CN103979528B - One step prepares the method for super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge - Google Patents
One step prepares the method for super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge Download PDFInfo
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Abstract
One step prepares the method for super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge, belongs to carbon nano-composite material Synthesis and application technical field.Described method steps is as follows: one, the preparation of carbon nanotube sponge; The preparation of two, super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge.The chemical gaseous phase depositing process being carbon source with ferrocene/dichlorobenzene used in the present invention can make hyperelastic carbon nanotube/amorphous carbon composite all-carbon sponge only prepare through the intensification temperature-fall period of primary first-order equation stove, and be replaced with gas phase carbon source (as acetylene) again carry out complicated processes prepared by carbon nanotube/amorphous carbon composite all-carbon sponge without the need to taking out from Reaktionsofen after obtained carbon nanotube sponge, thus substantially increase preparation efficiency, be beneficial to actual production.The method that this step prepares composite carbon nanometer tube sponge is skillfully constructed, simple to operate.
Description
Technical field
The invention belongs to carbon nano-composite material Synthesis and application technical field, relate to a kind of preparation method of carbon nano tube compound material, particularly an a kind of step prepares the method for super-elasticity amorphous carbon/carbon nanotube composite all-carbon sponge.
Background technology
Carbon nanotube is by the curling hollow structure of graphite synusia, because it has unique nanostructure and excellent performance, receives in recent years and studies widely and pay close attention to.This material is brought in macrocosm from microcosm with synthesis by the controlled synthesis of carbon nano-tube macroscopic body just, and carbon nanotube field in actual applications is greatly expanded.At present, the Main Morphology of carbon nano-tube macroscopic body has carbon nanotube long filament, carbon nano-tube film, carbon nano pipe array and carbon nanotube sponge.Wherein, three-dimensional carbon nano-tube macroscopic body has wider range of application.
The carbon nanotube sponge that the people such as osmanthus Xu Chun utilize chemical Vapor deposition process to synthesize is wound around by carbon nanotube is crisscross the aerogel piled up and form three-dimensional block.Carbon nanotube sponge has high specific surface area and porosity, lower density, good thermodynamic property and electroconductibility, has good application prospect in fields such as reinforced composite material, greasy dirt absorption, microelectronic devices.The people such as KyuHunKim can obtain having hyperelastic three-dimensional carbon nano material by covering Graphene coating on Single Walled Carbon Nanotube aerogel, and this will make carbon nanotube aerogel be able to widespread use in various fields such as electrode materials, artificial-muscle and other physical constructions.But this hyperelastic carbon nano tube/graphene aerogel is completed by the step such as polymer penetration, pyrolysis processing, reaction is complicated and consuming time longer, is very unfavorable for actual production, and its hyperelastic range of strain less (being only 2%).The people such as Zhao Wenqi can be prepared equally by chemical Vapor deposition process has hyperelastic carbon nanotube aerogel, and it has extraordinary superelastic properties, and when compressive strain is 50%, the loop of stress-strain(ed) curve is still very little.But its preparation method is first synthesizing carbon nanotubes sponge in the Reaktionsofen of ferrocene/dichlorobenzene phase carbon source, question response stove takes out product after being down to room temperature, be put in another again to be prepared hyperelastic carbon nanotube aerogel in the gas phases such as the acetylene Reaktionsofen that is carbon source, though this method is easy and simple to handle relative to chemical synthesis, but very long (whole process reaches tens of hours) consuming time, and then cost is higher for suitability for industrialized production.
Can directly synthesize and have hyperelastic carbon nanotube aerogel, becoming field of carbon nanotubes needs one of difficult problem of capturing.Therefore, develop preparation technology and be simply beneficial to actual production and the preparation method with hyperelastic full carbon aerogels remains a challenge.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of method that a step preparation has hyperelastic carbon nanotube/amorphous carbon composite all-carbon sponge, the method further simplify the step of preparation hyperelastic carbon nanotube/amorphous carbon composite all-carbon sponge, improves production efficiency.
