WO2019183767A1 - 收集装置及制备系统 - Google Patents

收集装置及制备系统 Download PDF

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Publication number
WO2019183767A1
WO2019183767A1 PCT/CN2018/080532 CN2018080532W WO2019183767A1 WO 2019183767 A1 WO2019183767 A1 WO 2019183767A1 CN 2018080532 W CN2018080532 W CN 2018080532W WO 2019183767 A1 WO2019183767 A1 WO 2019183767A1
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WIPO (PCT)
Prior art keywords
carbon nanotube
wheel body
collecting device
adjustment
collecting
Prior art date
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PCT/CN2018/080532
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English (en)
French (fr)
Inventor
李达
金赫华
李清文
勇振中
刘毛林
胡殿利
Original Assignee
苏州捷迪纳米科技有限公司
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Application filed by 苏州捷迪纳米科技有限公司 filed Critical 苏州捷迪纳米科技有限公司
Priority to JP2021501063A priority Critical patent/JP7089108B2/ja
Priority to RU2020134904A priority patent/RU2755803C1/ru
Priority to EP18912485.2A priority patent/EP3778460B1/en
Priority to PCT/CN2018/080532 priority patent/WO2019183767A1/zh
Priority to US17/042,014 priority patent/US11970355B2/en
Priority to KR1020207030795A priority patent/KR102445848B1/ko
Publication of WO2019183767A1 publication Critical patent/WO2019183767A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65H—HANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
    • B65H51/00—Forwarding filamentary material
    • B65H51/02—Rotary devices, e.g. with helical forwarding surfaces
    • B65H51/04—Rollers, pulleys, capstans, or intermeshing rotary elements
    • B65H51/08—Rollers, pulleys, capstans, or intermeshing rotary elements arranged to operate in groups or in co-operation with other elements
    • B65H51/10—Rollers, pulleys, capstans, or intermeshing rotary elements arranged to operate in groups or in co-operation with other elements with opposed coacting surfaces, e.g. providing nips
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65H—HANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
    • B65H54/00—Winding, coiling, or depositing filamentary material
    • B65H54/02—Winding and traversing material on to reels, bobbins, tubes, or like package cores or formers
    • B65H54/28—Traversing devices; Package-shaping arrangements
    • B65H54/2848—Arrangements for aligned winding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B1/00—Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • 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
    • D01F9/133—Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65H—HANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
    • B65H54/00—Winding, coiling, or depositing filamentary material
    • B65H54/02—Winding and traversing material on to reels, bobbins, tubes, or like package cores or formers
    • B65H54/28—Traversing devices; Package-shaping arrangements
    • B65H54/2803—Traversing devices; Package-shaping arrangements with a traversely moving package
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65H—HANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
    • B65H54/00—Winding, coiling, or depositing filamentary material
    • B65H54/70—Other constructional features of yarn-winding machines
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65H—HANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
    • B65H57/00—Guides for filamentary materials; Supports therefor
    • B65H57/14—Pulleys, rollers, or rotary bars
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • 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
    • C01B32/168—After-treatment
    • 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
    • D01D7/00—Collecting the newly-spun products
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65H—HANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
    • B65H2404/00—Parts for transporting or guiding the handled material
    • B65H2404/10—Rollers
    • B65H2404/13—Details of longitudinal profile
    • B65H2404/131—Details of longitudinal profile shape
    • B65H2404/1316—Details of longitudinal profile shape stepped or grooved
    • B65H2404/13161—Regularly spaced grooves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65H—HANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
    • B65H2701/00—Handled material; Storage means
    • B65H2701/30—Handled filamentary material
    • B65H2701/31—Textiles threads or artificial strands of filaments
    • B65H2701/314—Carbon fibres

Definitions

  • the invention relates to the technical field of carbon nanotube material preparation, in particular to a collecting device and a preparation system.
  • Carbon nanotubes are tubular one-dimensional nanomaterials made of single or multi-layer graphene. The unique structure gives them excellent strength, heat and electrical properties. CNTs have theoretically good mechanical, electrical and thermal properties and have great application prospects. Carbon nanotube film and carbon nanotube fiber formed by intertwining carbon nanotubes are common macroscopic bodies of carbon nanotubes, which can exert excellent performance of carbon nanotubes, and are in the fields of electromagnetic shielding, composite materials, electric heating, and the like. Wide application prospects. However, the actual prepared carbon nanotube macroscopic body has poor orientation and uniformity, and affects various properties of the final carbon nanotube macroscopic body.
  • the invention provides a collecting device for collecting carbon nanotube film or carbon nanotube fiber, comprising:
  • a pre-adjustment mechanism for adjusting an orientation of at least one bundle of carbon nanotube aggregates, the pre-adjustment mechanism comprising a first pre-adjustment sub-mechanism and a second pre-adjustment sub-mechanism; the first pre-adjustment sub-mechanism at least including along a first wheel body and a second wheel body disposed in one direction and rotatable, the first wheel body and the second wheel body being used for pre-pressing both sides of the carbon nanotube aggregate; the second pre- The adjustment sub-assembly includes at least a third wheel body for drawing carbon nanotube aggregates;
  • a winding mechanism for winding the carbon nanotube aggregates drawn from the pre-adjustment mechanism is provided.
  • the collecting device adjusts the orientation of at least one bundle of carbon nanotubes by adding the first pre-adjusting sub-mechanism and the second pre-adjusting sub-mechanism, thereby improving not only the internal structure of the carbon nanotube but also the carbon.
  • the orientation and uniformity of the nanotubes achieve the regulation of the force, electrical and thermal properties of the collected carbon nanotube materials, and contribute to the large-scale production of carbon nanotube films or carbon nanotube fibers of carbon nanotube materials with different properties.
  • the third wheel body is rotatable and is surrounded by a plurality of first annular protrusions for aligning the orientation of the carbon nanotube aggregates.
  • the first annular protrusion has a width of no more than 10 ⁇ m, and a spacing of the adjacent first annular protrusions is not more than 100 ⁇ m.
  • the collecting device further includes a first heating mechanism for adjusting a contact surface of the first pre-adjusting sub-mechanism and/or the second pre-adjusting sub-mechanism with the carbon nanotube aggregate temperature.
  • the contact surface of the first wheel body and/or the second wheel body with the carbon nanotube aggregate is provided with an annular limiting groove capable of accommodating the carbon nanotube aggregate.
  • the second pre-adjusting sub-mechanism further includes a fourth wheel body, the fourth wheel body and the third wheel body are spaced apart from each other in the second direction and are capable of collecting carbon nanotubes The body is drawn in the collecting direction.
  • the fourth wheel body is rotatable and is surrounded by a plurality of second annular protrusions for aligning the orientation of the carbon nanotube aggregates.
  • the width of the second annular protrusion is no more than 10 ⁇ m, and the spacing of the adjacent second annular protrusions is not more than 100 ⁇ m.
  • first wheel body and the second wheel body are oppositely rotated or turned to the opposite side, and the third wheel body and the fourth wheel body have different rotational speeds.
  • the first direction and the second direction are perpendicular to each other.
  • the winding mechanism includes a drum that is expandable and contractible in the axial direction, the drum being reciprocable and the reciprocating direction being non-perpendicular to the axial direction of the drum.
  • the winding mechanism includes a first reel, a second reel, and a collection belt that is tensioned between the first reel and the second reel; or
  • the winding mechanism includes a first rotating wheel, a second rotating wheel, and a collecting plate disposed between the first rotating wheel and the second rotating wheel and rotatable toward the pre-adjusting mechanism.
  • the spacing between the first reel and the second reel can be adjusted.
  • the invention also provides a preparation system for preparing a carbon nanotube film material or a carbon nanotube fiber material, comprising:
  • a synthesis device for floating catalytic synthesis of carbon nanotube aggregates comprising a reactor having at least one growth tube;
  • the collecting device is any one of the above collecting devices, and the collecting device is located at an outlet end side of the synthesizing device for collecting carbon nanotube aggregates prepared by the synthesizing device.
