WO2008022129A2 - Système et procédés pour centrifuger des nanotubes de carbone en fil, et fil obtenu par ce système et ces procédés - Google Patents

Système et procédés pour centrifuger des nanotubes de carbone en fil, et fil obtenu par ce système et ces procédés Download PDF

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Publication number
WO2008022129A2
WO2008022129A2 PCT/US2007/075903 US2007075903W WO2008022129A2 WO 2008022129 A2 WO2008022129 A2 WO 2008022129A2 US 2007075903 W US2007075903 W US 2007075903W WO 2008022129 A2 WO2008022129 A2 WO 2008022129A2
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WIPO (PCT)
Prior art keywords
cnts
yarn
cnt
zone
vacuum device
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Application number
PCT/US2007/075903
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English (en)
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WO2008022129A3 (fr
Inventor
P. Douglas Kirven
Timothy G. Clapp
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Cnt Technologies, Inc.
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Publication of WO2008022129A2 publication Critical patent/WO2008022129A2/fr
Publication of WO2008022129A3 publication Critical patent/WO2008022129A3/fr

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Classifications

    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
    • D02G3/16—Yarns or threads made from mineral substances
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01G—PRELIMINARY TREATMENT OF FIBRES, e.g. FOR SPINNING
    • D01G1/00—Severing continuous filaments or long fibres, e.g. stapling
    • D01G1/06—Converting tows to slivers or yarns, e.g. in direct spinning
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/22—Yarns or threads characterised by constructional features, e.g. blending, filament/fibre
    • D02G3/26—Yarns or threads characterised by constructional features, e.g. blending, filament/fibre with characteristics dependent on the amount or direction of twist
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2101/00—Inorganic fibres
    • D10B2101/10—Inorganic fibres based on non-oxides other than metals
    • D10B2101/12—Carbon; Pitch
    • D10B2101/122—Nanocarbons

