CN109440465B - A method for improving mechanical properties of carbon nanotube fibers by stretching impregnated organic matter - Google Patents
A method for improving mechanical properties of carbon nanotube fibers by stretching impregnated organic matter Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 122
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 82
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 82
- 239000005416 organic matter Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 230000008961 swelling Effects 0.000 claims abstract description 14
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 21
- 238000007598 dipping method Methods 0.000 claims description 12
- 230000009471 action Effects 0.000 claims description 2
- 230000008595 infiltration Effects 0.000 claims description 2
- 238000001764 infiltration Methods 0.000 claims description 2
- 238000003763 carbonization Methods 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 claims 1
- 238000002791 soaking Methods 0.000 abstract description 12
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 24
- 230000004048 modification Effects 0.000 description 8
- 238000012986 modification Methods 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/31—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated nitriles
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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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Inorganic Fibers (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
Abstract
The invention discloses a method for preparing carbon nano tube fiber by stretching and soakingA method for improving mechanical performance of impregnated organic matter includes such steps as putting the carbon nanotubes immersed in organic solution in a sealed container, filling CO in the container2The inner space of the container is in supercritical CO2And (3) after swelling reaction, slowly releasing pressure to obtain the modified carbon nanotube fiber, and selectively performing high-temperature treatment on the modified carbon nanotube fiber according to needs to pre-oxidize and carbonize organic matters entering the fiber to form the carbon nanotube fiber with a complete carbon structure. The invention is in supercritical CO2Soaking the primary carbon nanotube fiber in a stretched state with organic matter to modify supercritical CO2The organic solution can be effectively carried into the surface and the interior of the fiber, and the tensile modulus and the tensile strength of the carbon nanotube fiber are effectively improved. The method has the advantages of economy, environmental protection, controllable reaction, short reaction time, simple operation, suitability for industrial production and the like.
Description
Technical Field
The invention relates to a carbon nano tube fiber in supercritical CO2A method for improving mechanical property by stretching and dipping organic matter belongs to the technical field of fiber modification.
Background
The carbon nanotube fiber is a macroscopic form obtained by assembling a large number of carbon nanotubes, the tensile strength of the carbon nanotube fiber can stably reach more than 1.0GPa, but compared with the carbon nanotubes, the carbon nanotube fiber does not exert the mechanical advantages of the carbon nanotubes, and the carbon nanotube fiber is mainly because the Van der Waals force ratio among carbon tubes forming the fiber is weaker, a large number of gaps exist among carbon nanotube bundles, the contact area is small, the formed loose and mutually easily-sliding structures are formed, a large number of cavities exist in the fiber, the stacking density of the carbon tubes is not high, and the exertion of the excellent performance of the carbon nanotube body under the condition of macroscopic fiber is greatly limited. How to overcome the relative slippage between the carbon tubes is the key to prepare the high-performance carbon nanotube fiber by introducing a stable connecting part between the carbon tubes.
In the aspect of mechanical reinforcement of carbon nanotube fibers, some work has been focused on mechanical reinforcement of carbon nanotube fibers in addition to the conventional twisting, drawing and other processes, for example, chinese patent publication discloses an application with the following numbers: 201210513599.X, with the name: the method for electrically reinforcing carbon nano tube fiber adopts the main technical scheme that thermosetting resin precursor diluent is fully soaked in the carbon nano tube fiber, current is conducted in the soaked carbon nano tube fiber, so that thermosetting resin is quickly crosslinked and cured, and the reinforced fiber is obtained.
The infiltration of nascent Carbon Nanotube fibers into PAN is difficult because PAN forms a shell on Carbon Nanotube fibers, and Carbon Nanotube fibers have a loose structure but macromolecules cannot easily enter the interior, and studies have been made (Cui Y, Zhang M. cross-links in Carbon Nanotube Assembly by Using polyacrylic acid as a precarsor [ J ]. Acs applied Mater Interfaces,2013,5(16): 8173) 8178.) to show that 25 μm fibers can only infiltrate 2 μm into the interior of the fibers. Therefore, the method for effectively realizing the introduction of organic matters into the reinforcing carbon nano tube fiber inside the nascent carbon nano tube fiber without introducing other chemical components provides possibility for preparing the high-performance carbon nano tube fiber.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the existing carbon nano tube has the problem of damaging other properties while improving certain mechanical properties. .
In order to solve the above problems, the present invention provides a method for improving mechanical properties of carbon nanotube fibers by stretching and impregnating organic matter, characterized in that carbon nanotube fibers impregnated with an organic matter solution are placed in a closed container, and CO is charged into the container2The inner space of the container is in supercritical CO2State through swellingAfter the reaction, slowly releasing pressure to obtain the modified carbon nano tube fiber, and selectively performing high-temperature treatment on the modified carbon nano tube fiber according to the requirement to pre-oxidize and carbonize organic matters entering the fiber to form the carbon nano tube fiber with a complete carbon structure.
Preferably, the organic matter capable of producing all-carbon substances.
More preferably, the organic substance is polyacrylonitrile.