  • the growth tube is flared or cylindrical near the end of the collection device.
  • the tubular shape of the growth tube is square.
  • the preparation system further comprises:
  • a charging device for providing a reaction material and communicating with an inlet end of the synthesis device, the charging device comprising at least one injection mechanism and at least one feeding tube, one end of the feeding tube being in communication with the injection mechanism and the other end
  • the growth tubes are in communication.
  • the synthesis apparatus includes a reactor having a plurality of growth tubes arranged in a circular or matrix distribution.
  • the synthesizing device further includes a second heating mechanism for adjusting the temperature distribution of each of the inlet ends of the plurality of growth tubes.
  • FIG. 1 is a schematic structural view of a collecting device according to an embodiment of the present invention.
  • FIG. 2 is a schematic structural view of a collecting device according to another embodiment of the present invention.
  • Figure 3 is a cross-sectional view of the third wheel body of Figure 2;
  • Figure 4 is a cross-sectional view of the fourth wheel body of Figure 2;
  • Figure 5 is a side view of the first pre-adjustment mechanism of Figure 2;
  • FIG. 6 is a schematic structural view of a winding mechanism according to an embodiment of the present invention.
  • FIG. 7 is a schematic structural view of a collecting device according to still another embodiment of the present invention.
  • FIG. 8 is a schematic structural view of a preparation system according to an embodiment of the present invention.
  • Figure 9 is a side elevational view showing a partial structure of a synthesizing apparatus according to an embodiment of the present invention.
  • FIG. 10 is a SEM photograph of a sample 1 of a carbon nanotube film produced by a preparation system according to an embodiment of the present invention.
  • Figure 11 is a SEM photograph of a carbon nanotube film product sample 2 prepared by a comparative preparation system
  • Figure 12 is a graph of tensile stress-elongation at break of two carbon nanotube film products
  • Figure 13 is a schematic view showing the structure of a preparation system according to another embodiment of the present invention.
  • first pre-adjusting sub-mechanism 111, first wheel body, 112, second wheel body, 120, second pre-adjusting sub-mechanism, 121, third wheel body, 122, fourth wheel body , 130, winding mechanism, 131, first rotating wheel, 132, second rotating wheel, 133, collecting plate, 140, first annular protrusion, 150, second annular protrusion, 160, annular limiting groove;
  • feeding device 310
  • injection mechanism 320
  • feeding tube 400
  • carbon nanotube aggregates
  • Figure 1 illustrates a collection device 100 of the present invention.
  • the collection device 100 is used for collection of carbon nanotube film or carbon nanotube fibers, including a housing in communication with the outlet end of the synthesis device 200 and a pre-adjustment mechanism and winding mechanism 130 disposed within the housing.
  • a pre-adjustment mechanism is disposed in the housing and configured to adjust an orientation of the at least one bundle of carbon nanotube aggregates 400.
  • the pre-adjustment mechanism is used to adjust the orientation of a bundle of carbon nanotube aggregates, and can also be used to adjust the orientation of a plurality of bundles of carbon nanotube aggregates.
  • the pre-adjustment mechanism includes a first pre-adjustment sub-mechanism 110 and a second pre-adjustment sub-mechanism 120.
  • the first pre-adjustment sub-structure 110 includes at least a first wheel body 111 and a second wheel body 112 disposed in the first direction and rotatable, and the first wheel body 111 and the second wheel body 112 are used for the carbon nanotube aggregate
  • the two pre-compensation mechanisms 120 include at least a third wheel body 121 for drawing carbon nanotube aggregates.
  • the first wheel body 111, the second wheel body 112 and the third wheel body 121 may be a rotatable roller or roller structure, and the size thereof is matched with the carbon nanotube aggregate.
  • the carbon nanotube aggregates are first adjusted by the first pre-adjustment sub-structure 110, and then adjusted by the second pre-adjustment sub-structure 120.
  • the winding mechanism 130 is used for winding collection of carbon nanotube aggregates drawn from the pre-adjustment mechanism.
  • the collecting device 100 is configured to adjust the orientation of at least one bundle of carbon nanotubes by adding the first pre-adjusting sub-structure 110 and the second pre-adjusting sub-mechanism 120, respectively, not only improving the internal structure of the carbon nanotubes, but also The orientation and uniformity of the carbon nanotubes are improved, and the regulation of the force, electric and thermal properties of the carbon nanotube material is obtained, which contributes to the large-scale production of carbon nanotube films or carbon nanotube fibers with different properties.
  • the direction of the connection from the outlet end to the collecting mechanism is defined as the M direction
  • the M direction is defined as the rear end near the outlet end side, and the front end side away from the exit end side, and the left and right sides of the M direction are defined.
  • the left and right sides of the end and the upper and lower ends respectively correspond to the upper and lower sides.
  • the collecting device 100 for a horizontal furnace body is shown.
  • the collection device 100 is used for collection of carbon nanotube film or carbon nanotube fibers, which includes a housing, a pre-adjustment mechanism, and a winding mechanism 130.
  • the pre-adjustment mechanism includes a first pre-adjustment sub-mechanism 110 and a second pre-adjustment sub-mechanism 120, and is used for adjusting a plurality of bundles of carbon nanotube aggregates.
  • the first adjustment sub-structure 110 is disposed near the outlet end, and the second pre-adjustment sub-structure 120 is disposed between the first adjustment sub-structure 110 and the winding mechanism 130.
  • the first wheel body 111 and the second wheel body 112 are preferably disposed on the left and right sides of the M direction, that is, the first wheel body 111 and the second wheel body 112 are disposed on the left and right sides of the carbon nanotube aggregate.
  • each bundle of carbon nanotube aggregates is inconsistent in the direction of traction and the axial direction of the carbon nanotubes, and it is difficult to achieve uniform collection of multi-beam carbon nanotube aggregates.
  • the internal structure of the carbon nanotube material has a significant impact on various properties, and thus affects the overall performance of the carbon nanotube material.
  • the positive pressure exerted by the first wheel body 111 and the second wheel body 112 on the carbon nanotube aggregate can be changed to achieve different
  • the bundling and drawing effects are used to adjust the orientation of the carbon nanotube aggregates, thereby regulating the properties of the carbon nanotube material.
  • the spacing, the rotational speed, and the position between the first wheel body 111 and the second wheel body 112 can be adjusted correspondingly according to the yield and the output rate of the carbon nanotube aggregates to achieve the optimal pre-adjustment effect.
  • the wheel bodies disposed in the first direction may always be two, that is, only the first wheel body 111 and the second wheel body 112.
  • the number of wheel bodies disposed in the first direction may be other multiples, and preferably, the number of bundles of carbon nanotubes may be matched.
  • the second adjustment sub-assembly 120 includes a third wheel body 121 disposed on the lower side of the M direction, that is, the third wheel body 121 is disposed on the lower side of the carbon nanotube aggregate.
  • the third wheel body 121 is rotatable and is surrounded by a plurality of first annular protrusions 140 for aligning the orientation of the carbon nanotube aggregates.
  • a plurality of first annular protrusions 140 are disposed on the contact surface of the third wheel body 121 and the carbon nanotube aggregate.
  • the first annular protrusion 140 is disposed around the axial direction of the third wheel body 121, and the first ring is formed.
  • the width of the protrusions 140 is not more than 10 ⁇ m, and the pitch of the adjacent first annular protrusions 140 is not more than 100 ⁇ m.
  • the first wheel body 111 and the second wheel body 112 are rotatable and the directions of rotation of the two may be the same or different.
  • the first wheel body 111 and the second wheel body 112 rotate in opposite directions, and further preferably, the two may be opposite or reverse.
  • the width of the first annular protrusions 140 is not more than 10 ⁇ m, and the spacing of adjacent first annular protrusions 140 is not more than 100 ⁇ m.