The object of the invention is to be achieved through the following technical solutions:
An a kind of step preparation has the method for hyperelastic carbon nanotube/amorphous carbon composite all-carbon sponge, with ferrocene/dichlorobenzene for phase carbon source, utilize the method for chemical vapour deposition, a step preparation can have hyperelastic carbon nanotube/amorphous carbon composite all-carbon sponge, concrete preparation process is as follows:
One, the preparation of carbon nanotube sponge: the quartz substrate of cleaning is positioned over the silica tube middle part of Reaktionsofen and sealed silica envelope, Reaktionsofen heating schedule is set, logical argon gas is to get rid of residual air in silica tube, Reaktionsofen injects ferrocene/dichlorobenzene carbon source solution reaction 0.5 ~ 4h when being warming up to 820 ~ 940 DEG C under hydrogen/argon gas mixed atmosphere, turn off the injection of hydrogen and ferrocene/dichlorobenzene carbon source solution after reaction, lower the temperature with stove under argon shield;
The preparation of two, super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge: when being down to 600 ~ 750 DEG C; keep temperature and again pass into ferrocene/dichlorobenzene carbon source solution, hydrogen; after 5 ~ 60min; obtain carbon nanotube/amorphous carbon composite all-carbon sponge; turn off carbon source and cool to room temperature with the furnace under argon shield, collecting product.
In described step one, be 600 ~ 1000mL/min for emptying reaction room air passes into argon flow amount; During reaction, hydrogen flowing quantity is 100 ~ 500mL/min, and argon flow amount is 1600 ~ 2400mL/min, passes into simultaneously; The concentration of ferrocene/dichlorobenzene carbon source solution is 20 ~ 100mg/mL, and speed of feed is 0.1 ~ 0.3mL/min; During cooling, argon flow amount is 600 ~ 1000mL/min.
In described step 2, the concentration of ferrocene/dichlorobenzene carbon source solution is 20 ~ 100mg/mL, and ferrocene/dichlorobenzene carbon source solution speed of feed is 0.1 ~ 0.3mL/min, and argon flow amount is 1600 ~ 2400mL/min, and hydrogen flowing quantity is 100 ~ 500mL/min; During cooling, argon flow amount is 600 ~ 1000mL/min.
Compared with prior art, the invention has the beneficial effects as follows:
1, the chemical gaseous phase depositing process being carbon source with ferrocene/dichlorobenzene used in the present invention can make hyperelastic carbon nanotube/amorphous carbon composite all-carbon sponge only prepare through the intensification temperature-fall period of primary first-order equation stove, and be replaced with gas phase carbon source (as acetylene) again carry out complicated processes prepared by carbon nanotube/amorphous carbon composite all-carbon sponge without the need to taking out from Reaktionsofen after obtained carbon nanotube sponge, thus substantially increase preparation efficiency, be beneficial to actual production.
2, the super-elasticity carbon nanotube composite sponge prepared by the present invention still keeps vesicular structure, it is made up of carbon nanotube and the uniform amorphous carbon of thickness be coated on outside carbon nanotube, this composite carbon nanometer tube sponge has excellent mechanical property and super-elasticity, has good application prospect in the field such as energy storage, physical construction.
