CN114538414A - Synthesis method of single-walled carbon nanotube fiber - Google Patents
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Abstract
The invention discloses a method for synthesizing single-walled carbon nanotube fibers, belonging to the technical field of chemistry. The method uses radio frequency plasma to decompose ferric chloride (catalyst), thiophene (catalytic assistant) and coal tar (carbon source), and carries out vapor deposition in a vertical furnace to synthesize the single-walled carbon nanotube fiber. The method has simple flow, higher production efficiency and cheap used raw materials compared with the current floating catalysis method, is suitable for fibrous single-walled carbon nanotubes with lower production cost, and is used for manufacturing the conductive agent for special cables and lithium batteries.
Description
Technical Field
The invention relates to a method for synthesizing single-walled carbon nanotube fibers, belonging to the technical field of chemistry.
Background
The carbon nano fiber and the carbon nano tube have similar microstructure appearance and properties, so that the carbon nano fiber and the carbon nano tube have excellent physical and chemical properties. Therefore, the carbon nanofiber has wide application potential in the aspects of lithium ion battery materials, super capacitor materials, sensing materials, intelligent materials, devices thereof and the like. In recent years, carbon nanotubes have been widely used as an excellent conductive agent in the lithium ion battery industry of new energy automobiles. The capacity, the service life and the safety of the lithium battery are obviously improved. Along with the requirements of new energy automobiles on high energy density, safer and higher-rate charge and discharge of lithium ion batteries and the like, the performance of the lithium ion batteries is improved urgently. Compared with a multi-wall carbon nanotube, the single-wall carbon nanotube has higher length-diameter ratio, better mechanical strength and higher flexibility. The conductive agent is added into the anode and cathode materials, can provide stable and rich conductive networks in the lithium intercalation and deintercalation process, and effectively improve the mechanical property of the pole piece. Because the single-walled carbon nanotube fiber and the single-walled carbon nanotube have similar structures and properties, the single-walled carbon nanotube fiber and the single-walled carbon nanotube fiber can also be used as an efficient conductive agent to be applied to anode and cathode materials of a lithium ion battery.
The research and development of the carbon nano fiber and the carbon nano tube are synchronous, the preparation methods are basically the same, and the specific preparation processes are different. At present, the synthesis method of the single-walled carbon nanotube is mainly an arc discharge method, generally, under the inert atmosphere, graphite with a distance of a few millimeters generates arc discharge under the action of strong current, an anode is consumed, and carbon deposits are formed on the surface of a cathode. The method has high energy consumption and low yield, so the synthesis method with lower development cost is very important for the wider application of the single-walled carbon nanotube.
Compared with the arc discharge method, the CVD method has become the mainstream method of carbon nanotube laboratory and industrial production due to its advantages of simple equipment, low temperature, easily controlled parameters, etc. The plasma source is introduced into the CVD process, and because the plasma contains high-energy electrons, the electrons collide with gas-phase molecules to provide the activation energy required by the gas-phase molecular CVD reaction, so that the decomposition and ionization processes of the gas molecules are promoted, and high-activity chemical groups are generated. Further reducing the temperature of the CVD reaction and improving the reaction activity.
Disclosure of Invention
The invention provides a method for synthesizing single-walled carbon nanotube fibers, which comprises the following steps:
(1) dispersing ferric salt and thiophene in ethanol to prepare a catalyst system, and placing the catalyst system in a raw material storage tank 1; adding coal tar serving as a carbon source into a raw material storage tank 2;
(2) introducing helium into a hearth of the CVD device, and controlling the temperature to be 1000-1300 ℃; simultaneously pumping the catalyst system in the raw material storage tank 1 and the carbon source in the raw material storage tank 2 into an ultrasonic atomizer, and introducing the atomized catalyst system and the atomized carbon source into a hearth of a CVD device by taking hydrogen and helium as carriers respectively;
(3) and a plasma torch is arranged in a hearth of the CVD device, and after the atomized catalyst system and the carbon source enter the plasma torch, the radio frequency power supply starts to work to drive the plasma torch to decompose the raw materials and grow in a vapor deposition manner in the furnace to obtain the single-walled carbon nanotube fiber.
In one embodiment of the invention, the concentration of iron salt in the catalyst system is 0.5-0.6 g/mL; the concentration of thiophene is 0.16-0.25 g/mL.