Preferably, the concentration of the organic matter solution in the carbon nanotube fiber is 0.25-1 times of the critical overlapping concentration of the organic matter solution; the soaking times of the carbon nano tube fiber in the organic solution are 1 to 4 times.
Preferably, the carbon nanotube fiber is a nascent fiber which is not subjected to stretching treatment, and the tension of the nascent fiber is 1-20 cN.
Preferably, the container is filled with CO at the temperature of 100-200 DEG C2Introduction of CO2Previously, the air in the container was removed.
Preferably, the swelling reaction specifically means in supercritical CO2And (3) under the action of the gas, soaking the fibers in the gas form within 5-60 min from the beginning of the reaction to generate a swelling reaction.
Preferably, the slow pressure relief means that the air outlet valve is opened slowly, so that the pressure in the container is reduced to normal pressure within 5-10 min.
Preferably, the temperature of the high-temperature treatment is 180-280 ℃.
The invention also provides the carbon nano tube fiber prepared by the method for improving the mechanical property of the carbon nano tube fiber by stretching and dipping the organic matter.
The invention is in supercritical CO2Soaking the primary carbon nanotube fiber in a stretched state with organic matter to modify supercritical CO2The organic solution can be effectively carried into the surface and the interior of the fiber, so that the tensile modulus of the carbon nanotube fiber is effectively improved by 30-108 percent, and the tensile strength is improved by 4-330 percent; the preoxidation leads the organic matters on the surface and inside of the fiber to be further cyclized and achieves the purpose of densification of the fiber so as to improve the performance. Since the organic matter enters the voids inside the carbon nanotube fibers,the defects of the fiber are filled, meanwhile, the existence of tension ensures that the fiber is in a stretching state, the carbon nano tube fiber is stretched, the organic molecular chain orientation degree is ensured, and simultaneously, chemical cyclization reaction is carried out, so that macromolecules are crosslinked between the carbon nano tubes, the improvement of fiber strength and modulus is facilitated, and several influences are combined together, so that the carbon nano tube fiber is more compact, and the performance of the carbon nano tubes is greatly improved. The method has the advantages of economy, environmental protection, controllable reaction, short reaction time, simple operation, suitability for industrial production and the like.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below.
Example 1
A method for improving mechanical property of carbon nanotube fiber by stretching and dipping organic matter comprises the following steps:
(1) soaking the surface of the carbon nano tube fiber with 0.5 times of PAN/DMSO solution with critical crossover viscosity C;
(2) maintaining the carbon nanotube fibers at a tension of 4cN in a closed container;
(3) at 150 deg.C, air is removed, and CO is charged into the container2The pressure in the container reaches 10Mpa to reach supercritical CO2In the state, after the swelling reaction is carried out for 1h, the pressure is slowly released;
(4) repeating the steps (1) - (3) for 4 times to obtain the modified carbon nanotube fiber;
(5) the strength and modulus of the modified carbon nanotube fiber obtained by the instron test are both increased by 110% and 100% compared with those of the fiber before modification, and the PAN deposited on the surface is observed to be uniform and does not form a thick shell layer through SEM.
Example 2
A method for improving mechanical property of carbon nanotube fiber by stretching and dipping organic matter comprises the following steps:
(1) soaking the surface of the carbon nano tube fiber with 0.5 times of PAN/DMSO solution with critical crossover viscosity C;
(2) in the closed container, the carbon nano tube fiber is kept at a tension of 1.2 cN;
(3) at the temperature of 100 ℃, the temperature of the mixture is controlled,removing air and filling CO into the container2The pressure in the container reaches 8Mpa to supercritical CO2In the state, after the swelling reaction is carried out for 1h, the pressure is slowly released;
(4) repeating the steps (1) - (3) for 4 times to obtain the modified carbon nanotube fiber;
(5) the strength and modulus of the modified carbon nanotube fiber obtained by the instron test are both increased by 35% and 108% compared with those of the fiber before modification, and the PAN deposited on the surface is observed to be uniform and does not form a thick shell layer through SEM.
Example 3
A method for improving mechanical property of carbon nanotube fiber by stretching and dipping organic matter comprises the following steps:
(1) soaking the surface of the carbon nano tube fiber with 0.5 times of PAN/DMSO solution with critical crossover viscosity C;
(2) in the closed container, the carbon nano tube fiber is kept at the tension of 8.4 cN;
(3) at 200 deg.C, air is removed, and CO is charged into the container2The pressure in the container reaches 8Mpa to supercritical CO2In the state, after the swelling reaction is carried out for 1h, the pressure is slowly released;
(4) repeating the steps (1) - (3) for 4 times to obtain the modified carbon nanotube fiber;
(5) the strength and modulus of the modified carbon nanotube fiber obtained by the instron test are both increased by 4% and 72% compared with those of the fiber before modification, and the PAN deposited on the surface is observed to be uniform and does not form a thick shell layer through SEM.