  • the first annular protrusion 140 has a width of 0.2 to 5 ⁇ m, and the adjacent first annular protrusions 140 have a pitch of 50 to 90 ⁇ m.
  • the height of the first annular protrusion 140 may be 1 to 10 mm.
  • the first annular protrusion 140 may be integrally formed with the third wheel body 121, or may be separately formed and detachably mounted on the third wheel body 121.
  • the first annular protrusion 140 can be processed by laser etching or chemical etching or printing.
  • the first annular protrusion 140 When the third wheel body 121 rotates, the corresponding first annular protrusion 140 is rotated, and the first annular protrusion 140 is a plurality of spaced protrusions, which can perform the tangential force on the carbon nanotube aggregate.
  • the internal structure of the carbon nanotube aggregates is arranged to help align in a tangential direction.
  • the first annular protrusions 140 can also apply a certain positive pressure to the carbon nanotube aggregates respectively, and the third wheel body 121 is applied to the carbon nanotube aggregates by adjusting the rotation speed of the third wheel body 121. The pressure is different to achieve the drafting of the carbon nanotube aggregates to adjust the orientation of the carbon nanotube aggregates, thereby regulating the properties of the carbon nanotube material.
  • the second pre-adjusting sub-mechanism 120 further includes at least a fourth wheel body 122 that is rotatable, and the fourth wheel body 122 and the third wheel body 121 are spaced apart in the second direction and are Both can draw the carbon nanotube aggregates in the collecting direction.
  • the second direction is different from the first direction, and preferably the second direction and the first direction are perpendicular to each other.
  • the second direction and the first direction may also be other cases.
  • the fourth wheel body 122 and the third wheel body 121 are disposed on the upper and lower sides or the left and right sides of the M direction, and the positions of the two are set according to the arrangement of the first wheel body 111 and the second wheel body 112. Adjustment. Since the fourth wheel body 122 is added, by adjusting the fourth wheel body 122 and the third wheel body 121 to different rotational speeds, the edges applied by the third wheel body 121 and the fourth wheel body 122 to the carbon nanotube aggregates can be changed.
  • the positive pressure in the second direction is to further extract the carbon nanotube aggregates, and further adjust the orientation of the carbon nanotube aggregates, thereby achieving controllable adjustment of various properties of the carbon nanotube materials.
  • the number of the third wheel body 121 and the fourth wheel body 122 is the same and one. In other embodiments, the number of the third wheel body 121 and the fourth wheel body 122 may be two. Or more than one. In this way, by increasing the plurality of wheel bodies to perform various degrees of drafting on the carbon nanotube aggregates, the microstructure inside the carbon nanotube aggregates is further adjusted, and the orientation of the carbon nanotube aggregates is improved.
  • the fourth wheel body is surrounded by a plurality of second annular protrusions 150 for aligning the orientation of the carbon nanotube aggregates.
  • a plurality of second annular protrusions 150 may be disposed on the contact surface of the fourth wheel body 122 with the carbon nanotube aggregates, and the second annular protrusions 150 are disposed around the axial direction of the fourth wheel body 122.
  • the width of the second annular protrusion 150 is not more than 10 ⁇ m, and the pitch of the adjacent second annular protrusions 150 is not more than 100 ⁇ m. Similar to the first annular projection 140, preferably, the second annular projection 150 has a width of 0.2 to 5 ⁇ m, and the adjacent second annular projection 150 has a pitch of 1 to 80 ⁇ m. The height of the second annular projection 150 may be 1 to 10 mm. Further, the second annular protrusion 150 may be integrally formed with the corresponding fourth wheel body 122, or may be separately formed and detachably mounted on the corresponding fourth wheel body 122. The second annular protrusion 150 can be processed by laser etching or chemical etching or printing.
  • first annular protrusion 140 and the second annular protrusion 150 may be symmetrically distributed or may be staggered.
  • the corresponding first annular protrusion 140 and the second annular protrusion 150 are rotated, and the annular protrusions are a plurality of spaced protrusions, which can be used for carbon
  • the nanotube aggregates perform a force along the tangential direction to help arrange the internal structure of the carbon nanotube aggregates in the tangential direction to optimize the orientation adjustment effect.
  • the first annular protrusion 140 and the second annular protrusion 150 can also apply a certain positive pressure to both sides of the carbon nanotube aggregate, respectively, by adjusting the third wheel body 121 and the fourth wheel body 122 to different speeds.
  • the third wheel body 121 and the fourth wheel body 122 apply different positive pressures in the first direction to the carbon nanotube aggregates to achieve drafting of the carbon nanotube aggregates to adjust the carbon nanotube aggregation.
  • the width and spacing of the protrusions on the first annular protrusion 140 and the second annular protrusion 150 may be the same or different.
  • the widths and spacings of the corresponding protrusions on the first annular protrusion 140 and the second annular protrusion 150 are different, the distribution density of the respective protrusions can be adjusted, thereby achieving different orientation adjustment effects.
  • the middle portion of the contact surface of the first wheel body 111 and/or the second wheel body 112 with the carbon nanotube aggregate is provided with a ring-shaped limit capable of accommodating the carbon nanotube aggregate.
  • Bit slot 160 is provided.
  • the slot span of the annular stop groove 160 matches the size of the carbon nanotube aggregate to be accommodated.
  • the cross section of the annular limiting groove 160 in the axial direction may be a symmetrical triangle.
  • the annular limiting groove 160 has a symmetrical arc-shaped groove in the axial direction.
  • the annular limiting groove 160 can also be a groove of other shapes.
  • the carbon nanotube aggregate can be fixed and constrained not only to prevent the carbon nanotube aggregate from moving up and down when being pre-stressed by the first adjusting sub-structure 110;
  • the carbon nanotube aggregates are effectively collected in the annular limiting groove 160 to further ensure uniform collection and improve the orientation of the collected carbon nanotube aggregates.
  • the collecting device 100 further includes a first heating mechanism (not shown) disposed in the housing and configured to adjust the first pre-adjusting sub-structure 110 and/or the second pre-adjusting sub-mechanism 120 to aggregate with the carbon nanotubes. The temperature of the contact surface of the body.
  • the first heating mechanism includes a heating resistor wire and a controller, and the heating resistor wire is built in the end or inside of the first pre-adjusting sub-system 110 and/or the second pre-adjusting sub-mechanism 120, and the controller is disposed at Inside the housing and used to control the amount of heat generated by the heating resistor wire.
  • the first heating mechanism may also include a thermocouple or thermometer that measures the temperature of the respective contact surface on the pre-adjustment mechanism.
  • the temperature range of the first heating mechanism may be set to 100 to 500 °C. Further, the temperature of the first heating mechanism may range from 200 to 400 °C. It should be noted that the inside of the casing of the collecting device 100 is preferably an inert environment.
  • the gas inside the carbon nanotube aggregate can be discharged by appropriate heating, thereby improving the density of the collected carbon nanotube product.
  • the temperature of the contact surface with the carbon nanotube aggregates can be controlled, thereby improving the adjustment effect of the pre-adjustment mechanism on the internal structure of the carbon nanotube aggregates, improving the orientation and uniformity of the carbon nanotubes, and realizing the collection.
  • the regulation of various properties of carbon nanotube materials are described.
  • the winding mechanism 130 may be a roller that is rotatable to collect carbon nanotube aggregates. Since the carbon nanotube aggregate usually contains a trace amount of iron, the roller may be made of a micromagnetic material, which is advantageous for the adsorption collection of the carbon nanotube aggregate.
  • the winding mechanism 130 may be a drum (not shown) that is expandable and contractible in the axial direction.
  • the sleeve does not need to move the position; and when the collected carbon nanotube aggregate is a carbon nanotube film, the movable drum moves or reciprocates in one direction.
  • the direction of reciprocation is not perpendicular to the axial direction of the drum.
  • the direction of reciprocation is parallel to the axial direction of the drum.