In one embodiment of the present invention, the mass ratio of the iron salt to the thiophene is (2-4): 1.
in one embodiment of the invention, the iron salt may be selected from ferric chloride.
In one embodiment of the invention, the flow rate of the atomized catalyst introduced into the hearth of the CVD device is 8-10 mL/min; the flow rate of the atomized carbon source introduced into the hearth of the CVD device is 300 mL/min.
In one embodiment of the present invention, 3000sccm hydrogen and 1000sccm helium are used as carriers in step (2).
In one embodiment of the present invention, the rf power driving conditions of the plasma torch in step (3) are: the power is 5-8kW, and the frequency is 10-15 MHz.
In one embodiment of the present invention, the method comprises the following steps:
1) weighing ferric chloride and thiophene, adding into an ethanol solution, stirring for dissolving, and adding into a CVD equipment raw material storage tank 1; weighing coal tar as a carbon source, and adding the coal tar into a raw material storage tank 2;
2) heating the CVD furnace chamber to 1200 ℃ under the condition of introducing helium; then pumping the raw materials in the storage tank 1 and the storage tank 2 into an ultrasonic atomizer simultaneously; after the raw material is pumped into the ultrasonic atomizer, the ultrasonic atomizer starts to work, and meanwhile, 3000sccm hydrogen and 1000sccm helium are used as carriers to bring the atomized raw material into a plasma torch;
3) after the atomized raw materials enter a plasma torch, a radio frequency power supply starts to work to drive the plasma torch to decompose the raw materials, and single-walled carbon nanotube fibers grow in a furnace through vapor deposition; and (3) cooling the grown single-walled carbon nanotube fiber by a stainless steel water cooling jacket at the lower end, and collecting a product.
The invention also provides a single-walled carbon nanotube fiber based on the preparation method.
The invention also provides the application of the single-walled carbon nanotube fiber in lithium ion battery materials, super capacitor materials, sensing materials and intelligent materials.
Advantageous effects
The invention decomposes ferric chloride (catalyst), thiophene (catalytic assistant) and coal tar (carbon source) by using radio frequency plasma, and synthesizes the single-walled carbon nanotube fiber by vapor deposition in a vertical furnace. The method has simple flow, higher production efficiency and low cost of used raw materials compared with the current floating catalysis method, is suitable for fibrous single-walled carbon nanotubes with lower production cost, and is used for manufacturing the conductive agent for special cables and lithium batteries.
Drawings
FIG. 1 is a scanning electron microscope image of the single-walled carbon nanotube fiber obtained in example 1, magnified 100000 times.
FIG. 2 is a scanning electron micrograph of the single-walled carbon nanotube fiber obtained in example 1 magnified 1000000 times.
Detailed Description
The coal tar involved in the embodiment of the invention is purchased from Hubei weiKun energy low-temperature coal tar B0029.
Example 1
26.3g of ferric chloride and 12.5g of thiophene were weighed, 50g of ethanol was added, and the mixture was stirred and dissolved to obtain a catalyst solution. 3kg of coal tar was weighed as a carbon source.
A vertical corundum tube furnace with the tube diameter of 100mm and the height of 1500mm is used as a reactor, and heat is preserved after a hearth is heated to 1200 ℃ under helium purging. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into the ultrasonic atomizer, respectively, and the atomized raw material was taken into the plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow rate of the atomized catalyst solution is controlled to be 8mL/min, the flow rate of the atomized coal tar is controlled to be 300mL/min, and mixed gas of 3000sccm hydrogen and 1000sccm helium is used as carrier gas. A radio frequency power supply with the power of 5kW and the frequency of 13.56MHz is used for driving a plasma torch, reaction raw materials are subjected to ultrasonic full atomization and then enter the plasma torch for decomposition, single-walled carbon nanotube fibers are synthesized through vapor deposition in a vertical furnace, and reaction products are cooled by a stainless steel water cooling jacket at the lower end and then collected.
Example 2
26.3g of ferric chloride and 12.5g of thiophene were weighed, 50g of ethanol was added, and the mixture was stirred and dissolved to obtain a catalyst solution. 3kg of coal tar was weighed as a carbon source.
