018034625 A1 WO2018034625 A1 WO 2018034625A1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
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- 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
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/08—Processes in which the treating agent is applied in powder or granular form
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/74—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polycondensates of cyclic compounds, e.g. polyimides, polybenzimidazoles
Definitions
- the present invention relates to a production method of vertically/horizontally aligned and/or randomly oriented carbon nanotubes (CNTs) produced on polymeric nanofiber substrate.
- CNTs carbon nanotubes
- These polymer/CNT structures can be used to enhance energy storage in supercapacitors.and if they are embedded into thermoset/thermoplastic resins and also they can be incorporated as interleaves in composite materials. Direct implementation of these structures is a route to establish nano-enhanced composite structures for advanced applications such as primary load bearing components, energy storage, and multifunctional components such as structural composites within energy storage applications.
- Some of the related patents on vertically grown carbon nanotubes, methods and applications are US2001024633 (A1 ) , KR201 10037556 (A) , US2013285160 (A1 ) .
- RU201 1 1 18647 (A) proposed several manufacturing methods including the method of manufacturing a film consisting of a polymer matrix reinforced with a vertically oriented array of carbon nanotubes grown on a substrate includes heat treatment at a temperatu re no higher than the temperature of destruction of the polymer matrix.
- the present invention belongs to the field of preparation of composite prepregs and interleaves materials.
- This invention further proposes a method for the preparation of such carbon nanotubes random ly and/or vertically and/or horizontally grown on polymeric nanofibers and their thermoset/thermoplastic prepregs.
- the invention eliminates the removal of CNTs arrays from substrate, further handling problems and the damage of CNTs arrays related to it.
- These random and/or vertically, horizontally oriented array of carbon nanotubes grown on a polymer substrate enable direct transfer of there nanostructures to composites, ease composite manufacturing and can also be used as interleaves materials.
- Carbon nanotubes fabricated onto polymeric nanofibers can form an ordered layer of nanomaterials which can enhance the properties of advanced composites.
- carbon nanotube dispersed thermoset resins for prepreg manufacturing and/or composite manufacturing, however; critical volume fraction and dispersion/distribution issues can limit the enhancing mechanisms expected from these nanomaterials.
- the controlled morphology of carbon nanotubes synthesized directly onto polymer nanofibers can remove these concerns encountered in the prior studies including handling and their composite manufacturing includes thermoset/thermoplastic prepregs.
- Figure 1 The technical illustration of present invention .
- Figure 1 describes the production steps of present invention.
- Figure 2 a) camera image of catalyst doped polymeric nanofibers b) camera image of produced polymer/carbon nanotubes in controlled morphology c) SEM image of catalyst doped polymeric nanofibers d) SEM image of randomly oriented carbon nanotubes grown on nanofiber substrate
- Figure 2 represents a) camera image of catalyst doped polymeric nanofibers b) camera image of produced polymer/carbon nanotubes in controlled morphology c) SEM image of catalyst doped polymeric nanofibers d) SEM image of randomly oriented carbon nanotubes grown on nanofiber substrate Definitions of the Com ponents/ Sect ions/ Parts that form t he I nvent ion
- the present invention discloses a production method of carbon nanotubes grown on high temperature resistant polymeric nanofibers and use of their thermoset/thermoplastic prepregs/interleaves in composite materials.
- the production method of carbon nanotubes and the prepregs of them comprises the steps below:
- Manufacturing of heat resistant high performance nanofibers with the methods includes electrospinning, deposition , film forming, gel spinning from polymers with high melting and degradation temperatures (above 500 ° C) includes polybenzim idazole and its derivatives.