  • the reciprocating direction and the axial direction of the drum may exhibit a certain angle to achieve the collection of the carbon nanotube film.
  • the rotating drum can be axially stretched, so that the area of the collected carbon nanotube film can be further changed, so that the thickness of the prepared carbon nanotube film can be controlled, thereby obtaining carbon nanotube film materials with different properties.
  • the winding mechanism 130 can include a first reel, a second reel, and a collection belt (not shown) that is tensioned between the first reel and the second reel.
  • the axial direction of the first and second reels is perpendicular to the direction of the extension of the outlet end.
  • the spacing between the first rotor and the second rotor can be adjusted.
  • the width direction dimension of the collected carbon nanotube aggregate film is adjusted, thereby adjusting the area of the carbon nanotube film.
  • the winding mechanism 130 may include a first reel 131 , a second reel 132 , and a first reel 131 and a second reel 132 and can be oriented toward The collecting plate 133 is rotated in the direction of the adjustment mechanism.
  • the collecting plate 133 may be a plate member that is slightly magnetic and has a certain thickness.
  • the spacing between the first reel 131 and the second reel 132 can be adjusted.
  • the collecting plate 133 can be configured as a telescopic plate member, so that the length dimension of the collected carbon nanotube aggregate film can be adjusted by adjusting the spacing between the first rotating wheel 131 and the second rotating wheel 132. Further, the area of the carbon nanotube film is adjusted.
  • the vertical furnace body collecting device 100 is shown.
  • the collection device 100 is used for collection of carbon nanotube film or carbon nanotube fibers, including a housing in communication with the outlet end of the synthesis device 200 and a pre-adjustment mechanism and winding mechanism 130 disposed within the housing.
  • the pre-adjustment mechanism includes a first pre-adjustment sub-structure 110 and a second pre-adjustment sub-mechanism 120, and is used to adjust the orientation of a bundle of carbon nanotube aggregates.
  • the present embodiment is different from the first embodiment in that the second adjustment sub-assembly 120 is disposed near the outlet end of the synthesizing device 200.
  • the first pre-adjustment sub-structure 110 is disposed between the second adjustment sub-structure 120 and the winding mechanism 130.
  • the invention also provides a preparation system for the preparation of a carbon nanotube film material or a carbon nanotube fiber material.
  • the preparation system will be described in detail below with reference to the drawings.
  • the preparation system includes a synthesis device 200 and a collection device 100.
  • Synthetic device 200 for floating catalytic synthesis of carbon nanotube aggregates.
  • the synthesis device 200 includes a reactor 210 having at least one growth tube 211.
  • the collecting device 100 is located on the outlet end side of the synthesizing device 200 for collecting carbon nanotube aggregates prepared by the synthesizing device 200.
  • the collection device 100 is in communication with the outlet end of the synthesis device 200.
  • the collection device 100 can be sealingly coupled to the synthesis device 200 via a flange (not shown).
  • the reactor 210 may be a multi-tube horizontal structure, and the number of the growth tubes 211 is two.
  • a plurality of growth tubes 211 are disposed together inside the reactor 210 and share one reaction furnace body.
  • the yield of the carbon nanotubes can be greatly improved, and the quality of the carbon nanotubes in each growth tube 211 can be ensured to improve the performance of the entire carbon nanotube material.
  • the number of the growth tubes 211 may be one or more.
  • the reactor 210 can be horizontally disposed, and of course can also be a multi-tube structure that is inclined at an angle.
  • Growth tube 211 can be prepared from quartz tubes, corundum tubes, or other materials commonly used in the art.
  • the tubular shape of the growth tube 211 is square, which can change the structure of the carbon nanotube aggregates generated by the growth tube 211, thereby adjusting the uniformity of the collected carbon nanotube aggregates.
  • the growth tube 211 can be a conventional hollow tube structure.
  • the end portion of the growth tube 211 close to the collection device 100 has a flared shape.
  • the end of the growth tube 211 in a flared shape, the probability of the carbon nanotube aggregate adhering to the inner wall of the growth tube 211 can be reduced to improve the continuity of the collection of the carbon nanotube aggregate.
  • the end of the growth tube 211 near the collection device 100 can be cylindrical or other conventional shape.
  • the preparation system also includes a charging device 300 in communication with the inlet end of the synthesis device 200 for providing a reaction feed.
  • the charging device 300 may include at least one injection mechanism 310 and at least one feeding tube 320.
  • One end of the feeding tube 320 is in communication with the injection mechanism 310, and the other end is in communication with the growth tube 211.
  • the injection mechanism 310 can be one of a syringe pump, a liquid ejector, and an ultrasonic atomization injection mechanism capable of regulating an injection rate.
  • the number of the feeding tube 320 and the injection mechanism 310 are matched with the number of the growth tubes 211.
  • the feeding tubes 320 may be connected in series or in a side by side manner.
  • the performance of the carbon nanotube material can be regulated by controlling the injection mechanism 310 to separately regulate the carbon nanotube materials prepared by different internal structures.
  • the number of the feeding tube 320 and the injection mechanism 310 may be one, which is simple in structure and easy to operate.
  • the feeding tube 320 may be other than one, and the injection mechanism 310 may be one, such that the plurality of feeding tubes 320 may share one injection mechanism 310.
  • the number of feed tubes 320 and injection mechanisms 310 can also be other reasonable quantities.
  • a plurality of growth tubes 211 may be used to grow carbon nanotube aggregates to prepare a pure carbon nanotube material.
  • one or more of the growth tubes 211 may be disposed to prepare other materials to prepare the carbon nanotube-containing composite material to have different properties of the composite material, and to broaden the application field of the material.
  • the synthesizing apparatus 200 includes a reactor 210 having a plurality of growth tubes 211, which may be arranged in an annular configuration. In other embodiments, the plurality of growth tubes 211 may be arranged in a side-by-side or matrix manner.
  • the synthesizing device 200 further includes a second heating mechanism 212 for adjusting the temperature distribution of each region of the inlet ends of the plurality of growth tubes 211.
  • the second heating mechanism 212 may be three spaced heaters disposed on the inner wall of the reactor 210 to respectively adjust the temperature of each region of the inlet end of the growth tube 211 to control the carbon nanometer.
  • the carbon nanotube film material can be prepared by the preparation system of the present embodiment.
  • the preparation step comprises: firstly dissolving a catalyst and a growth promoter in a carbon source to prepare a reaction liquid, and the reaction liquid is introduced into the growth tube 211 in the reactor 210 through the charging device 300 and the carrier gas, and the catalytic cracking reaction is continuously generated.
  • the carbon nanotube aggregates are collected by collecting continuous aggregates of carbon nanotubes to obtain a carbon nanotube film. Since the preparation process of the carbon nanotube film is relatively common, the above preparation process may be a raw material, a ratio, and a process condition commonly used in the art, and will not be described herein.
  • the carbon nanotube film product prepared by the preparation system (including the pre-adjustment mechanism) of the present embodiment was used, and the obtained product was designated as sample 1.
  • the pre-adjustment mechanism in the preparation system of the present embodiment is removed, and other mechanisms remain unchanged, and this is used as a comparative preparation system (without a pre-adjustment mechanism) and according to the preparation of sample 1
  • the carbon nanotube material film product was also prepared under the process conditions, and the obtained product was designated as sample 2.
  • 10 and 11 are SEM images of Sample 1 and Sample 2, respectively.
  • the orientation of the carbon nanotube material film (sample 1) adjusted by the pre-adjustment mechanism was better than that of the carbon nanotube material film (sample 2) which was not adjusted by the pre-adjustment mechanism.
  • Figure 12 is a graph of tensile stress-elongation at break of Samples 1 and 2.
  • FIG. 13 is a preparation system for a vertical furnace body according to another embodiment of the present invention.
  • the preparation system includes a synthesis device 200 and a collection device 100.
  • Synthetic device 200 for floating catalytic synthesis of carbon nanotube aggregates.