Definitions

  • the present invention pertains generally to nanotechnology and textile arts. More specifically, the present invention pertains to systems and methods for drawing and drafting Carbon nanotubes (CNTs) and spinning the CNTs into yarn for use in commercial applications.
  • CNTs Carbon nanotubes
  • the present invention in a preferred embodiment, is particularly but not exclusively, a vacuum processing system coupled to an electromagnetic spinning apparatus for making yarn from CNTs, or other fiber strands.
  • Carbon nanotubes are often described as having perfect atomic structures wherein a graphene sheet is rolled up into the shape of a cylinder and capped with an end containing hexagonal and pentagonal rings.
  • Fig. IA illustrates side and end views of such a structure having walls one atom thick and a diameter on the order of l-2rmi.
  • arrays of CNTs or "CNT fibers" are grown on substrates.
  • CNT lengths on the order of about 1 to 4.5mm have been produced according to methods developed by Los Alamos National Laboratory as disclosed in published U.S.
  • the resulting nanostructure has a length to diameter ratio exceeding 10,000.
  • CNTs are at least one order of magnitude stronger than any other known material and have a theoretical strength of about 300 GPa. hi practice, measured strengths have been up to about 150 GPa, and the strength may improve upon annealing. For comparison, Kevlar® and other aramid fibers currently used in bullet-proof vest have a strength of only about 3 GPa, and carbon fibers used for making space shuttles and other aerospace structures have strengths of only about 2-5 GPa. In addition to remarkable strength, CNTs also possess high elasticity and are excellent electrical and thermal conductors.
  • CNT fibers (110) are processed for commercial use by spinning or twisting into yarn for additional processing into fabric, non-woven, and or composites.
  • Fig. IB illustrates typical yarn (130) twisted from fiber strands, such as cotton fiber (120).
  • the resulting yarn (130) has turns either in the counterclockwise or clockwise direction, known as "S" twist or "Z” twist, respectively, as shown in Fig. 1 C.
  • the degree of twist in yarn may be expressed in turns per meter (tpm). More twist is required for increased strength up to an optimum twist wherein the fibers in the yarn become more perpendicular than parallel to the length of yarn.
  • base yarns made from CNTs high twist rates are required on the order of 10,000 to 100,000 (tpm) wherein the diameter of the resulting base yarn is small and around lOOnm.
  • the base yarns are then cabled to make thicker yarns, or blended with other materials for commercial applications such as aerospace structures and personal body armor.
  • Figures 2A through 2C generally illustrate the steps by which CNTs (110) are made into yarn (230) for structural materials.
  • Reference character (220) generally represents a spin zone (220) to twist the fiber into yarn (230).
  • Fig. 2C further shows base yarns (230) cabled together to form thicker yarns (240) using a secondary spin zone (220a).
  • the present invention specifically addresses and alleviates the above mentioned deficiencies associated with the prior art. More particularly, the present invention is a yarn comprising: a multiplicity of carbon nanotubes (CNTs) helically twisted about a longitudinal axis to form a CNT twist rate, wherein the CNT twist rate is between about 10,000 turns per meter and 100,000 turns per meter.
  • the yarn of the invention further comprises: an outer twist zone with respect to the longitudinal axis; an inner twist zone, wherein the CNTs of the outer twist zone and the inner twist zone are twisted in opposite directions with respect to the longitudinal axis.
  • the invention is further a system for drawing carbon nanotubes (CNTs) from a substrate comprising: an array of CNTs formed on the substrate about an axis; a vacuum device comprising a low pressure orifice, a high pressure orifice, and an intermediate pressure orifice, the low pressure orifice arranged at a distance (d) from the array of CNTs along the axis; wherein the low pressure orifice draws the CNTs from the substrate aligned substantially parallel to the axis.
  • CNTs carbon nanotubes
  • the low pressure orifice comprises a size an a shape substantially relating to a change in pressure along the axis; the change in pressure substantially relating to a velocity gradient along the axis, wherein the velocity gradient is proportional to a CNT removal rate and a velocity of the CNTs along the axis which can be controlled by a user by selecting the low pressure orifice size and shape.
  • the distance (d) can be adjusted by a user to affect a removal rate of the CNTs from the substrate.
  • conductive particles are introduced at the high pressure orifice, wherein the conductive particles combine with the CNTs to make a resulting mass that has a greater electrical conductivity than the CNTs alone.
  • the system is characterized wherein the vacuum device has a cavity, the cavity having a velocity gradient associated therewith, the velocity gradient able to strip electrons from an air mixture within the cavity creating a plasma mass, the plasma mass combining with the CNTs removed from the substrate making a resulting mass more electrically conductive.
  • the invention is a method for drawing carbon nanotubes (CNTs) from a CNT array on a substrate comprising the steps of: aligning a vacuum device low pressure orifice at a distance (d) to the CNTs; applying a velocity gradient to the CNT array to remove the CNTs using the low pressure orifice.
  • This method further comprises varying a size and a shape of the low pressure orifice to affect the velocity gradient as chosen by a user; and varying the distance (d) to affect the velocity gradient as chosen by the user.
  • this method includes the steps of: introducing conductive particles to the vacuum device; combining the conductive particles to the CNTs within the vacuum device, making a combination that is more electrically conductive as compared to the CNTs alone.
  • This method additionally includes: configuring the vacuum device to contain within a velocity gradient; stripping electrons from an air mixture within the vacuum device using the velocity gradient creating a plasma mass; combining the plasma mass to the CNTs within the vacuum device, making a combination that is more electrically conductive as compared to the CNTs alone.
  • the invention is a system for making a base yarn from carbon nanotubes (CNTs) comprising: a CNT array grown on a substrate; a mechanical roller to remove the CNTs from the CNT array; a vacuum device for drafting the CNTs into a sliver; and a first spin zone to impart a rotational force on the sliver to form a base yarn.
  • CNTs carbon nanotubes
