CN114477146A - High-density orientation method for carbon nano tube in unit width - Google Patents
High-density orientation method for carbon nano tube in unit width Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 197
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 178
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 178
- 238000000034 method Methods 0.000 title claims abstract description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 171
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- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 21
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 16
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- 230000001788 irregular Effects 0.000 claims description 3
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- 239000011521 glass Substances 0.000 description 12
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
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- 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
Abstract
The invention relates to a high-density orientation method of carbon nano tubes in unit width, which comprises the following steps: preparing a carbon nano tube flat belt by adopting a floating catalysis method; respectively erecting two ends of a carbon nano tube flat belt on a first winding shaft and a second winding shaft; pressing the erected carbon nanotube flat belt into water; and carrying out high-energy ultrasonic treatment on the carbon nanotube flat belt through an ultrasonic amplitude transformer immersed in water. The aim of the method for aligning the carbon nanotubes in high density in unit width is to solve the problem of how to realize the alignment of the carbon nanotubes in high density without acid, surfactant or other additives.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a high-density orientation method of carbon nano tubes in unit width.
Background
The carbon nano tube is considered as an ideal reinforcement of a composite material and a wave-absorbing material, the performance of the carbon nano tube is best in the axial direction, the carbon nano tube needs to be aligned to realize effective reinforcement of the carbon nano tube on the composite material or optimization of dielectric performance, and the existing methods for aligning the carbon nano tube include a liquid phase method and an array method.
The solution-based carbon nanotube orientation arrangement method needs to firstly realize the dispersion and separation of carbon nanotubes through the physical adsorption or chemical modification of a surfactant or a small aromatic molecule, a macrocyclic conjugate and a strong acid, and then realize the horizontal orientation arrangement of the carbon nanotubes by combining various physical and chemical methods. (CN200810060546.0 film formation by chain molecule combination and LB method using nitric acid, CN02111337, CN200410009281.3, CN201010247437.7 carbon nanotube solution electrification arrangement, 201811073606 carbon nanotube aromatic ring molecule dispersion and pulling)
The array method is a technique of depositing catalyst particles on a substrate, growing carbon nanotubes by a CVD method, and pulling the carbon nanotubes to align them by a mechanical force. The density of the carbon nanotubes aligned by the array method is similar to that of the liquid phase method, but the substrate size is limited, the number of steps is large, the cost is high, and the application is limited. (CN1504408A carbon nanotube array Structure and method for producing the same)
The current high-density orientation arrangement of the carbon nanotubes has the following problems:
1. in the liquid phase method, the carbon tube structure is damaged due to acid treatment, and the performance loss is serious;
2. the carbon tube processed by any method and a liquid phase method has limited density in unit width, and is difficult to exceed 200 pieces/cm;
3. the carbon tube density which can be processed by the array method is difficult to exceed 200/cm due to the limitation of the amount of the catalyst.
Therefore, the technical problem to be solved at present is how to align carbon nanotubes with high density without the need of acid, surfactant or other additives.
Accordingly, the inventors provide a method for high density alignment of carbon nanotubes per unit width.
Disclosure of Invention
(1) Technical problem to be solved
The embodiment of the invention provides a high-density orientation method for carbon nanotubes in unit width, which solves the technical problem of realizing high-density orientation arrangement of the carbon nanotubes without acid, surfactant or other additives.
(2) Technical scheme
The invention provides a high-density orientation method of carbon nanotubes in unit width, which comprises the following steps:
preparing a carbon nano tube flat belt by adopting a floating catalysis method;
respectively erecting two ends of the carbon nano tube flat belt on a first winding shaft and a second winding shaft;
pressing the erected carbon nanotube flat belt into water;
and carrying out high-energy ultrasonic treatment on the carbon nanotube flat belt through an ultrasonic amplitude transformer immersed in water.
Furthermore, the carbon nanotube ribbon is a porous network structure, and pores of the porous network structure are open pore structures and are irregular shapes surrounded by overlapped tube bundles or carbon tubes.
Further, the two ends of the carbon nanotube ribbon are respectively erected on the first winding shaft and the second winding shaft, and the method specifically comprises the following steps:
and two ends of the carbon nano tube flat belt are respectively wound on the first winding shaft and the second winding shaft, and the winding length is greater than 1 cm.