  • the synthesis device 200 includes a reactor 210 having at least one growth tube 211.
  • the collection device 100 is in communication with the outlet end of the synthesis device 200 for collecting carbon nanotube aggregates prepared by the synthesis device 200.
  • the collection device 100 can be sealingly coupled to the synthesis device 200 by a flange.
  • the reactor 210 is a single tube vertical structure. In other embodiments, the reactor 210 can be a multi-tube vertical structure. The reactor 210 can be vertically disposed, and of course can be inclined at an angle.

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Abstract

一种收集装置及制备系统，包括预调整机构，设置于所述壳体内并用于调整至少一束碳纳米管聚集体，其包括分别沿第一方向和第二方向调整碳纳米管聚集体的第一预调整子机构和第二预调整子机构；缠绕机构，用于缠绕收集通过所述预调整机构的碳纳米管聚集体。上述收集装置，通过增加第一预调整子机构和第二预调整子机构，两者分别对至少一束碳纳米管聚集体进行取向调整，不仅改善了碳纳米管内部结构，而且提高了碳纳米管的取向和均匀性，达到了对收集碳纳米管材料的力、电、热学性能的调控。

Description

收集装置及制备系统 技术领域
本发明涉及碳纳米管材料制备技术领域，特别是涉及收集装置及制备系统。
背景技术
碳纳米管(Carbon nanotubes，CNTs)为单层或多层石墨烯卷曲而成的管状一维纳米材料，独特的结构为其带来了优异的力、热、电学性能。CNTs在理论上具有良好的力学、导电和导热性能，具有非常大的应用前景。由碳纳米管相互交织在一起形成的碳纳米管薄膜和碳纳米管纤维是目前常见的碳纳米管宏观体，可以发挥碳纳米管的优异性能，在电磁屏蔽、复合材料、电加热等领域有广泛的应用前景。然而，实际所制备的碳纳米管宏观体的取向性和均匀性较差，影响最终碳纳米管宏观体的各项性能。
发明内容
基于此，有必要针对以上至少一种技术问题，提供一种收集装置及制备系统。
本发明提供一种收集装置，用于碳纳米管膜或碳纳米管纤维的收集，包括：
预调整机构，用于调整至少一束碳纳米管聚集体的取向，所述预调整机构包括第一预调整子机构和第二预调整子机构；所述第一预调整子机构至少包括沿第一方向设置且能够转动的第一轮体和第二轮体，所述第一轮体和所述第二轮体用于对碳纳米管聚集体的两侧进行预压；所述第二预调整子机构至少包括用于对碳纳米管聚集体进行牵伸的第三轮体；
缠绕机构，用于将从预调整机构中引出的碳纳米管聚集体进行缠绕收集。
上述收集装置，通过增加第一预调整子机构和第二预调整子机构，两者分别对至少一束碳纳米管聚集体进行取向调整，不仅改善了碳纳米管内部结构，而且也提高了碳纳米管的取向和均匀性，达到了对收集碳纳米管材料的力、电、热学性能的调控，有助于不同性能碳纳米管材料的碳纳米管薄膜或碳纳米管纤维的规模化生产。
在其中一个实施例中，所述第三轮体能够转动且环绕设有若干第一环形凸起，所述第一环形凸起用于整理碳纳米管聚集体的取向。
在其中一个实施例中，所述第一环形凸起的宽度不大于10μm，且相邻所述第一环形凸起的间距不大于100μm。
在其中一个实施例中，所述收集装置还包括第一加热机构，用于调节所述第一预调整子机构和/或所述第二预调整子机构与碳纳米管聚集体的接触面的温度。
在其中一个实施例中，所述第一轮体和/或所述第二轮体上与碳纳米管聚集体的接触面上开设有能够容纳碳纳米管聚集体的环形限位槽。
在其中一个实施例中，所述第二预调整子机构还包括第四轮体，所述第四轮体和所述第三轮体沿第二方向间隔错开设置且均能够对碳纳米管聚集体沿收集方向进行牵伸。
在其中一个实施例中，所述第四轮体能够转动且环绕设有若干第二环形凸起，所述第二环形凸起用于整理碳纳米管聚集体的取向。
在其中一个实施例中，所述第二环形凸起的宽度不大于10μm，且相邻所述第二环形凸起的间距不大于100μm。
在其中一个实施例中，所述第一轮体和所述第二轮体为相向转动或背向转动，所述第三轮体和所述第四轮体的转速不等。
在其中一个实施例中，所述第一方向与所述第二方向相互垂直。
在其中一个实施例中，所述缠绕机构包括能够沿轴向伸缩的转筒，所述转筒能够做往复运动且所述往复运动方向与所述转筒的轴向方向不垂直。
在其中一个实施例中，所述缠绕机构包括第一转轮、第二转轮和张紧于所述第一转轮和所述第二转轮之间的收集带；或
所述缠绕机构包括第一转轮、第二转轮和设置于所述第一转轮和所述第二转轮之间且能够朝向所述预调整机构方向转动的收集板。
在其中一个实施例中，所述第一转轮和所述第二转轮之间的间距能够调节。
本发明还提供一种制备系统，用于碳纳米管膜材料或碳纳米管纤维材料的制备，包括：
合成装置，用于浮动催化合成碳纳米管聚集体，其包括具有至少一个生长管的反应器；
收集装置，为以上任一所述的收集装置，所述收集装置位于所述合成装置的出口端侧，用于收集所述合成装置所制备的碳纳米管聚集体。
在其中一个实施例中，所述生长管靠近所述收集装置的端部为喇叭状或圆筒状。
在其中一个实施例中，所述生长管的管形为方形。
在其中一个实施例中，所述制备系统还包括：
加料装置，用于提供反应原料且与所述合成装置的入口端连通，所述加料装置包括至少一个注射机构和至少一个加料管，所述加料管的一端与所述注射机构连通，另一端与所述生长管连通。
在其中一个实施例中，所述合成装置包括具有多个生长管的反应器，若干所述生长管的排列方式为环形分布或矩阵分布。
在其中一个实施例中，所述合成装置还包括第二加热机构，用于调节若干个生长管中入口端的各区域的温度分布。
附图说明
图1为本发明一实施方式的收集装置的结构示意图；
图2为本发明另一实施方式的收集装置的结构示意图；
图3为图2中第三轮体的剖视图；
图4为图2中第四轮体的剖视图；
图5为图2中第一预调整子机构的侧视图；
图6为本发明一实施方式的缠绕机构的结构示意图；
图7为本发明又一实施方式的收集装置的结构示意图；
图8为本发明一实施方式的制备系统的结构示意图；
图9为本发明一实施方式合成装置的局部结构的侧视图；
图10为通过本发明一实施方式的制备系统所制备的碳纳米管薄膜产物试样1的SEM照片；
图11为通过对比制备系统所制备的碳纳米管薄膜产物试样2的SEM照片；
图12为两个碳纳米管薄膜产物的拉伸应力-断裂伸长率图；
图13为本发明另一实施方式的制备系统的结构示意图。
图中标记说明：
100、收集装置，110、第一预调整子机构，111、第一轮体，112、第二轮体，120、第二预调整子机构，121、第三轮体，122、第四轮体，130、缠绕机构，131、第一转轮，132、第二转轮，133、收集板，140、第一环形凸起，150、第二环形凸起，160、环形限位槽；