  • this embodiment is characterized wherein the CNTs are removed from the substrate in the form of a web, the system further comprising: a first set of rollers to draft the CNT web into a sliver; and a second set of rollers to further draft the CNT sliver.
  • the system in this particular embodiment is further characterized wherein the CNT web is a first CNT web, further comprising a convergence zone to direct the CNT web into the first set of rollers; and a second CNT web wherein the first and second CNT webs combine in the convergence zone.
  • This system further comprises: a second spin zone to impart a rotational force in a reverse direction of that the first spin zone; and a spool to take up the base yarn. More specifically, the rotational force is imparted with a magnetic flux. Or optionally, the rotational force is imparted with forced air.
  • the invention is not only applicable to CNT fibers and comprises a method for forming yarn from electrically conductive fibers, the method comprising: providing the electrically conductive fibers (ECFs) upstream from a spin zone; directing the ECFs into the spin zone; twisting the ECFs, using a rotating magnetic field, producing a yarn having a twist rate associated therewith. This further comprises drafting the ECFs using a vacuum device prior to the directing and the twisting.
  • ECFs electrically conductive fibers
  • the invention is an induction motor comprising: a center axis; a plurality of pole segments radially aligned about the center axis; a plurality of conductive wires wrapped around each of the plurality of pole segments, the plurality of pole segments and the conductive wires together forming a motor stator assembly; a rotor area located in an area closest to the center axis; a polyphase AC current applied to the plurality of conductive wires producing a rotating magnetic field in the rotor area, the rotor area having a multiplicity of electrically conductive carbon nanotube fibers (CNTs), the rotating magnetic field imparting a rotational force on the CNTs.
  • CNTs electrically conductive carbon nanotube fibers
  • the induction motor of the present invention is characterized wherein the pole segments comprise end portions; the end portions shaped with a point generally pointed though the center axis. Further to the induction motor the plurality of pole segments comprises powdered ferrite to minimize core losses.
  • the induction motor is claimed wherein the rotor area contains a liquid medium having a density greater than the CNTs, wherein the liquid medium and the CNTs rotate together causing a centripetal force on the CNTs with respect to the center axis.
  • FIG. 1A is an illustration of side and end views of an exemplary single-walled carbon nanotube (SWNT).
  • SWNT single-walled carbon nanotube
  • Figure IB illustrates an example of how fiber, in general, is twisted to form yarn.
  • Figure 1C further illustrates generally how yarn is twisted and the direction of twist.
  • Figures 2A through 2C generally illustrate the process by which CNTs are drawn from a substrate and twisted together to form base yarn, wherein several base yarns are further cabled together to form a thicker yarn suitable for commercial applications.
  • Figure 3 A is a schematic illustration of an exemplary vacuum drawing device of the present invention.
  • Figure 3B is a perspective view of a similar apparatus as shown in Fig. 3 A also illustrating the low pressure vacuum orifice of the present invention having different shapes to achieve a predetermined velocity gradient.
  • Figures 3 C and 3D illustrate alternative embodiments of the low pressure orifice of the present invention.
  • Figure 4A-C are drawings to be viewed in succession, illustrating an embodiment for making base yarn of the present invention.
  • Figure 5 A is a perspective illustration of an induction motor configured to serve as a spin zone of the present invention
  • Figure 5B is a top plan view of the induction motor of Fig. 5 A.
  • Figure 6 is a stress vs. strain curve for yarn made from CNTs
  • Vacuum device (350) contains low pressure (310), high pressure (330) and intermediate pressure (320) orifices, with corresponding pressures associated therewith P 1 P 3 P 2 , where P 1 ⁇ P 2 ⁇ P 3 .
  • P 2 P ATM - More specifically, in a preferred embodiment, P 1 is vacuum pressure at 0 psi, P 1 is in the range of 14 to 30 psi, and P 3 is around 30 psi, with all pressures being absolute.
  • Air velocities V 1 and V 3 are in the range of 100 to 332 m/s.
  • System (300) overcomes an issue in the prior art where if the CNTs (110) are removed too rapidly, the relatively weak forces holding successive rows of CNTs together will break. In the past the removal rate has been very slow on the order of a few cm/min that is not very practical for commercial yarn production.
  • the present invention not only draws the CNTs from the substrate, but also drafts the CNTs. Drafting the CNTs will pull the parallel CNTs closer together where Van der Waals forces between CNTs will cause them the stick together. The result is that the CNTs can be removed at a much higher rate.
  • the vacuum force and corresponding air velocity is operable to exceed 100 m/s at a distance three times the orifice diameter at the leading edge of the CNT substrate.
  • other speed variables include vacuum force (pressure differential) and shape of the orifice (as shown in Figs. 3B-3D).
  • the present invention additionally contemplates adding conductive particles (361) at high pressure orifice (330).
  • the conductive particles (361) will combine with the CNTs to form a resulting mass that is more conductive.
  • These particles (361) could be mechanically inert for example, nanospheres. These nanospheres could be electrically conducting such as copper. They could also have a high permeability such as ferrite spheres.
  • the conducting particles (361) would be more dense than the CNTs (110) facilitating removal later. While in the small bore (520) of the spin zone, the rotational acceleration would force the particles to the outer region of the spin zone and separate the particles from the CNTs. The spheres (361) could then be recycled.
  • a conducting liquid could also be employed.
  • the liquid being more dense would compact the CNTs in the spin zone. As required in the industry, higher strength yarns are compacted while being spun. Further along in the yarn production, as the CNTs sliver is spun using an electromagnetic spin zone (440, Figs. 5 A-B), the yarn made therefrom would be spun more tightly and therefore have a higher strength.
  • Low pressure conducting Plasma with possibly non-oxidizing gases (362) would similarly serve to increase conductivity of a resulting mass as it mixes with the CNTs. Plasma (362) is formed within vacuum cavity (363) when the velocity gradient causes the air inside to be stripped of its electrons.
  • CNTs (110) may be more generally labeled as electrically conductive fibers (ECFs).