Furthermore, the depth of the carbon nanotube flat belt pressed into water is 1-10 cm.
Further, the distance between one end of the ultrasonic amplitude transformer, which faces the carbon nanotube flat belt, and the carbon nanotube flat belt is 1-10 cm.
Further, the high-energy ultrasonic treatment of the carbon nanotube flat belt by the ultrasonic amplitude transformer immersed in water specifically comprises the following steps:
the carbon nano tube flat belt moves from the first winding shaft to the second winding shaft;
opening the amplitude transformer and processing the carbon nanotube flat belt;
wherein the part of the moving carbon nanotube flat belt in water is always kept in the projection plane of the amplitude transformer.
Further, the rotating speeds of the first and second bobbins include a releasing speed and a collecting speed, and the collecting speed is greater than or equal to the releasing speed.
Further, when the collecting speed is equal to the releasing speed, the speed range is 0.5-200 m/min.
Further, when the collecting speed is greater than the releasing speed, the speed range is 0.5-200 m/min, and the speed difference is less than or equal to 1 m/min.
Furthermore, the ultrasonic power of the ultrasonic horn is 10-2000W.
(3) Advantageous effects
In conclusion, the invention induces bubbles in water through ultrasound, the bubbles expand and break to break up the network part, and the broken network is straightened by the pulling force of the collecting shaft, thereby realizing that the carbon nano tube achieves high-density orientation in water without acid, surfactant or additive, and avoiding the problems that the conductivity is reduced because the wall structure of the acid-adding carbon tube is damaged and the surfactant is not easy to clean and does not conduct electricity.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments of the present invention will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic flow chart of a method for high-density alignment of carbon nanotubes per unit width according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of an ultrasonic treatment process in a method for high-density alignment of carbon nanotubes per unit width according to an embodiment of the present invention;
FIG. 3 is a SEM structural comparison of the carbon nanotube orientation before and after sonication provided by an embodiment of the present invention;
FIG. 4 is a schematic diagram of a TEM structure of a carbon nanotube according to an embodiment of the present invention;
fig. 5 is a raman spectrum before and after the ultrasonic treatment provided by the embodiment of the present invention.
Detailed Description
The embodiments of the present invention will be described in further detail with reference to the drawings and examples. The following detailed description of the embodiments and the accompanying drawings are provided to illustrate the principles of the invention and are not intended to limit the scope of the invention, i.e., the invention is not limited to the embodiments described, but covers any modifications, alterations, and improvements in the parts, components, and connections without departing from the spirit of the invention.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.
Fig. 1 is a schematic flow chart of a method for high-density orientation of carbon nanotubes in a unit width according to an embodiment of the present invention, the method including the following steps:
s100, preparing a carbon nano tube flat belt by adopting a floating catalysis method;
s200, respectively erecting two ends of a carbon nano tube flat belt on a first winding shaft and a second winding shaft;
s300, pressing the erected carbon nanotube flat belt into water;
s400, performing high-energy ultrasonic treatment on the carbon nanotube flat belt through an ultrasonic amplitude transformer immersed in water.
In the embodiment, bubbles are triggered in water through ultrasound, the bubbles expand and break to break up the network part, and the broken network is straightened by the tensile force of the collecting shaft, so that the carbon nano tube can achieve high-density orientation in water without acid, surfactant or additive, and the problems that the wall structure of the acid-adding carbon tube is damaged, and the surfactant is not easy to clean and does not conduct electricity to cause the reduction of the conductivity are solved.
1. Porosity of the material
The porosity calculation method comprises the following steps:
where ρ b is the ribbon bulk density and ρ CNT is the density of close-packed carbon nanotubes (1.2 g/cm)3). The densities of the flat belts before and after treatment were 0.26g/cm respectively3And 0.67g/cm3Calculated as the bandlet porosity before treatment 78.3%, 44.2% after treatment, the porosity was reduced by 43.6%.
2. Degree of orientation
The difference in the peak values of the 2D peaks in the raman spectrum was used to indicate the degree of alignment of the carbon nanotubes, and the 2D relative peak intensity of the flat band before treatment was 0.2408, and after treatment was 0.4025, the alignment of the carbon nanotubes was increased by 67.2%.