200、合成装置，210、反应器，211、生长管，212、第二加热机构；
300、加料装置，310、注射机构，320、加料管，400、碳纳米管聚集体。
具体实施方式
为使本发明的上述目的、特征和优点能够更加明显易懂，下面结合附图对本发明的具体实施方式做详细的说明。在下面的描述中阐述了很多具体细节以便于充分理解本发明。但是本发明能够以很多不同于在此描述的其它方式来实施，本领域技术人员可以在不违背本发明内涵的情况下做类似改进，因此本发明不受下面公开的具体实施例的限制。
除非另有定义，本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的，不是旨在于限制本发明。本文所使用的术语“和/或”包括一个或多个相关的所列项目的任意的和所有的组合。
图1示意了本发明的收集装置100。收集装置100用于碳纳米管膜或碳纳米管纤维的收集，其包括与合成装置200的出口端连通的壳体以及设置于壳体内的预调整机构和缠绕机构130。
预调整机构，设置于壳体内并用于调整至少一束碳纳米管聚集体400的取向。具体地，预调整机构用于调整一束碳纳米管聚集体的取向，也可用来调整两束及以上多束的碳纳米管聚集体的取向。
预调整机构包括第一预调整子机构110和第二预调整子机构120。
第一预调整子机构110至少包括沿第一方向设置且能够转动的第一轮体111和第二轮体112，第一轮体111和第二轮体112用于对碳纳米管聚集体的两侧进行预压，第二预调整子机构120至少包括用于对碳纳米管聚集体进行牵伸的第三轮体121。该第一轮体111、第二轮体112和第三轮体121可为能够转动的滚轮或辊轮结构，且其尺寸以匹配碳纳米管聚集体为准。在本实施方式中，碳纳米管聚集体先经过第一预调整子机构110进行第一道取向调整，再经过第二预调整子机构120进行第二道取向调整。
缠绕机构130用于将从预调整机构中引出的碳纳米管聚集体进行缠绕收集。
上述的收集装置100，通过增加第一预调整子机构110和第二预调整子机构120，两者分别对至少一束碳纳米管聚集体进行取向调整，不仅改善碳纳米管内部结构，而且也提高了碳纳米管的取向和均匀性，达到了对收集碳纳米管材料的力、电、热学性能的调控，有助于不同性能碳纳米管薄膜或碳纳米管纤维的规模化生产。
请参见图1中，定义图中从出口端至收集机构的连线方向为M方向，定义该M方向上靠近出口端侧为后端，远离出口端侧为前端，同时定义M方向的左右两端和上下两端分别对应的左、右侧和上、下侧。
实施例一
如图2所示为卧式炉体用收集装置100。收集装置100用于碳纳米管膜或碳纳米管纤维的收集，其包括壳体、预调整机构和缠绕机构130。其中，预调整机构包括第一预调整子机构110和第二预调整子机构120，且用于调整多束碳纳米管聚集体。
第一调整子机构110靠近出口端设置，第二预调整子机构120设置于第一调整子机构110和缠绕机构130之间。第一轮体111和第二轮体112优选地设置于M方向的左右侧，也即第一轮体111和第二轮体112设置于碳纳米管聚集体的左右侧。
由于碳纳米管聚集体在多数情况下为多束，每一束碳纳米管聚集体被牵引方向和碳纳米管的轴向均不一致，很难实现多束碳纳米管聚集体的均匀收集，而碳纳米管材料的内部结构对各项性能均有重大影响，故而会影响碳纳米管材 料的整体性能。通过设置在左右侧的第一轮体111和第二轮体112，可将多束碳纳米管聚集体集成一束，以使聚集后的碳纳米管聚集体以一个完整的形状被收集，进而优化提高收集后的碳纳米管聚集材料的均匀性。同样地，通过调整第一轮体111和第二轮体112之间的转速，从而可改变第一轮体111和第二轮体112对碳纳米管聚集体所施加的正压力，以实现不同的集束和牵伸效果，以调整碳纳米管聚集体的取向，从而可调控碳纳米管材料的各项性能。此时，第一轮体111和第二轮体112之间的间距、转速以及其位置均可根据碳纳米管聚集体的产量和产出速率进行相应的调整，以到达最佳预调整效果。需要说明的是，在此情况下，沿第一方向设置的轮体可始终为2个，即仅为第一轮体111和第二轮体112。当然，沿第一方向设置的轮体的数量可为其他多个，优选地，可为匹配多束碳纳米管聚集体的数量。
第二调整子机构120包括第三轮体121，该第三轮体121设置在M方向的下侧，也即第三轮体121设置在碳纳米管聚集体的下侧。第三轮体121能够转动且环绕设有若干第一环形凸起140，第一环形凸起140用于整理碳纳米管聚集体的取向。
请参见图3，第三轮体121与碳纳米管聚集体接触面上设有若干第一环形凸起140，第一环形凸起140环绕于第三轮体121的轴向设置，第一环形凸起140的宽度不大于10μm，且相邻第一环形凸起140的间距不大于100μm。第一轮体111和第二轮体112能够转动且两者转动方向可相同或不同。优选地，第一轮体111和第二轮体112的转动方向相反，进一步优选地，两者可为相向转动或背向转动。
该第一环形凸起140的宽度不大于10μm，且相邻第一环形凸起140的间距不大于100μm。优选地，该第一环形凸起140的宽度为0.2～5μm，且相邻第一环形凸起140的间距为50～90μm。该第一环形凸起140的高度可为1～10mm。进一步地，该第一环形凸起140可与第三轮体121一体构成，也可为分别加工成型，可拆卸安装在第三轮体121上。该第一环形凸起140可通过激光蚀刻或化学蚀刻或印刷等方式加工制备而得。
由于第三轮体121转动时，带动相应的第一环形凸起140转动，第一环形 凸起140为若干间隔设置的凸起，其既可对碳纳米管聚集体进行沿切线方向的力，以帮助整理碳纳米管聚集体的内部结构沿切线方向排列。此外该第一环形凸起140还可分别对碳纳米管聚集体施加一定的正压力，通过调整第三轮体121的转速，从而使得第三轮体121对碳纳米管聚集体所施加的正压力不同，以实现对碳纳米管聚集体的牵伸，以调整碳纳米管聚集体的取向，从而可调控碳纳米管材料的各项性能。
请继续参见图2，在本实施方式中，第二预调整子机构120还至少包括能够转动的第四轮体122，第四轮体122和第三轮体121沿第二方向间隔错开设置且均能够对碳纳米管聚集体沿收集方向进行牵伸。该第二方向与第一方向不同，优选地，第二方向与第一方向为相互垂直。当然，第二方向和第一方向也可为其他情况。
进一步地，第四轮体122和第三轮体121设置在M方向的上下两侧或左右两侧，两者的设置位置可根据第一轮体111和第二轮体112的设置情况做相应的调整。由于增加了第四轮体122，通过调节第四轮体122和第三轮体121为不同的转速，可改变第三轮体121和第四轮体122对碳纳米管聚集体所施加的沿第二方向的正压力，以实现对碳纳米管聚集体的进一步牵伸，进一步调整碳纳米管聚集体的取向，从而实现碳纳米管材料的各项性能的可控调节。在本实施方式中，第三轮体121和第四轮体122的个数相同且均为1个，在其他实施方式中，第三轮体121和第四轮体122的个数可为2个或其他多个。如此，通过增加多个轮体对碳纳米管聚集体进行多种程度的牵伸，进一步调节碳纳米管聚集体内部的微观结构，改善碳纳米管聚集体的取向性。
进一步地，请参见图4，第四轮体环绕设有若干第二环形凸起150，第二环形凸起150用于整理碳纳米管聚集体的取向。具体的，第四轮体122上与碳纳米管聚集体接触面上可设有若干第二环形凸起150，第二环形凸起150环绕于第四轮体122的轴向设置。