  • vacuum device (350) is comparatively located further downstream in the yarn production process than in the Fig. 3 example.
  • Vacuum (350) now serves to draft and align the sliver (413) to the spin zone (440).
  • a vacuum force (350) could be located downstream of the spin zones (440, 441).
  • high (330), intermediate (320) and low pressure (310) ports are configured differently as compared to Fig. 3 A.
  • Fig 4A illustrates CNT array (210) having CNTs mechanically drafted therefrom using roller (415).
  • a CNT web (410) results from this process and the web is drawn more closely together using convergence zone (420).
  • an additional web (411) (or multiple webs) drawn from another substrate could be combined in convergence zone (420).
  • First roller (430) drafts the incoming cluster of fibers (412) into a sliver (413). This drafting, causing the fibers to be more elongated, will ultimately result in higher twist rates and a stronger base yarn (480).
  • Second set of rollers (431) further drafts sliver (413) wherein second rollers (431) rotate faster than first set of rollers (430).
  • first spin zone (440) is configured to only spin the outer fibers (460) of sliver (413) while second spin zone (441) is configured to spin inner fibers (461) in the opposite direction of first spin zone (440).
  • the resulting base yarn (480) will have a false twist and a zero net twist about axis (450).
  • Base yarn (480) is taken in by spool (470) and it is to be further appreciated that base yarn (480) could be cabled with other base yarns, similar to Fig. 2C.
  • CNTs could be blended with other materials throughout the process, to form materials with different structural properties. These materials could be any high strength engineering material such as carbon fibers, glasses, and aramid fibers. Natural materials such as cotton, hemp and others may also be used. The percentages of any added fiber would be determined per the specific application.
  • the base yarn (480) will be about the same size as individual cotton fibers. Therefore, the base yarn could alternatively be cut at around one inch intervals similar to cotton fibers (120) and then integrated to existing textile systems.
  • induction motor (440) of present invention is illustrated, hi this particular embodiment, induction motor (440) will provide a true twist, different from spin zones (440, 441) of Fig. 4C.
  • Motor (440) has a polyphase AC current supplied to the stator windings (532). The applied current results in a rotating magnetic field of constant magnitude in the space occupied by the rotor (520). The field rotates at synchronous speed determined by the frequency and phase of the AC current, and the number of poles in the stator winding (532). hi this .
  • a pair of pole segments (533) about center axis (450) make up a stator pole, hi place of a typical rotor, the CNTs sliver (413) will serve as the rotor conductor.
  • the rotating magnetic field cuts the conductor in the rotor (413)
  • voltages are induced and current flows.
  • These currents experience a sideways force due to the magnitude of the stator (530) magnetic field. The resulting torque will pull it in the same direction of rotation as the stator field.
  • the invention embodiment of Figs. 5A-5B is an improvement over existing spin zones having a conventional rotor, because a rotor spinning at such high speeds (10 5 Hz) will cause the outer surface to have a velocity greater than the speed of sound. In practice, this has caused problems of instability. Because the CNT rotor (413) is so small, the surface velocity stays below the speed of sound and it can spin relatively faster.
  • a preferred embodiment of motor 440 uses a four phase system.
  • Pole segments (533) contain end portions (531) that are pointed in shape to help direct the rotating magnetic field to the small diameter CNT web (413).
  • a power ferrite is used over an iron laminate on pole segments (533) to help protect against eddy current and core loses to allow the rotating magnetic field to keep changing at high speeds.
  • the low density property of the CNTs (110) will allow the CNTs
  • liquid may occupy the rotor area (520).
  • a conducting liquid in particular, may be used where the spin is produced electromagnetically. In this design the rotational chamber (520) is kept small to reduce pressures created by centripetal acceleration.
  • Fig. 6 the stress vs. strain properties of yarn made from CNTs (110) is illustrated. Since it has been observed that the resistance of CNT yarn (480) should follow the stress vs. strain curve, the present invention seeks to provide a method of non-destructive testing by measuring the resistance of the resultant yarn during testing. Hence, essentially working backward, a peak strain and yield strength of the yarn (480) could be determined.
  • the method relies on the electrical conducting properties of the CNTs.
  • This system utilizes the unique electrical conducting properties of the CNTs to manipulate the fibers to twist around themselves to form the yarn.
  • the electrical resistance in the longitudinal direction of the yarn provides manufacturing information on the diameter, packing density and twist rate, even during production of the yarn, which provides inputs to yarn control systems and methods for ensuring uniformity and quality of strength and other yarn properties, preferably in real-time feedback on the machine during the operation of the method.
  • the system and methods are also operable to detect defects and approaching defects such as thin places, thick places, or material composition, with corrective or other adjustments being made as part of the preferred process of making the CNT yarn.
  • Dynamic resistance methods using time-dependent electrical current operate to allow more precise observation of the structural properties of the CNT yarns in real time during the production and post analysis.
  • Dynamic inspection can be measured by inducing electrical current into the fabricated yarn and monitoring the eddy current relaxation generated from the applied time-dependent magnetic field. These measurements will detect variations in the structural properties of the CNT yarn (480) by comparing against known measurements.
  • An alternate method of the present invention is to measure the capacitance of two plates with the yarn passing between the plates. Still further, an alternate method would be to measure the capacitance of a coaxial capacitor where the conducting CNT yarn becomes the center conductor of the coaxial capacitor and comparing against known values.
  • These electrical properties of the CNT can be applied to measure stress-strain behavior of the CNT yarn.
  • This system is operable to provide a non-destructive method for measuring properties such as peak strain to monitor and control critical CNT yarn strength properties.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Inorganic Fibers (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)