3. Number of carbon nanotubes arranged per unit width
The carbon nanotubes have a diameter of 20nm and were determined by TEM (Transmission Electron Microscope) characterization, and SEM (scanning Electron Microscope) microscopic observation of the sonicated sample was performed, as shown in fig. 3, to see that the carbon nanotubes were closely aligned. The array number calculation method comprises the following steps:
wherein N is the number of carbon nanotubes in a unit width, L is a unit width (1cm), dCNTIs the carbon nanotube diameter and P is the porosity. The number of carbon nanotubes per unit width was calculated to be 279000. Compared with a liquid phase method and an array method, the method has the advantage that the increase is more than 130 times.
In some alternative embodiments, the ribbon of carbon nanotubes is a porous network structure, the pores of which are open pore structures and are irregular shapes surrounded by overlapping bundles or tubes.
Specifically, the microstructure of the carbon nanotube flat belt is in a network shape, after the flat belt is put into water, the network is filled with water, the ultrasonic wave causes bubbles in the water, the bubbles expand and break to break the network part, and the broken network is straightened by the pulling force of the collecting shaft to form orientation. Carbon nanotubes are discrete bundles of a single tubular object (e.g., a pair of chopsticks) comprising a plurality of carbon tubes, the walls of which are held together by van der waals forces, and a bundle comprising 3 to 100 carbon tubes (e.g., a pair of chopsticks).
In some optional embodiments, two ends of the carbon nanotube ribbon are respectively mounted on the first winding shaft and the second winding shaft, specifically:
the two ends of the carbon nano tube flat belt are respectively wound on the first winding shaft and the second winding shaft, and the winding length is larger than 1 cm.
Specifically, the flat belt is wound on a winding shaft, the diameter of the winding shaft is 2.1cm, and the length of the winding shaft is about 6.6cm, so that the flat belt is similar to a winding wool or a fishing line; in order to ensure that the flat belt is not scattered, the flat belt needs to be wound for a plurality of circles, generally not less than 1 m; the winding length is determined by the requirement and the shape of the winding shaft, taking the figure 2 as an example, the first winding shaft is wound by at least 1m and can be wound by at most 1000m, the second winding shaft only needs to be fixed, and the length is larger than 1 cm; if a large winding shaft is replaced, the winding can be longer, and the current longest winding is 10000m, and the winding can also be longer. Meanwhile, the first winding shaft and the second winding shaft do not need to be located on the same horizontal plane, the height is adjustable, the result is not affected, and the transverse dislocation does not exceed the length of one winding shaft.
In some optional embodiments, the carbon nanotube ribbon is pressed into the water to a depth of 1-10 cm. Wherein, the water inlet depth only relates to the design of the device, and the flat belt can be 1 cm-10 cm under the ultrasonic head regardless of the principle.
In some optional embodiments, the distance between one end of the ultrasonic amplitude transformer facing the carbon nanotube flat belt and the carbon nanotube flat belt is 1-10 cm. Wherein, the ultrasound acts on the carbon nanotube flat belt, and the carbon nanotube flat belt is in an effective range of ultrasonic energy. The effective range of the ultrasonic head is about 5-10 cm from the ultrasonic head downwards, the carbon nano tube flat belt is scattered when the distance between the carbon nano tube flat belt and the ultrasonic is less than 1cm, and no action or little action is generated when the distance is more than 10 cm.
In some optional embodiments, in step S400, the carbon nanotube ribbon is subjected to high-energy ultrasonic treatment by an ultrasonic horn immersed in water, which specifically includes the following steps:
s401, moving the carbon nano tube flat belt from the first winding shaft to the second winding shaft;
s402, opening an amplitude transformer and processing the carbon nanotube flat belt;
wherein, the part of the moving carbon nanotube flat belt in water is always kept in the projection plane of the amplitude transformer.
In some alternative embodiments, the rotation speeds of the first and second spools include a release speed and a collection speed, and the collection speed is greater than or equal to the release speed.
Specifically, when the release speed is equal to the collection speed, the carbon nanotube ribbon is subjected to a smaller tension; when the releasing speed is lower than the collecting speed, the carbon nanotube flat belt is subjected to larger tension; when the release rate is higher than the collection rate, the carbon nanotube ribbons are accumulated in water and cannot be continuously treated.