3, the method that this step prepares composite carbon nanometer tube sponge is skillfully constructed, simple to operate.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of the carbon nanotube/amorphous carbon composite all-carbon sponge obtained in embodiment 2;
Fig. 2 is the transmission electron microscope photo of the carbon nanotube/amorphous carbon composite all-carbon sponge obtained in embodiment 2;
Fig. 3 is the compression cycle curve of the carbon nanotube sponge obtained in embodiment 2;
Fig. 4 is the compression cycle curve of the carbon nanotube/amorphous carbon composite all-carbon sponge obtained in embodiment 2.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is further described; but be not limited thereto; everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
embodiment 1
A kind of preparation method with super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge provided in the present embodiment, realizes in the steps below:
One, the preparation of carbon nanotube sponge: the middle part, the quartz reaction chamber quartz substrate of cleaning being positioned over High Temperature Furnaces Heating Apparatus, then seals quartz reaction chamber, regulates heating schedule and starts to heat up; The argon gas air got rid of in reaction chamber passing into 800mL/min in temperature-rise period keeps atmosphere to stablize; After temperature rises to 820 ~ 940 DEG C, adjustment argon flow amount is 2000mL/min, and pass into the hydrogen of 100 ~ 500mL/min, open precise injection pump, in reaction chamber, implantation concentration is the ferrocene/dichlorobenzene carbon source reaction soln of 20 ~ 100mg/mL, speed of feed is 0.1 ~ 0.3mL/min, and the reaction times is 0.5 ~ 4h.Subsequently, feed-disabling ferrocene/dichlorobenzene carbon source reaction soln also turns off hydrogen, and Reaktionsofen is cooled under the argon gas atmosphere that airshed is 800mL/min is protected;
The preparation of two, super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge: when temperature is down to 600 ~ 750 DEG C, arranging Reaktionsofen temperature control program makes it keep 20min at this temperature, argon flow amount is adjusted to 2000mL/min simultaneously, hydrogen flowing quantity is 100 ~ 500mL/min, and is the ferrocene/dichlorobenzene carbon source reaction soln of 20 ~ 100mg/mL with the speed feeding concentration of 0.1 ~ 0.3mL/min.After reaction 20min, feed-disabling ferrocene/dichlorobenzene carbon source reaction soln turn off hydrogen again, regulates argon flow amount to 800mL/min.After cooling to room temperature with the furnace, take out quartz substrate and collect the carbon nanotube/amorphous carbon composite all-carbon sponge prepared in quartz substrate.
What the present embodiment obtained have super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge has 3 D stereo reticulated structure, still there is extraordinary super-elasticity, when strain is 10 ~ 50%, stress-strain(ed) curve loop is very little, still can restore to the original state completely when being compressed to 80% strain.
embodiment 2
The quartz substrate of cleaning is positioned over the middle part, quartz reaction chamber of High Temperature Furnaces Heating Apparatus, then seals quartz reaction chamber, regulate heating schedule and start to heat up; The argon gas air got rid of in reaction chamber passing into 800mL/min in temperature-rise period keeps atmosphere to stablize; After temperature rises to 880 DEG C, adjustment argon flow amount is 2000mL/min, and passes into the hydrogen of 300mL/min, open precise injection pump, in reaction chamber, implantation concentration is the ferrocene/dichlorobenzene carbon source reaction soln of 60mg/mL, and speed of feed is 0.1mL/min, and the reaction times is 2h.Subsequently, feed-disabling ferrocene/dichlorobenzene carbon source reaction soln also turns off hydrogen, and Reaktionsofen is cooled under the argon gas atmosphere that airshed is 800mL/min is protected.When temperature is down to 600 ~ 750 DEG C, arranging Reaktionsofen temperature control program makes it keep 30min at this temperature, argon flow amount is adjusted to 2000mL/min simultaneously, hydrogen flowing quantity is 300mL/min, and is the ferrocene/dichlorobenzene carbon source reaction soln of 20 ~ 100mg/mL with the speed feeding concentration of 0.1 ~ 0.3mL/min.After reaction 30min, feed-disabling ferrocene/dichlorobenzene carbon source reaction soln turn off hydrogen again, regulates argon flow amount to 800mL/min.After cooling to room temperature with the furnace, take out quartz substrate and collect the carbon nanotube/amorphous carbon composite all-carbon sponge prepared in quartz substrate.Fig. 1 and Fig. 2 is respectively scanning electron microscope and the transmission electron microscope photo of carbon nanotube/amorphous carbon composite all-carbon sponge.Can find out that from Fig. 1 and Fig. 2 carbon nanotube/amorphous carbon composite all-carbon sponge is by the stacking porous material be entwined of the carbon nanotube of the coated amorphous carbon of outer wall.On microcosmic, the uniform amorphous carbon of carbon nanotube outer cladding a layer thickness, form microcosmic core shell structure, amorphous carbon thickness is at about 20nm.Fig. 3 is the compression cycle curve of carbon nanotube sponge, and Fig. 4 is the compression cycle curve of this carbon nanotube/amorphous carbon composite all-carbon sponge.As can be seen from Fig. 3 and Fig. 4, under identical compressive strain, maximum stress value and the Young's modulus of composite sponge obviously increase, and stress-strain(ed) curve loop line obviously becomes narrow, namely has super-elasticity.