第二环形凸起150的宽度不大于10μm，且相邻第二环形凸起150的间距不大于100μm。类似于第一环形凸起140，优选地，该第二环形凸起150的宽度为0.2～5μm，且相邻第二环形凸起150的间距为1～80μm。该第二环形凸起150的 高度可为1～10mm。进一步地，该第二环形凸起150可与对应的第四轮体122一体构成，也可为分别加工成型，可拆卸安装在对应的第四轮体122上。该第二环形凸起150可通过激光蚀刻或化学蚀刻或印刷等方式加工制备而得。
在一实施方式中，第一环形凸起140和第二环形凸起150可为对称分布设置，也可为错开设置。
由于第三轮体121和第四轮体122转动时，带动相应的第一环形凸起140和第二环形凸起150转动，环形凸起均为若干间隔设置的凸起，其既可对碳纳米管聚集体进行沿切线方向的力，以帮助整理碳纳米管聚集体的内部结构沿切线方向排列，优化取向调整效果。此外该第一环形凸起140和第二环形凸起150还可分别对碳纳米管聚集体的两侧施加一定的正压力，通过调整第三轮体121和第四轮体122为不同的转速，从而使得第三轮体121和第四轮体122对碳纳米管聚集体所施加的沿第一方向的正压力不同，以实现对碳纳米管聚集体的牵伸，以调整碳纳米管聚集体的取向，从而可调控碳纳米管材料的各项性能。
在一实施方式中，第一环形凸起140和第二环形凸起150上所对应的凸起宽度和间距可相同也可不同。当第一环形凸起140和第二环形凸起150上对应的凸起宽度和间距不同时，如此可调节各自凸起的分布密度，从而实现不同取向调整效果。
在一实施方式中，请参见图5所示，第一轮体111和/或第二轮体112上与碳纳米管聚集体的接触面的中部开设有能够容纳碳纳米管聚集体的环形限位槽160。
环形限位槽160的开槽跨度与需容纳的碳纳米管聚集体的尺寸相匹配。在本实施方式中，该环形限位槽160沿轴向的截面可为对称的三角形。在另一实施方式中，该环形限位槽160沿轴向的截面为对称的弧形槽。在其他实施方式中，环形限位槽160还可为其他形状的槽体。
通过增加该环形限位槽160，如此不仅可以用来固定和限位碳纳米管聚集体，以避免碳纳米管聚集体在受第一调整子机构110预压时发生上下移动；此外，还可有效的将碳纳米管聚集体聚集在环形限位槽160中，进一步保证均匀收集，提高收集后的碳纳米管聚集体的取向。
在一实施方式中，收集装置100还包括第一加热机构(未图示)，设置于壳体内并用于调节第一预调整子机构110和/或第二预调整子机构120与碳纳米管聚集体的接触面的温度。
在一实施方式中，第一加热机构包括加热电阻丝和控制器，加热电阻丝内置于第一预调整子机构110和/或第二预调整子机构120的端部或内部，控制器设置在壳体内且用于控制加热电阻丝的发热量。第一加热机构还可包括测量预调整机构上相应接触面温度的热电偶或测温仪。
在一实施方式中，第一加热机构的温度范围可设置为100～500℃。进一步的，第一加热机构的温度范围可为200～400℃。需要说明的是，收集装置100的壳体内优选为惰性环境。
通过增加第一加热机构，经过适当的加热可排出碳纳米管聚集体内部的气体，提高收集后的碳纳米管产品的致密性。此外，还可控制与碳纳米管聚集体的接触面的温度，从而有利于提高预调整机构对碳纳米管聚集体的内部结构的调整效果，提高碳纳米管的取向和均匀性，实现对收集碳纳米管材料的各项性能的调控。
在本实施方式中，缠绕机构130可为能够转动以收集碳纳米管聚集体的辊筒。由于碳纳米管聚集体中通常含有微量的铁元素，该辊筒可为带微磁性材质，如此可有利于对碳纳米管聚集体的吸附收集。
在一实施方式中，缠绕机构130可为能够沿轴向伸缩的转筒(未图示)。当收集的碳纳米管聚集体为碳纳米管纤维时，套筒可不需要移动位置；而当收集的碳纳米管聚集体为碳纳米管薄膜时，可移动转筒做沿一个方向运动或往复运动，如此可收集到一定面积的碳纳米管薄膜。该往复运动方向与转筒轴向方向不垂直，优选的，该往复运动方向与转筒轴向方向平行。当然，该往复运动方向与转筒轴向方向可呈现一定夹角，以实现碳纳米管薄膜的收集。设置的转筒能够沿轴向伸缩，如此可进一步改变收集的碳纳米管薄膜的面积，从而可控制所制备的碳纳米管薄膜的厚度，进而获得不同性能的碳纳米管薄膜材料。
在另一实施方式中，缠绕机构130可包括第一转轮、第二转轮和张紧于第一转轮和所述第二转轮之间的收集带(未图示)。第一转轮和第二转轮的轴向 与出口端的延伸线方向相垂直。在一实施方式中，第一转轮和第二转轮之间的间距能够调节。如此通过调节第一转轮和第二转轮之间的间距，从而调节所收集的碳纳米管聚集体薄膜的宽度方向尺寸，进而调节碳纳米管薄膜的面积。
在又一实施方式中，请参见图6所示，缠绕机构130可包括第一转轮131、第二转轮132和设置于第一转轮131和第二转轮132之间且能够朝向预调整机构方向转动的收集板133。该收集板133可为略带磁性和一定厚度的板件。在一实施方式中，第一转轮131和第二转轮132之间的间距能够调节。相应的，可设置收集板133为能够伸缩的板件，如此通过调节第一转轮131和第二转轮132之间的间距，从而调节所收集的碳纳米管聚集体薄膜的长度方向尺寸，进而调节碳纳米管薄膜的面积。
实施例二
如图7所示为立式炉体用收集装置100。收集装置100用于碳纳米管膜或碳纳米管纤维的收集，其包括与合成装置200的出口端连通的壳体以及设置于壳体内的预调整机构和缠绕机构130。预调整机构包括第一预调整子机构110和第二预调整子机构120，且用于调整一束碳纳米管聚集体的取向。
本实施例除了适用于立式炉体所生长的碳纳米管膜或碳纳米管纤维的收集外，还与实施例一的区别在于：第二调整子机构120靠近合成装置200的出口端设置，第一预调整子机构110设置于第二调整子机构120和缠绕机构130之间。
本实施例的其他内容可参见实施例一，在此不再赘述。
本发明还提供一种制备系统，用于碳纳米管膜材料或碳纳米管纤维材料的制备。下面结合附图详细介绍制备系统。
实施例三
请参见图8所示，为本发明的一实施方式的包含卧式炉体的制备系统。制备系统包括合成装置200和收集装置100。合成装置200，用于浮动催化合成碳纳米管聚集体。合成装置200包括具有至少一个生长管211的反应器210。收集装置100位于合成装置200的出口端侧，用于收集合成装置200所制备的碳纳米管聚集体。收集装置100与合成装置200的出口端连通，例如，收集装置100 可通过法兰(未图示)与合成装置200密封连接。
在本实施方式中，该反应器210可为多管卧式结构，生长管211的个数为两个。多个生长管211共同设置在反应器210内部，且共用一个反应炉体。如此，通过设置多管，即可大大提高碳纳米管的产量，又可保证每个生长管211中碳纳米管的质量，以提高整个碳纳米管材料的性能。当然，在其他实施方式中，生长管211的个数可为一个或其他多个。
该反应器210可为水平设置，当然也可为倾斜一定角度的多管结构。生长管211可为石英管、刚玉管或其他本领域常用材料制备而得。在一实施方式中，生长管211的管形为方形，如此可改变生长管211生成的碳纳米管聚集体的结构，进而调节收集的碳纳米管聚集体的均匀性。当然，在其他实施方式中，生长管211可为常用的中空圆管结构。
在本实施方式中，生长管211靠近收集装置100的端部为喇叭状。如此，由于浮动催化合成碳纳米管聚集体过程中，需要通入载气，生长管211内部会出现湍流，碳纳米管聚集体会向上飘，容易粘附在生长管211的内壁上，从而造成收集中断。通过将生长管211的末端设置成喇叭状，如此可减少碳纳米管聚集体粘附到生长管211的内壁几率，以提高碳纳米管聚集体收集的连续性。当然，在其他实施方式中，生长管211靠近收集装置100的端部可为圆筒状或其他常规形状。
制备系统还包括加料装置300，该加料装置300与合成装置200的入口端连通，用于提供反应原料。