In some alternative embodiments, when the collection speed is equal to the release speed, the speed ranges from 0.5 to 200 m/min. The speed of ribbon release and collection determines the tension on the ribbon, the release speed is the same as the collection speed, the tension is small, the collection speed is faster than the release speed, and the tension is large.
In some optional embodiments, when the collection speed is greater than the release speed, the speed range is 0.5-200 m/min, and the speed difference is less than or equal to 1 m/min. Wherein, when the speed difference is larger than 1m/min, the carbon nano tube flat belt can be broken by pulling.
In some optional embodiments, the ultrasonic power of the ultrasonic horn is 10-2000W. The ultrasonic power determines the amount of the induced bubbles, and further determines the scattering degree of the network structure of the carbon nanotube flat belt, the carbon nanotube flat belt cannot be completely scattered, and the completely scattered carbon nanotube flat belt becomes slurry and cannot be stressed and oriented.
Several comparative examples are described below
Examples 1 to 3: the ultrasonic energy is used as a variable, the higher the power is, the better the orientation effect is
Example 1
1. The carbon nano tube flat belt is prepared by a floating catalysis method, the width of the flat belt is 1mm, the thickness of the flat belt is 100um, and the porosity of the flat belt is 90%. The length of the carbon nano-tube is 500um, the diameter is 20nm, and the number of the carbon nano-tubes contained in each meter is 107And (4) root. The single bundle contains 10-100 carbon nanotubes. The pores in the network are open pore structures, with dimensions between 20nm and 200um, and are irregularly shaped surrounded by overlapping bundles of tubes. The flat belt is wound on the winding shaft.
2. And (3) penetrating the winding shaft A containing the flat belt on the stepping motor A, pulling out the flat belt from the winding shaft A, winding the flat belt on the winding shaft B, and penetrating the winding shaft B on the stepping motor B. A water tank is arranged at the lower position, the length of the water tank is 50cm, the depth is 5cm, the width is 3cm, and deionized water is poured into the water tank to reach the depth of 3 cm.
3. The flat belt is pressed into the water. And pressing a part of the flat belt suspended on the water tank into water by using two glass shafts, wherein the water entry depth is more than 2cm, and the part which is not immersed in water is still suspended in the air and is not scraped against the edge of the water tank.
4. And erecting high-energy ultrasound. And (3) erecting high-energy ultrasound, immersing the amplitude transformer into water, wherein the diameter of the amplitude transformer is 5mm, and the projection of the amplitude transformer covers the flat belt and is about 2cm away from the flat belt.
5. High-energy ultrasonic treatment of the flat band. And sequentially opening the stepping motor B and the stepping motor A to enable the flat belt to move from the winding shaft A to the winding shaft B, wherein the speed of the winding shaft A, B is 1 m/min. The part of the moving flat belt in the water tank is always kept in the projection plane of the amplitude transformer, and immediately the ultrasonic is started, wherein the ultrasonic power is 10W, and the frequency is 22Hz, so that the flat belt is processed.
6. A treated sample was obtained. Thirdly, obtaining the high-density oriented carbon tube sample from the treated narrow band on the winding shaft B. The porosity of the ribbons before treatment was 78.3%, the degree of orientation was 0.2408, the number of carbon nanotubes per unit width was 65000, the porosity of the samples after treatment was 61.6%, the degree of orientation was 0.2885, and the number of carbon nanotubes per unit width was about 89000.
Example 2
1. The carbon nano tube flat belt is prepared by a floating catalysis method, the width of the flat belt is 1mm, the thickness of the flat belt is 100um, and the porosity of the flat belt is 90%. The length of the carbon nano-tube is 500um, the diameter is 20nm, and the number of the carbon nano-tubes contained in each meter is 107And (4) root. The single bundle contains 10-100 carbon nanotubes. The pores in the network are open pore structures, with dimensions between 20nm and 200um, and are irregularly shaped surrounded by overlapping bundles of tubes. The flat belt is wound on the winding shaft.
2. And (3) penetrating the winding shaft A containing the flat belt on the stepping motor A, pulling out the flat belt from the winding shaft A, winding the flat belt on the winding shaft B, and penetrating the winding shaft B on the stepping motor B. A water tank is arranged at the lower position, the length of the water tank is 50cm, the depth is 5cm, the width is 3cm, and deionized water is poured into the water tank to reach the depth of 3 cm.