embodiment 3
The quartz substrate of cleaning is positioned over the middle part, quartz reaction chamber of High Temperature Furnaces Heating Apparatus, then seals quartz reaction chamber, regulate heating schedule and start to heat up; The argon gas air got rid of in reaction chamber passing into 800mL/min in temperature-rise period keeps atmosphere to stablize; After temperature rises to 880 DEG C, adjustment argon flow amount is 2000mL/min, and passes into the hydrogen of 300mL/min, open precise injection pump, in reaction chamber, implantation concentration is the ferrocene/dichlorobenzene carbon source reaction soln of 60mg/mL, and speed of feed is 0.1mL/min, and the reaction times is 2h.Subsequently, feed-disabling ferrocene/dichlorobenzene carbon source reaction soln also turns off hydrogen, and Reaktionsofen is cooled under the argon gas atmosphere that airshed is 800mL/min is protected.When temperature is down to 600 ~ 750 DEG C, arranging Reaktionsofen temperature control program makes it keep 60min at this temperature, argon flow amount is adjusted to 2000mL/min simultaneously, hydrogen flowing quantity is 300mL/min, and is the ferrocene/dichlorobenzene carbon source reaction soln of 20 ~ 100mg/mL with the speed feeding concentration of 0.1 ~ 0.3mL/min.After reaction 60min, feed-disabling ferrocene/dichlorobenzene carbon source reaction soln turn off hydrogen again, regulates argon flow amount to 800mL/min.After cooling to room temperature with the furnace, take out quartz substrate and collect the carbon nanotube/amorphous carbon composite all-carbon sponge prepared in quartz substrate.By sem observation, coated amorphous carbon layer thickness is about 35nm.
embodiment 4
The quartz substrate of cleaning is positioned over the middle part, quartz reaction chamber of High Temperature Furnaces Heating Apparatus, then seals quartz reaction chamber, regulate heating schedule and start to heat up; The argon gas air got rid of in reaction chamber passing into 800mL/min in temperature-rise period keeps atmosphere to stablize; After temperature rises to 880 DEG C, adjustment argon flow amount is 2000mL/min, and passes into the hydrogen of 300mL/min, open precise injection pump, in reaction chamber, implantation concentration is the ferrocene/dichlorobenzene carbon source reaction soln of 60mg/mL, and speed of feed is 0.1mL/min, and the reaction times is 2h.Subsequently, feed-disabling ferrocene/dichlorobenzene carbon source reaction soln also turns off hydrogen, and Reaktionsofen is cooled under the argon gas atmosphere that airshed is 800mL/min is protected.When temperature is down to 600 ~ 750 DEG C, arranging Reaktionsofen temperature control program makes it keep 45min at this temperature, argon flow amount is adjusted to 2000mL/min simultaneously, hydrogen flowing quantity is 300mL/min, and is the ferrocene/dichlorobenzene carbon source reaction soln of 20 ~ 100mg/mL with the speed feeding concentration of 0.1 ~ 0.3mL/min.After reaction 45min, feed-disabling ferrocene/dichlorobenzene carbon source reaction soln turn off hydrogen again, regulates argon flow amount to 800mL/min.After cooling to room temperature with the furnace, take out quartz substrate and collect the carbon nanotube/amorphous carbon composite all-carbon sponge prepared in quartz substrate.By sem observation, coated amorphous carbon layer thickness is about 28nm.