进一步地，该加料装置300可包括至少一个注射机构310和至少一个加料管320，加料管320的一端与注射机构310连通，另一端与生长管211连通。该注射机构310可为能够调控注射速率的注射泵、液体喷射器和超声雾化注入机构中的一种。
在本实施方式中，加料管320和注射机构310的个数均与生长管211的个数相匹配，此时加料管320可采用串联或并排方式。如此可通过控制注射机构310来分别调控所制备不同内部结构的碳纳米管材料，从而调控碳纳米管材料的性能。
在一实施方式中，加料管320和注射机构310的个数可为一个，如此结构简单且便于操作。在另一实施方式中，加料管320可为其他多个，注射机构310可为一个，如此多个加料管320可共用一个注射机构310。当然，加料管320和注射机构310的个数还可为其他合理的数量。
需要说明的是，多个生长管211可都用来生长碳纳米管聚集体以制备纯的碳纳米管材料。此外，还可设置其中的一个或多个生长管211用来制备其他材料，从而制备含碳纳米管的复合材料以使该复合材料具备不同的性能，扩宽材料的应用领域。
在一实施方式中，请参见图9所示，合成装置200包括具有多个生长管211的反应器210，若干生长管211的排列方式可为环形分布。在其他实施方式中，若干生长管211的排列方式可为并排或矩阵方式分布。
进一步地，请继续参见图8所示，合成装置200还包括第二加热机构212，用于调节若干个生长管211中入口端的各区域的温度分布。在本实施方式中，第二加热机构212可为三个间隔设置的加热器，该加热器设置在反应器210的内壁，分别对生长管211的入口端的各区域温度进行调节，从而控制碳纳米管聚集体的生长。
收集装置100的具体内容可参见实施例一所述，在此不再赘述。
通过本实施例的制备系统可制备得到碳纳米管薄膜材料。制备步骤包括：首先在碳源中溶入催化剂和生长促进剂配制成反应液，反应液通过加料装置300和载气一起通入到反应器210中的生长管211中，发生催化裂解反应生成连续碳纳米管聚集体，将碳纳米管连续聚集体进行收集得到碳纳米管薄膜。由于碳纳米管薄膜的制备工艺较为常见，上述制备过程可为本领域常用的原料、配比和工艺条件，在此不再赘述。
采用本实施例的制备系统(含预调整机构)所制备得到的碳纳米管薄膜产品，将得到的产品标记为试样1。为了说明预调整机构所发挥的作用，将本实施例制备系统中的预调整机构去掉，其他机构保持不变，并以此作为对比制备系统(不含预调整机构)且按照制备试样1的工艺条件也制备碳纳米管材料薄膜产品，将得到的产品记为试样2。
图10和图11分别为试样1和试样2的SEM图。通过对比可知，相比于未经过预调整机构调整的碳纳米管材料薄膜(试样2)，经过预调整机构调整的碳纳米管材料薄膜(试样1)的取向性更好。
图12为试样1和试样2的拉伸应力-断裂伸长率图。通过对比可知，相比于未经过预调整机构调整的碳纳米管材料薄膜(试样2)，经过预调整机构调整的碳纳米管材料薄膜(试样1)的力学性能更佳。
实施例四
请参阅图13所示，为本发明的另一实施方式的保含立式炉体的制备系统。制备系统包括合成装置200和收集装置100。合成装置200，用于浮动催化合成碳纳米管聚集体。合成装置200包括具有至少一个生长管211的反应器210。收集装置100与合成装置200的出口端连通，用于收集合成装置200所制备的碳纳米管聚集体。具体地，收集装置100可通过法兰与合成装置200密封连接。
在本实施方式中，反应器210为单管立式结构。在其他实施方式中，该反应器210可为多管立式结构。该反应器210可为垂直设置，当然也可为倾斜一定角度。
收集装置100的其他具体内容可参见实施例二所述，在此不再赘述。
本实施例的其他内容可参见实施例三所述，在此不再赘述。
以上所述实施例的各技术特征可以进行任意的组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。

Claims (15)

  1. 一种收集装置，用于碳纳米管膜或碳纳米管纤维的收集，其特征在于，包括：
    预调整机构，用于调整至少一束碳纳米管聚集体的取向，所述预调整机构包括第一预调整子机构和第二预调整子机构；所述第一预调整子机构至少包括沿第一方向设置且能够转动的第一轮体和第二轮体，所述第一轮体和所述第二轮体用于对碳纳米管聚集体的两侧进行预压；所述第二预调整子机构至少包括用于对碳纳米管聚集体进行牵伸的第三轮体；
    缠绕机构，用于将从预调整机构中引出的碳纳米管聚集体进行缠绕收集。
  2. 根据权利要求1所述的收集装置，其特征在于，所述第三轮体能够转动且环绕设有若干第一环形凸起，所述第一环形凸起用于整理碳纳米管聚集体的取向。
  3. 根据权利要求2所述的收集装置，其特征在于，所述第一环形凸起的宽度不大于10μm，且相邻所述第一环形凸起的间距不大于100μm。
  4. 根据权利要求1所述的收集装置，其特征在于，所述收集装置还包括：
    第一加热机构，用于调节所述第一预调整子机构和/或所述第二预调整子机构与碳纳米管聚集体的接触面的温度。
  5. 根据权利要求1所述的收集装置，其特征在于，所述第一轮体和/或所述第二轮体上与碳纳米管聚集体的接触面上开设有能够容纳碳纳米管聚集体的环形限位槽。
  6. 根据权利要求1所述的收集装置，其特征在于，所述第二预调整子机构还包括第四轮体，所述第四轮体和所述第三轮体沿第二方向间隔错开设置且均能够对碳纳米管聚集体沿收集方向进行牵伸。
  7. 根据权利要求6所述的收集装置，其特征在于，所述第四轮体能够转动且环绕设有若干第二环形凸起，所述第二环形凸起用于整理碳纳米管聚集体的取向。
  8. 根据权利要求6所述的收集装置，其特征在于，所述第一轮体和所述第二轮体为相向转动或背向转动，所述第三轮体和所述第四轮体的转速不等。
  9. 根据权利要求1-8任一所述的收集装置，其特征在于，所述缠绕机构包括能够沿轴向伸缩的转筒，所述转筒能够做往复运动且所述往复运动方向与所述转筒的轴向方向不垂直。
  10. 根据权利要求1-8任一所述的收集装置，其特征在于，所述缠绕机构包括第一转轮、第二转轮和张紧于所述第一转轮和所述第二转轮之间的收集带；或
    所述缠绕机构包括第一转轮、第二转轮和设置于所述第一转轮和所述第二转轮之间且能够朝所述预调整机构方向转动的收集板。
  11. 一种制备系统，用于碳纳米管膜材料或碳纳米管纤维材料的制备，其特征在于，包括：
    合成装置，用于浮动催化合成碳纳米管聚集体，其包括具有至少一个生长管的反应器；
    收集装置，为权利要求1-10任一所述的收集装置，所述收集装置位于所述合成装置的出口端侧，用于收集所述合成装置所制备的碳纳米管聚集体。
  12. 根据权利要求11所述的制备系统，其特征在于，所述生长管靠近所述收集装置的端部为喇叭状或圆筒状。
  13. 根据权利要求11或12所述的制备系统，其特征在于，所述制备系统还包括：
    加料装置，用于提供反应原料且与所述合成装置的入口端连通，所述加料装置包括至少一个注射机构和至少一个加料管，所述加料管的一端与所述注射机构连通，另一端与所述生长管连通。
  14. 根据权利要求13所述的制备系统，其特征在于，所述合成装置包括具有多个生长管的反应器，若干所述生长管的排列方式为环形分布或矩阵分布。
  15. 根据权利要求14所述的制备系统，其特征在于，所述合成装置还包括第二加热机构，用于调节若干个生长管中入口端的各区域的温度分布。
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