Abstract

L'invention concerne un système et un procédé pour le traitement de nanotubes de carbone (NTC) pour former un arrangement longitudinal structuré, ou un fil de base. L'invention concerne également un arrangement de NTC ayant une multiplicité de NTC disposés sur un substrat et plusieurs procédés pour le retrait. L'invention concerne également un dispositif d'étirage pour aligner et étirer les NTC afin de former un ruban d'étirage, un appareil de filage comprenant au moins une zone de torsion pour assurer la rotation aux NTC ou au ruban d'étirage pour obtenir une orientation torsadée, diamétralement condensée, longitudinale, des fibres de NTC, et la reprise pour le ramassage du fil. De préférence, le système pour traiter les NTC afin de former un arrangement longitudinal structuré est un procédé de filage ; de façon encore plus préférée, c'est un procédé de filage électromagnétique (EM).
PCT/US2007/075903 2006-08-14 2007-08-14 Système et procédés pour centrifuger des nanotubes de carbone en fil, et fil obtenu par ce système et ces procédés WO2008022129A2 (fr)

Applications Claiming Priority (6)

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US83748406P 2006-08-14 2006-08-14
US60/837,484 2006-08-14
US84543006P 2006-09-18 2006-09-18
US84538006P 2006-09-18 2006-09-18
US60/845,380 2006-09-18
US60/845,430 2006-09-18

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WO2008022129A3 WO2008022129A3 (fr) 2008-06-26

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WO2015001668A1 (fr) 2013-07-05 2015-01-08 村田機械株式会社 Appareil de fabrication de fil
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JP5943149B2 (ja) * 2013-07-22 2016-06-29 村田機械株式会社 糸製造装置
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WO2017131061A1 (fr) * 2016-01-29 2017-08-03 日立造船株式会社 Procédé permettant de fabriquer un fil de nanotubes de carbone
WO2017135234A1 (fr) * 2016-02-04 2017-08-10 日立造船株式会社 Procédé de production d'un fil torsadé de nanotubes de carbone, et fil torsadé de nanotubes de carbone
CN112391712A (zh) * 2019-08-12 2021-02-23 中国科学院苏州纳米技术与纳米仿生研究所 一种碳纳米管弹性包芯纱及其制备方法与应用
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Cited By (35)

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KR101578082B1 (ko) * 2008-07-16 2015-12-16 주식회사 뉴파워 프라즈마 전기 전도성 복합 소재로 구성되는 유도 코일을 구비한 전기 모터를 탑재한 전기 자동차
KR20100008731A (ko) * 2008-07-16 2010-01-26 주식회사 뉴파워 프라즈마 전기 전도성 복합 소재로 구성되는 유도 코일을 구비한전기 모터 및 이를 구비한 전기 자동차
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