embodiment 5
The quartz substrate of cleaning is positioned over the middle part, quartz reaction chamber of High Temperature Furnaces Heating Apparatus, then seals quartz reaction chamber, regulate heating schedule and start to heat up; The argon gas air got rid of in reaction chamber passing into 800mL/min in temperature-rise period keeps atmosphere to stablize; After temperature rises to 880 DEG C, adjustment argon flow amount is 2000mL/min, and passes into the hydrogen of 300mL/min, open precise injection pump, in reaction chamber, implantation concentration is the ferrocene/dichlorobenzene carbon source reaction soln of 60mg/mL, and speed of feed is 0.1mL/min, and the reaction times is 2h.Subsequently, feed-disabling ferrocene/dichlorobenzene carbon source reaction soln also turns off hydrogen, and Reaktionsofen is cooled under the argon gas atmosphere that airshed is 800mL/min is protected.When temperature is down to 600 ~ 750 DEG C, arranging Reaktionsofen temperature control program makes it keep 20min at this temperature, argon flow amount is adjusted to 2000mL/min simultaneously, hydrogen flowing quantity is 300mL/min, and is the ferrocene/dichlorobenzene carbon source reaction soln of 20 ~ 100mg/mL with the speed feeding concentration of 0.1 ~ 0.3mL/min.After reaction 20min, feed-disabling ferrocene/dichlorobenzene carbon source reaction soln turn off hydrogen again, regulates argon flow amount to 800mL/min.After cooling to room temperature with the furnace, take out quartz substrate and collect the carbon nanotube/amorphous carbon composite all-carbon sponge prepared in quartz substrate.By sem observation, coated amorphous carbon layer thickness is about 15nm.
embodiment 6
The quartz substrate of cleaning is positioned over the middle part, quartz reaction chamber of High Temperature Furnaces Heating Apparatus, then seals quartz reaction chamber, regulate heating schedule and start to heat up; The argon gas air got rid of in reaction chamber passing into 800mL/min in temperature-rise period keeps atmosphere to stablize; After temperature rises to 880 DEG C, adjustment argon flow amount is 2000mL/min, and passes into the hydrogen of 300mL/min, open precise injection pump, in reaction chamber, implantation concentration is the ferrocene/dichlorobenzene carbon source reaction soln of 60mg/mL, and speed of feed is 0.1mL/min, and the reaction times is 2h.Subsequently, feed-disabling ferrocene/dichlorobenzene carbon source reaction soln also turns off hydrogen, and Reaktionsofen is cooled under the argon gas atmosphere that airshed is 800mL/min is protected.When temperature is down to 600 ~ 750 DEG C, arranging Reaktionsofen temperature control program makes it keep 10min at this temperature, argon flow amount is adjusted to 2000mL/min simultaneously, hydrogen flowing quantity is 300mL/min, and is the ferrocene/dichlorobenzene carbon source reaction soln of 20 ~ 100mg/mL with the speed feeding concentration of 0.1 ~ 0.3mL/min.After reaction 10min, feed-disabling ferrocene/dichlorobenzene carbon source reaction soln turn off hydrogen again, regulates argon flow amount to 800mL/min.After cooling to room temperature with the furnace, take out quartz substrate and collect the carbon nanotube/amorphous carbon composite all-carbon sponge prepared in quartz substrate.By sem observation, coated amorphous carbon layer thickness is about 12nm.
embodiment 7
The quartz substrate of cleaning is positioned over the middle part, quartz reaction chamber of High Temperature Furnaces Heating Apparatus, then seals quartz reaction chamber, regulate heating schedule and start to heat up; The argon gas air got rid of in reaction chamber passing into 800mL/min in temperature-rise period keeps atmosphere to stablize; After temperature rises to 880 DEG C, adjustment argon flow amount is 2000mL/min, and passes into the hydrogen of 300mL/min, open precise injection pump, in reaction chamber, implantation concentration is the ferrocene/dichlorobenzene carbon source reaction soln of 60mg/mL, and speed of feed is 0.1mL/min, and the reaction times is 2h.Subsequently, feed-disabling ferrocene/dichlorobenzene carbon source reaction soln also turns off hydrogen, and Reaktionsofen is cooled under the argon gas atmosphere that airshed is 800mL/min is protected.When temperature is down to 600 ~ 750 DEG C, arranging Reaktionsofen temperature control program makes it keep 5min at this temperature, argon flow amount is adjusted to 2000mL/min simultaneously, hydrogen flowing quantity is 300mL/min, and is the ferrocene/dichlorobenzene carbon source reaction soln of 20 ~ 100mg/mL with the speed feeding concentration of 0.1 ~ 0.3mL/min.After reaction 5min, feed-disabling ferrocene/dichlorobenzene carbon source reaction soln turn off hydrogen again, regulates argon flow amount to 800mL/min.After cooling to room temperature with the furnace, take out quartz substrate and collect the carbon nanotube/amorphous carbon composite all-carbon sponge prepared in quartz substrate.By sem observation, coated amorphous carbon layer thickness is about 8nm.