A vertical corundum tube furnace with the tube diameter of 100mm and the height of 1500mm is used as a reactor, and heat is preserved after a hearth is heated to 1200 ℃ under helium purging. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into the ultrasonic atomizer, respectively, and the atomized raw material was taken into the plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow of the atomized catalyst solution is controlled to be 9mL/min, the flow of the atomized coal tar is controlled to be 300mL/min, mixed gas of 3000sccm hydrogen and 1000sccm helium is used as carrier gas, and the coal tar is purchased from Hubei Wei Kun energy low-temperature coal tar b 0029. A radio frequency power supply with the power of 5kW and the frequency of 13.56MHz is used for driving a plasma torch, reaction raw materials are subjected to ultrasonic full atomization and then enter the plasma torch for decomposition, single-walled carbon nanotube fibers are synthesized through vapor deposition in a vertical furnace, and reaction products are cooled by a stainless steel water cooling jacket at the lower end and then collected.
Example 3
30g of ferric chloride and 8g of thiophene are weighed, 50g of ethanol is added, and the mixture is stirred and dissolved to be used as a catalyst solution. 3kg of coal tar was weighed as a carbon source.
A corundum tube vertical furnace with the tube diameter of 100mm and the height of 1500mm is used as a reactor, and heat is preserved after a hearth is heated to 1200 ℃ under helium purging. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into the ultrasonic atomizer, respectively, and the atomized raw material was taken into the plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow rate of the atomized catalyst solution is controlled to be 9mL/min, the flow rate of the atomized coal tar is controlled to be 300mL/min, and mixed gas of 3000sccm hydrogen and 1000sccm helium is used as carrier gas. The coal tar purchased from Hubei weikun energy low-temperature coal tar b0029 drives a plasma torch by using a radio frequency power supply with power of 5kW and frequency of 13.56MHz, reaction raw materials enter the plasma torch to be decomposed after being sufficiently atomized by ultrasonic, single-walled carbon nanotube fibers are synthesized by vapor deposition in a vertical furnace, and reaction products are collected after being cooled by a stainless steel water cooling jacket at the lower end.
Example 4
30g of ferric chloride and 8g of thiophene are weighed, 50g of ethanol is added, and the mixture is stirred and dissolved to be used as a catalyst solution. 3kg of coal tar was weighed as a carbon source.
A vertical corundum tube furnace with the tube diameter of 100mm and the height of 1500mm is used as a reactor, and heat is preserved after a hearth is heated to 1200 ℃ under helium purging. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into the ultrasonic atomizer, respectively, and the atomized raw material was taken into the plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow of the atomized catalyst solution is controlled to be 10mL/min, the flow of the atomized coal tar is controlled to be 300mL/min, mixed gas of 3000sccm hydrogen and 1000sccm helium is used as carrier gas, and the coal tar is purchased from Hubei Wei Kun energy low-temperature coal tar b 0029. A radio frequency power supply with the power of 5kW and the frequency of 13.56MHz is used for driving a plasma torch, reaction raw materials are subjected to ultrasonic full atomization and then enter the plasma torch for decomposition, single-walled carbon nanotube fibers are synthesized through vapor deposition in a vertical furnace, and reaction products are cooled by a stainless steel water cooling jacket at the lower end and then collected.
Example 5
25.2g of ferric chloride and 8.4g of thiophene are weighed, 50g of ethanol is added, and the mixture is stirred and dissolved to be used as a catalyst solution. 3kg of coal tar was weighed as a carbon source.
A corundum tube vertical furnace with the tube diameter of 100mm and the height of 1500mm is used as a reactor, and heat is preserved after a hearth is heated to 1200 ℃ under helium purging. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into the ultrasonic atomizer, respectively, and the atomized raw material was taken into the plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow of the atomized catalyst solution is controlled to be 10mL/min, the flow of the atomized coal tar is controlled to be 300mL/min, mixed gas of 3000sccm hydrogen and 1000sccm helium is used as carrier gas, and the coal tar is purchased from Hubei Wei Kun energy low-temperature coal tar b 0029. A radio frequency power supply with the power of 5kW and the frequency of 13.56MHz is used for driving a plasma torch, reaction raw materials are subjected to ultrasonic full atomization and then enter the plasma torch for decomposition, single-walled carbon nanotube fibers are synthesized through vapor deposition in a vertical furnace, and reaction products are cooled by a stainless steel water cooling jacket at the lower end and then collected.