- Random and/or vertically and/or horizontally aligned carbon nanotubes growth on polymeric nanofibers by chemical vapor deposition (CVD) following the procedure as coating nanofibers/fibers with catalyst includes as iron nitrate/ cobalt/nickel by dipping into the catalyst solution and/or related wet processes under ambient room conditions, which can range from 23°C to 28°C and 20% to 70% humidity, drying in an oven that heated up to an optim ized temperature according to polymeric nanofiber chemical structure, placing into a tube furnace where CVD and/or other methods to grown carbon nanotubes, heating up to growth temperature (range from 550°C to 800°C) in a pure hydrogen environment, stabilizing the temperature while using ethanol/ethylene/acetylene/methane/methylacetylene/ carbon monoxide/benzene gas during carbon nanotubes growth .
- CVD chemical vapor deposition
- Achieving 'fuzzy fiber' architecture onto nanofibers within CNT fibers including their orientation which is obtained by growing CNTs in situ , directly on surface of coated polymeric nanofiber includes random and/or vertically, horizontally aligned CNTs that form a forest like structure on the surface of each nanofiber/fiber.
- Controlled morphology of CNTs will support to achieve controlled volume fraction of nano-reinforcementto be used for thermoset/thermoplastic prepregs and composites as interleaves and/or embedded into resin .
- thermoset/thermoplastic prepregs incorporating random and/or vertically and/or horizontally aligned carbon nanotubes grown on polymeric nanofibers with the methods including polymer deposition by electrostatic forces, ultrasonic deposition, coating of the resin , melting the resin .
Abstract
The present invention relates to a production method of vertically/horizontally aligned and/or randomly oriented carbon nanotubes (CNTs) produced on polymeric nanofiber substrate. These polymer/CNT structures can be used to enhance energy storage in supercapacitors, if they are embedded into thermoset/thermoplastic resins and also they can be incorporated as interleaves in composite materials. Direct implementation of these structures is a route to establish nano-enhanced composite structures for advanced applications such as primary load bearing components, energy storage, and multifunctional components such as structural composites within energy storage applications.
Description
RANDOMLY DI STRI BUTED AND/ OR VERTI CALLY/ HORI ZONTALLY GROWN CARBON NANOTUBES ON POLYMERI C NANOFI BERS AND TH El R COMPOSI TES
Technical Field of the I nvention
The present invention relates to a production method of vertically/horizontally aligned and/or randomly oriented carbon nanotubes (CNTs) produced on polymeric nanofiber substrate. These polymer/CNT structures can be used to enhance energy storage in supercapacitors.and if they are embedded into thermoset/thermoplastic resins and also they can be incorporated as interleaves in composite materials. Direct implementation of these structures is a route to establish nano-enhanced composite structures for advanced applications such as primary load bearing components, energy storage, and multifunctional components such as structural composites within energy storage applications.
Prior Art of the I nvention
Some of the related patents on vertically grown carbon nanotubes, methods and applications are US2001024633 (A1 ) , KR201 10037556 (A) , US2013285160 (A1 ) . Especially RU201 1 1 18647 (A) proposed several manufacturing methods including the method of manufacturing a film consisting of a polymer matrix reinforced with a vertically oriented array of carbon nanotubes grown on a substrate includes heat treatment at a temperatu re no higher than the temperature of destruction of the polymer matrix. However, the present invention belongs to the field of preparation of composite prepregs and interleaves materials.
This invention further proposes a method for the preparation of such carbon nanotubes random ly and/or vertically and/or horizontally grown on polymeric nanofibers and their thermoset/thermoplastic prepregs. The invention eliminates the removal of CNTs arrays from substrate, further handling problems and the damage of CNTs arrays related to it. These random and/or vertically, horizontally oriented array of carbon nanotubes grown on a polymer substrate enable direct transfer of there nanostructures to composites, ease composite manufacturing and can also be used as interleaves materials.