3. The flat belt is pressed into the water. And pressing a part of the flat belt suspended on the water tank into water by using two glass shafts, wherein the water entry depth is more than 2cm, and the part which is not immersed into water is still suspended in the air and is not scraped with the edge of the water tank.
4. And erecting high-energy ultrasound. And (3) erecting high-energy ultrasound, immersing the amplitude transformer into water, wherein the diameter of the amplitude transformer is 5mm, and the projection of the amplitude transformer covers the flat belt and is about 2cm away from the flat belt.
5. High-energy ultrasonic treatment of the flat band. And sequentially opening the stepping motor B and the stepping motor A to enable the flat belt to move from the winding shaft A to the winding shaft B, wherein the speed of the winding shaft A, B is 1 m/min. The part of the moving flat belt in the water tank is always kept in the projection plane of the amplitude transformer, and immediately the ultrasonic is started, wherein the ultrasonic power is 500W, and the frequency is 22Hz, so that the flat belt is processed.
6. A treated sample was obtained. Thirdly, obtaining the high-density oriented carbon tube sample from the treated narrow band on the winding shaft B. The porosity of the flat ribbon before treatment was 78.3%, the degree of orientation was 0.2408, the number of carbon nanotubes arranged per unit width was 65000, the porosity of the sample after treatment was 58.4%, the degree of orientation was 0.3182, and the number of carbon nanotubes arranged per unit width was about 95000.
Example 3
1. The carbon nano tube flat belt is prepared by a floating catalysis method, the width of the flat belt is 1mm, the thickness of the flat belt is 100um, and the porosity of the flat belt is 90%. The length of the carbon nano-tube is 500um, the diameter is 20nm, and the number of the carbon nano-tubes contained in each meter is 107And (4) root. The single bundle contains 10-100 carbon nanotubes. The pores in the network are open pore structures, with dimensions between 20nm and 200um, and are irregularly shaped surrounded by overlapping bundles of tubes. The flat belt is wound on the winding shaft.
2. And (3) penetrating the winding shaft A containing the flat belt on the stepping motor A, pulling out the flat belt from the winding shaft A, winding the flat belt on the winding shaft B, and penetrating the winding shaft B on the stepping motor B. A water tank is arranged at the lower position, the length of the water tank is 50cm, the depth is 5cm, the width is 3cm, and deionized water is poured into the water tank to reach the depth of 3 cm.
3. The flat belt is pressed into the water. And pressing a part of the flat belt suspended on the water tank into water by using two glass shafts, wherein the water entry depth is more than 2cm, and the part which is not immersed in water is still suspended in the air and is not scraped against the edge of the water tank.
4. And erecting high-energy ultrasound. And (3) erecting high-energy ultrasound, immersing the amplitude transformer into water, wherein the diameter of the amplitude transformer is 5mm, and the projection of the amplitude transformer covers the flat belt and is about 2cm away from the flat belt.
5. High-energy ultrasonic treatment of the flat band. And sequentially opening the stepping motor B and the stepping motor A to enable the flat belt to move from the winding shaft A to the winding shaft B, wherein the speed of the winding shaft A, B is 1 m/min. The part of the moving flat belt in the water tank is always kept in the projection plane of the amplitude transformer, and then the ultrasonic is started, wherein the ultrasonic power is 2000W, and the frequency is 22Hz, so that the flat belt is processed.
6. A treated sample was obtained. Thirdly, obtaining the high-density oriented carbon tube sample from the treated narrow band on the winding shaft B. The porosity of the ribbons before treatment was 78.3%, the degree of orientation was 0.2408, the number of carbon nanotubes per unit width was 65000, the porosity of the samples after treatment was 45.5%, the degree of orientation was 0.4017, and the number of carbon nanotubes per unit width was approximately 209000.
Examples 4 to 6: the distance between the ultrasonic head and the flat belt is variable, and the effect is better when the distance is smaller
Example 4
1. The carbon nano tube flat belt is prepared by a floating catalysis method, the width of the flat belt is 1mm, the thickness of the flat belt is 100um, and the porosity of the flat belt is 90%. The length of the carbon nano-tube is 500um, the diameter is 20nm, and the number of the carbon nano-tubes contained in each meter is 107And (4) root. The single bundle contains 10-100 carbon nanotubes. The pores in the network are open pore structures, with dimensions between 20nm and 200um, and are irregularly shaped surrounded by overlapping bundles of tubes. The flat belt is wound on the winding shaft.