Comparative example 1:
referring to example 1, the flow rate of the catalyst solution was changed from 8mL/min to 20mL/min only as follows:
26.3g of ferric chloride and 12.5g of thiophene were weighed, 50g of ethanol was added, and the mixture was stirred and dissolved to obtain a catalyst solution. 3kg of coal tar was weighed as a carbon source.
A vertical corundum tube furnace with the tube diameter of 100mm and the height of 1500mm is used as a reactor, and heat is preserved after a hearth is heated to 1200 ℃ under helium purging. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into the ultrasonic atomizer, respectively, and the atomized raw material was taken into the plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow rate of the atomized catalyst solution is controlled to be 20mL/min, the flow rate of the atomized coal tar is controlled to be 300mL/min, and mixed gas of 3000sccm hydrogen and 1000sccm helium is used as carrier gas. Coal tar is purchased from Hubei weiwoman energy low-temperature coal tar b 0029. A radio frequency power supply with the power of 5kW and the frequency of 13.56MHz is used for driving a plasma torch, reaction raw materials are subjected to ultrasonic full atomization and then enter the plasma torch for decomposition, single-walled carbon nanotube fibers are synthesized through vapor deposition in a vertical furnace, and reaction products are cooled by a stainless steel water cooling jacket at the lower end and then collected.
Comparative example 2:
referring to example 1, the weight of the weighed ferric chloride was changed to 6g only, as follows:
6g of ferric chloride and 12.5g of thiophene are weighed, 50g of ethanol is added, and the mixture is stirred and dissolved to be used as a catalyst solution. 3kg of coal tar was weighed as a carbon source.
A vertical corundum tube furnace with the tube diameter of 100mm and the height of 1500mm is used as a reactor, and heat is preserved after a hearth is heated to 1200 ℃ under helium purging. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into the ultrasonic atomizer, respectively, and the atomized raw material was taken into the plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow rate of the atomized catalyst solution is controlled to be 8mL/min, the flow rate of the atomized coal tar is controlled to be 300mL/min, and mixed gas of 3000sccm hydrogen and 1000sccm helium is used as carrier gas. Coal tar is purchased from Hubei weikun energy low-temperature coal tar b 0029. A radio frequency power supply with the power of 5kW and the frequency of 13.56MHz is used for driving a plasma torch, reaction raw materials are subjected to ultrasonic full atomization and then enter the plasma torch for decomposition, single-walled carbon nanotube fibers are synthesized through vapor deposition in a vertical furnace, and reaction products are cooled by a stainless steel water cooling jacket at the lower end and then collected.
Comparative example 3:
referring to example 1, benzene was selected as a carbon source in the reaction.
26.3g of ferric chloride and 12.5g of thiophene were weighed, 50g of ethanol was added, and the mixture was stirred and dissolved to obtain a catalyst solution. 3kg of benzene were weighed out as carbon source.
A vertical corundum tube furnace with the tube diameter of 100mm and the height of 1500mm is used as a reactor, and heat is preserved after a hearth is heated to 1200 ℃ under helium purging. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into the ultrasonic atomizer, respectively, and the atomized raw material was taken into the plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow rate of the atomized catalyst solution was controlled to be 8mL/min, the flow rate of the atomized benzene was controlled to be 300mL/min, and a mixed gas of 3000sccm hydrogen and 1000sccm helium was used as a carrier gas. A radio frequency power supply with the power of 5kW and the frequency of 13.56MHz is used for driving a plasma torch, reaction raw materials are subjected to ultrasonic full atomization and then enter the plasma torch for decomposition, single-walled carbon nanotube fibers are synthesized through vapor deposition in a vertical furnace, and reaction products are cooled by a stainless steel water cooling jacket at the lower end and then collected.
Comparative example 4:
referring to example 1, cyclohexane was selected as a carbon source during the reaction, specifically as follows:
26.3g of ferric chloride and 12.5g of thiophene were weighed, 50g of ethanol was added, and the mixture was stirred and dissolved to obtain a catalyst solution. 3kg of cyclohexane were weighed out as carbon source.