Brief Description and Obj ectives of t he I nvention
Carbon nanotubes fabricated onto polymeric nanofibers can form an ordered layer of nanomaterials which can enhance the properties of advanced composites. There are numerous examples of carbon nanotube dispersed thermoset resins for prepreg manufacturing and/or composite manufacturing, however; critical volume fraction and dispersion/distribution issues can limit the enhancing mechanisms expected from these nanomaterials. I n this invention , the controlled morphology of carbon nanotubes synthesized directly onto polymer nanofibers can remove these concerns encountered in the prior studies including handling and their composite manufacturing includes thermoset/thermoplastic prepregs. These advantages would avoid an additional step of carbon nanotube integration to composites by direct manufacturing of carbon nanotubes onto high temperature polymeric fibers. The already grown carbon nanotubes would remain onto the polymeric fibers during composite or energy storage applications.
Definit ion of t he Figures Describing t he I nvention
Figure 1 . The technical illustration of present invention . Figure 1 describes the production steps of present invention. ( I ) production of high performance nanofibers ( I I ) catalyst deposition on nanofibers ( I I I ) random and/or vertically oriented array of carbon nanotubes growth on a polymer substrate ( I V) embedding these structures into thermoplastic/thermoset resins and/or (V) use of in structural composites as interlaminar reinforcement.
Figure 2. a) camera image of catalyst doped polymeric nanofibers b) camera image of produced polymer/carbon nanotubes in controlled morphology c) SEM image of catalyst doped polymeric nanofibers d) SEM image of randomly oriented carbon nanotubes grown on nanofiber substrateFigure 2 represents a) camera image of catalyst doped polymeric nanofibers b) camera image of produced polymer/carbon nanotubes in controlled morphology c) SEM image of catalyst doped polymeric nanofibers d) SEM image of randomly oriented carbon nanotubes grown on nanofiber substrate
Definitions of the Com ponents/ Sect ions/ Parts that form t he I nvent ion
1 . High temperature resistant nanofibers
2. Catalyst deposition
3. Carbon nanotubes grown on nanofiber substrate 4. Nanofibrous substrate
5. Polymer/carbon nanotubes in controlled morphology
6. Polymer/carbon nanotubes in controlled morphologies reinforced prepregs
7. Composite lamina/ply
Detailed Description of the I nvention
The present invention discloses a production method of carbon nanotubes grown on high temperature resistant polymeric nanofibers and use of their thermoset/thermoplastic prepregs/interleaves in composite materials. The production method of carbon nanotubes and the prepregs of them comprises the steps below:
1 . Manufacturing of heat resistant high performance nanofibers with the methods includes electrospinning, deposition , film forming, gel spinning from polymers with high melting and degradation temperatures (above 500° C) includes polybenzim idazole and its derivatives.
2. Random and/or vertically and/or horizontally aligned carbon nanotubes growth on polymeric nanofibers by chemical vapor deposition (CVD) following the procedure as coating nanofibers/fibers with catalyst includes as iron nitrate/ cobalt/nickel by dipping into the catalyst solution and/or related wet processes under ambient room conditions, which can range from 23°C to 28°C and 20% to 70% humidity, drying in an oven that heated up to an optim ized temperature according to polymeric nanofiber chemical structure, placing into a tube furnace where CVD and/or other methods to grown carbon nanotubes, heating up to growth temperature (range from 550°C to 800°C) in a pure hydrogen environment, stabilizing the temperature while using ethanol/ethylene/acetylene/methane/methylacetylene/ carbon monoxide/benzene gas during carbon nanotubes growth .
Achieving 'fuzzy fiber' architecture onto nanofibers within CNT fibers including their orientation which is obtained by growing CNTs in situ , directly on surface of coated polymeric nanofiber includes random and/or vertically, horizontally aligned CNTs that form a forest like structure on the surface of each nanofiber/fiber.
Controlled morphology of CNTs will support to achieve controlled volume fraction of nano-reinforcementto be used for thermoset/thermoplastic prepregs and composites as interleaves and/or embedded into resin .
Preparation of thermoset/thermoplastic prepregs incorporating random and/or vertically and/or horizontally aligned carbon nanotubes grown on polymeric nanofibers with the methods including polymer deposition by electrostatic forces, ultrasonic deposition, coating of the resin , melting the resin .