Example 4
A method for improving mechanical property of carbon nanotube fiber by stretching and dipping organic matter comprises the following steps:
(1) soaking the surface of the carbon nano tube fiber with 0.5 times of PAN/DMSO solution with critical crossover viscosity C;
(2) in the closed container, the carbon nanotube fiber is kept at 4cN tension;
(3) at 100 deg.C, air is removed, and CO is charged into the container2The pressure in the container reaches 10Mpa to reach supercritical CO2In the state, after the swelling reaction is carried out for 1h, the pressure is slowly released;
(4) repeating the steps (1) - (3) for 4 times to obtain the modified carbon nanotube fiber;
(5) the strength and modulus of the modified carbon nanotube fiber obtained by the instron test are both increased by 73 percent and 42 percent compared with the strength and modulus of the fiber before modification, and the PAN deposited on the surface is observed to be uniform and does not form a thick shell layer by SEM.
Example 5
A method for improving mechanical property of carbon nanotube fiber by stretching and dipping organic matter comprises the following steps:
(1) soaking the surface of the carbon nano tube fiber with 0.5 times of PAN/DMSO solution with critical crossover viscosity C;
(2) in the closed container, the carbon nanotube fiber is kept at 4cN tension;
(3) at 200 deg.C, air is removed, and CO is charged into the container2The pressure in the container reaches 12Mpa to reach supercritical CO2In the state, after the swelling reaction is carried out for 1h, the pressure is slowly released;
(4) repeating the steps (1) - (3) for 4 times to obtain the modified carbon nanotube fiber;
(5) the strength and modulus of the modified carbon nanotube fiber obtained by the instron test are both increased by 30% and 108% compared with those of the fiber before modification, and the PAN deposited on the surface is observed to be uniform and does not form a thick shell layer through SEM.
Example 6
A method for improving mechanical property of carbon nanotube fiber by stretching and dipping organic matter comprises the following steps:
(1) soaking the surface of the carbon nano tube fiber with 0.5 times of PAN/DMSO solution with critical crossover viscosity C;
(2) in the closed container, the carbon nanotube fiber is kept at 4cN tension;
(3) at 150 deg.C, air is removed, and CO is charged into the container2The pressure in the container reaches 10Mpa to reach supercritical CO2In the state, after swelling reaction for 20min, slowly releasing pressure;
(4) repeating the steps (1) - (3) for 4 times to obtain the modified carbon nanotube fiber;
(5) the strength and modulus of the modified carbon nanotube fiber obtained by the instron test are both increased by 70% compared with those of the fiber before modification, the modulus is increased by 200%, and the PAN deposited on the surface is observed to be uniform through SEM and does not form a thick shell layer.
Example 7
A method for improving mechanical property of carbon nanotube fiber by stretching and dipping organic matter comprises the following steps:
(1) soaking the surface of the carbon nano tube fiber with 1 time of PAN/DMSO solution with critical overlapping viscosity C;
(2) in the closed container, the carbon nanotube fiber is kept at 4cN tension;
(3) at 150 deg.C, air is removed, and CO is charged into the container2The pressure in the container reaches 10Mpa to reach supercritical CO2In the state, after the swelling reaction is carried out for 1h, the pressure is slowly released;
(4) the strength and modulus of the modified carbon nanotube fiber obtained by the instron test are both increased by 93% and 125% compared with those of the fiber before modification, and the PAN deposited on the surface is observed to be uniform but form a thick PAN shell layer through SEM observation.
Example 8
A method for improving mechanical property of carbon nanotube fiber by stretching and dipping organic matter comprises the following steps:
(1) soaking the surface of the carbon nano tube fiber with 0.5 times of PAN/DMSO solution with critical crossover viscosity C;
(2) in the closed container, the carbon nanotube fiber is kept at 4cN tension;
(3) at 150 deg.C, air is removed, and CO is charged into the container2The pressure in the container reaches 10Mpa to reach supercritical CO2In the state, after the swelling reaction is carried out for 1h, the pressure is slowly released;
(4) repeating the steps (1) - (3) for 4 times, dividing the fiber into 5 temperature sections at the pre-oxidation temperature of 180-280 ℃, and allowing each section to stay for 10min to obtain the pre-oxidized modified carbon nanotube fiber;
(5) the strength of the modified carbon nanotube fiber after pre-oxidation is reduced by 30% compared with the strength before pre-oxidation, but the modulus is increased by 90%, the overall strength is improved by 32% compared with the strength before non-treatment, and the modulus is improved by 328% according to the instron test. No surface deposited PAN was observed by SEM.
Claims (6)
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| CN107055513A (en) * | 2010-06-22 | 2017-08-18 | 设计纳米管有限责任公司 | Modified carbon nano-tube, its production method and thus obtained product |
| KR101408277B1 (en) * | 2012-12-04 | 2014-06-16 | 숭실대학교산학협력단 | Method for preparing carbon nanotube fiber with enhanced spinning using surfactant and carbon nanotube fiber prepared by the same |
| CN107740282A (en) * | 2017-10-20 | 2018-02-27 | 东华大学 | A kind of PAN carbon fibre precursors processing method |
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