A vertical corundum tube furnace with the tube diameter of 100mm and the height of 1500mm is used as a reactor, and heat is preserved after a hearth is heated to 1200 ℃ under helium purging. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into the ultrasonic atomizer, respectively, and the atomized raw material was taken into the plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow rate of the atomized catalyst solution was controlled to be 8mL/min, the flow rate of the atomized cyclohexane was controlled to be 300mL/min, and a mixed gas of 3000sccm hydrogen and 1000sccm helium was used as a carrier gas. A radio frequency power supply with the power of 5kW and the frequency of 13.56MHz is used for driving a plasma torch, reaction raw materials are subjected to ultrasonic full atomization and then enter the plasma torch for decomposition, single-walled carbon nanotube fibers are synthesized through vapor deposition in a vertical furnace, and reaction products are cooled by a stainless steel water cooling jacket at the lower end and then collected.
And (3) performance testing:
after the reaction, the collected carbon nanotube fibers were weighed. Mechanically pulverizing to obtain carbon nanotube powder, and making into slurry (97.5% NMP + 2% CNT + 0.25% dispersant + 0.5% PVP). The resistivity after coating is tested, 7.5g of slurry, 50g of HSV and 15.6g of LCO are proportioned, and the addition amount of CNT is 0.3 percent. The test results are shown in table 1:
TABLE 1 Properties of carbon nanotube fibers obtained by different methods
| Carbon nanotube fiber | Mass/g | Resistivity/omega cm |
| Example 1 | 215.21 | 8.06 |
| Example 2 | 217.32 | 9.23 |
| Example 3 | 216.5 | 8.29 |
| Example 4 | 217.27 | 8.47 |
| Example 5 | 216.89 | 8.5 |
| Comparative example 1 | 164.2 | 16.25 |
| Comparative example 2 | 179.83 | 15.21 |
| Comparative example 3 | 168.67 | 16.36 |
| Comparative example 4 | 189.35 | 25.37 |
As can be seen from the table, comparative example 1 only changed the flow ratio of the catalyst to the carbon source, and comparative example 2 only changed the ratio of ferric chloride to thiophene, and the yield of carbon tubes was decreased and conductivity was deteriorated after the change, as compared to example 1. Comparative example 3 only changed the carbon source to benzene and comparative example 4 only changed the carbon source to cyclohexane, and both the carbon tube yield was decreased and the conductivity was deteriorated as compared with example 1.
Claims (10)
1. A method for synthesizing single-walled carbon nanotube fibers is characterized by comprising the following steps:
(1) dispersing ferric salt and thiophene in ethanol to prepare a catalyst system, and placing the catalyst system in a raw material storage tank 1; adding coal tar serving as a carbon source into a raw material storage tank 2;
(2) introducing helium into a hearth of the CVD device, and controlling the temperature to be 1000-1300 ℃; simultaneously pumping the catalyst system in the raw material storage tank 1 and the carbon source in the raw material storage tank 2 into an ultrasonic atomizer, and introducing the atomized catalyst system and the atomized carbon source into a hearth of a CVD device by taking hydrogen and helium as carriers respectively;
(3) and a plasma torch is arranged in a hearth of the CVD device, and after the atomized catalyst system and the carbon source enter the plasma torch, the radio frequency power supply starts to work to drive the plasma torch to decompose the raw materials and grow in a vapor deposition manner in the furnace to obtain the single-walled carbon nanotube fiber.
2. The method of claim 1, wherein the concentration of the iron salt in the catalyst system is 0.5-0.6 g/mL; the concentration of thiophene is 0.16-0.25 g/mL.
3. The method according to claim 1, wherein the mass ratio of the iron salt to the thiophene is (2-4): 1.
4. the method of claim 1, wherein in step (2), the atomized catalyst is introduced into the furnace of the CVD apparatus at a flow rate of 8-10 mL/min.
5. The method of claim 1, wherein in step (2), the atomized carbon source is introduced into the hearth of the CVD apparatus at a flow rate of 300 mL/min.
6. The method of claim 1, wherein 3000 seem hydrogen and 1000 seem helium are used as carriers in step (2).
7. The method of claim 1, wherein the RF power driving conditions of the plasma torch in step (3) are: the power is 5-8kW, and the frequency is 10-15 MHz.
8. The method of any one of claims 1 to 7, wherein the iron salt is ferric chloride.
9. Single-walled carbon nanotube fibers prepared by the method of any one of claims 1 to 8.
10. The use of the single-walled carbon nanotube fiber of claim 9 in lithium ion battery materials, supercapacitor materials, sensing materials, smart materials.
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