Claims
CLAI MS
A production method of vertically/horizontally aligned and/or randomly oriented carbon nanotubes (CNTs) on polymeric nanofibers characterized by comprising the steps below,
(a) Manufacturing of heat resistant high performance nanofibers with the methods includes electrospinning, deposition, film forming, gel spinning from polymers with high melting and degradation temperatures above 500° C includes polybenzimidazole and its derivatives,
(b) Random and/or vertically and/or horizontally aligned carbon nanotubes growth on polymeric nanofibers by chemical vapor deposition (CVD) following the procedure,
- coating nanofibers/fibers with catalyst includes as iron nitrate and/or cobalt and/or nickel by dipping into the catalyst solution and/or related wet processes under ambient room conditions, which can range from 23°C to 28°C and 20% to 70% humidity,
- drying in an oven that heated up to an optimized temperature according to polymeric nanofiber chemical structure,
- placing into a tube furnace where CVD and/or other methods to grow carbon nanotubes,
- heating up to growth temperature that has a range from 550°C to 800°C in a pure hydrogen environment ,
- stabilizing the temperature while using ethanol, ethylene, acetylene, methane, methylacetylene, carbon monoxide, benzene gas during carbon nanotubes growth.
(c) Achieving 'fuzzy fiber' architecture onto nanofibers within CNT fibers including their orientation which is obtained by growing CNTs in situ, directly on surface of coated polymeric nanofiber includes random and/or vertically, horizontally aligned CNTs that form a forest like structure on the surface of each nanofiber/fiber.
Vertically/horizontally aligned and/or randomly oriented carbon nanotubes (CNTs) produced on polymeric nanofiber with the method according to claim 1 .
3. Use of carbon nanotubes for thermoset and/or thermoplastic prepregs and composites as interleaves and/or embedded into resin.
4. A preparation method of thermoset and/or thermoplastic prepregs incorporating carbon nanotubes according to claim 2 characterized by using the methods including polymer deposition by electrostatic forces or ultrasonic deposition or coating of the resin or melting the resin.
5. Thermoset and/or thermoplastic prepregs prepared by using the method according to claim 4.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/TR2016/050289 WO2018034625A1 (en) | 2016-08-16 | 2016-08-16 | Randomly distributed and/or vertically/horizontally grown carbon nanotubes on polymeric nanofibers and their composites |
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| PCT/TR2016/050289 WO2018034625A1 (en) | 2016-08-16 | 2016-08-16 | Randomly distributed and/or vertically/horizontally grown carbon nanotubes on polymeric nanofibers and their composites |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109094051A (en) * | 2018-08-20 | 2018-12-28 | 吉林省贞靓科技有限公司 | A kind of ultralight, ultra-thin, flexible, ventilative superfine fibre composite membrane and preparation method thereof with multiple spectra electromagnetic wave proof performance |
| CN109592666A (en) * | 2018-11-24 | 2019-04-09 | 天津大学 | A kind of preparation method of celestial being's palmate carbon nano pipe array |
| CN110079878A (en) * | 2019-06-18 | 2019-08-02 | 广东工业大学 | A kind of electrostatic spinning nozzle and electrostatic spinning apparatus |
| CN111261859A (en) * | 2020-01-21 | 2020-06-09 | 山东大学 | Metal phosphide/carbon composite material and preparation method and application thereof |
| CN111318180A (en) * | 2020-03-16 | 2020-06-23 | 中国人民解放***箭军工程设计研究院 | Preparation method of film material containing oriented carbon nanotubes |
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| CN109094051A (en) * | 2018-08-20 | 2018-12-28 | 吉林省贞靓科技有限公司 | A kind of ultralight, ultra-thin, flexible, ventilative superfine fibre composite membrane and preparation method thereof with multiple spectra electromagnetic wave proof performance |
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| CN111318180A (en) * | 2020-03-16 | 2020-06-23 | 中国人民解放***箭军工程设计研究院 | Preparation method of film material containing oriented carbon nanotubes |
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