Claims (8)
1. a step prepares the method for super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge, it is characterized in that described method steps is as follows:
One, the preparation of carbon nanotube sponge: the quartz substrate of cleaning is positioned over the silica tube middle part of Reaktionsofen and sealed silica envelope, Reaktionsofen heating schedule is set, logical argon gas is to get rid of residual air in silica tube, Reaktionsofen injects ferrocene/dichlorobenzene carbon source solution reaction 0.5 ~ 4h when being warming up to 820 ~ 940 DEG C under hydrogen/argon gas mixed atmosphere, turn off the injection of hydrogen and ferrocene/dichlorobenzene carbon source solution after reaction, lower the temperature with stove under argon shield;
The preparation of two, super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge: when being down to 600 ~ 750 DEG C; keep temperature and again pass into ferrocene/dichlorobenzene carbon source solution, hydrogen; after 5 ~ 60min; obtain carbon nanotube/amorphous carbon composite all-carbon sponge; turn off carbon source and cool to room temperature with the furnace under argon shield, collecting product.
2. a step according to claim 1 prepares the method for super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge, it is characterized in that in described step one, is 600 ~ 1000mL/min for emptying reaction room air passes into argon flow amount.
3. a step according to claim 1 prepares the method for super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge, it is characterized in that in described step one, and during reaction, hydrogen flowing quantity is 100 ~ 500mL/min, and argon flow amount is 1600 ~ 2400mL/min.
4. a step according to claim 1 prepares the method for super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge, it is characterized in that in described step one, the concentration of ferrocene/dichlorobenzene carbon source solution is 20 ~ 100mg/mL, and speed of feed is 0.1 ~ 0.3mL/min.
5. a step according to claim 1 prepares the method for super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge, it is characterized in that in described step one, and during cooling, argon flow amount is 100 ~ 300mL/min.
6. a step according to claim 1 prepares the method for super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge, it is characterized in that in described step 2, the concentration of ferrocene/dichlorobenzene carbon source solution is 20 ~ 100mg/mL, and ferrocene/dichlorobenzene carbon source solution speed of feed is 0.1 ~ 0.3mL/min.
7. a step according to claim 1 prepares the method for super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge, it is characterized in that in described step 2, and during reaction, argon flow amount is 1600 ~ 2400mL/min, and hydrogen flowing quantity is 100 ~ 500mL/min.
8. a step according to claim 1 prepares the method for super-elasticity carbon nanotube/amorphous carbon composite all-carbon sponge, it is characterized in that in described step 2, and during cooling, argon flow amount is 600 ~ 1000mL/min.
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| CN107986261B (en) * | 2018-01-09 | 2021-01-05 | 郑州大学 | Device and method for preparing oversized carbon nanotube three-dimensional porous block |
| CN110871270B (en) * | 2018-09-04 | 2021-07-20 | 天津大学 | Preparation method of high-elasticity high-heat-conductivity three-dimensional carbon nanotube composite material |
| CN112176313A (en) * | 2019-07-02 | 2021-01-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Glassy carbon/carbon nanotube film composite material and preparation method and application thereof |
| CN112174115B (en) * | 2020-09-16 | 2022-04-12 | 华中科技大学 | Hierarchical carbon nanotube dry glue, preparation and application as adhesive |
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