2. And (3) penetrating the winding shaft A containing the flat belt on the stepping motor A, pulling out the flat belt from the winding shaft A, winding the flat belt on the winding shaft B, and penetrating the winding shaft B on the stepping motor B. A water tank is arranged at the lower position, the length of the water tank is 50cm, the depth is 5cm, the width is 3cm, and deionized water is poured into the water tank to reach the depth of 3 cm.
3. The flat belt is pressed into the water. And pressing a part of the flat belt suspended on the water tank into water by using two glass shafts, wherein the water entry depth is more than 2cm, and the part which is not immersed in water is still suspended in the air and is not scraped against the edge of the water tank.
4. And erecting high-energy ultrasound. And (3) erecting high-energy ultrasound, immersing the amplitude transformer into water, wherein the diameter of the amplitude transformer is 5mm, and the projection of the amplitude transformer covers the flat belt and is 10cm away from the flat belt.
5. High-energy ultrasonic treatment of flat belts. And sequentially opening the stepping motor B and the stepping motor A to enable the flat belt to move from the winding shaft A to the winding shaft B, wherein the speed of the winding shaft A, B is 1 m/min. The part of the moving flat belt in the water tank is always kept in the projection plane of the amplitude transformer, and immediately the ultrasonic is started, wherein the ultrasonic power is 500W, and the frequency is 22Hz, so that the flat belt is processed.
6. A treated sample was obtained. Thirdly, obtaining the high-density oriented carbon tube sample from the treated narrow band on the winding shaft B. The porosity of the ribbons before treatment was 78.3%, the degree of orientation was 0.2408, the number of carbon nanotubes per unit width was 65000, the porosity of the samples after treatment was 66.9%, the degree of orientation was 0.3077, and the number of carbon nanotubes per unit width was approximately 89600.
Example 5
1. The carbon nano tube flat belt is prepared by a floating catalysis method, the width of the flat belt is 1mm, the thickness of the flat belt is 100um, and the porosity of the flat belt is 90%. The carbon nano-tube contained in the nano-tube has the length of 500um and the diameter of 20nm, and the number of the carbon nano-tubes contained in each meter is 107And (4) root. The single bundle contains 10-100 carbon nanotubes. The pores in the network are open pore structures, with dimensions between 20nm and 200um, and are irregularly shaped surrounded by overlapping bundles of tubes. The flat belt is wound on the winding shaft.
2. And (3) penetrating the winding shaft A containing the flat belt on the stepping motor A, pulling out the flat belt from the winding shaft A, winding the flat belt on the winding shaft B, and penetrating the winding shaft B on the stepping motor B. A water tank is arranged at the lower position, the length of the water tank is 50cm, the depth is 5cm, the width is 3cm, and deionized water is poured into the water tank to reach the depth of 3 cm.
3. The flat belt is pressed into the water. And pressing a part of the flat belt suspended on the water tank into water by using two glass shafts, wherein the water entry depth is more than 2cm, and the part which is not immersed in water is still suspended in the air and is not scraped against the edge of the water tank.
4. And erecting high-energy ultrasound. And (3) erecting high-energy ultrasound, immersing the amplitude transformer into water, wherein the diameter of the amplitude transformer is 5mm, and the projection of the amplitude transformer covers the flat belt and is 5cm away from the flat belt.
5. High-energy ultrasonic treatment of the flat band. And sequentially opening the stepping motor B and the stepping motor A to enable the flat belt to move from the winding shaft A to the winding shaft B, wherein the speed of the winding shaft A, B is 1 m/min. The part of the moving flat belt in the water tank is always kept in the projection plane of the amplitude transformer, and immediately the ultrasonic is started, wherein the ultrasonic power is 500W, and the frequency is 22Hz, so that the flat belt is processed.
6. A treated sample was obtained. Thirdly, obtaining the high-density oriented carbon tube sample from the treated narrow band on the winding shaft B. The porosity of the flat ribbon before treatment was 78.3%, the degree of orientation was 0.2408, the number of carbon nanotubes arranged per unit width was 65000, the porosity of the sample after treatment was 54.8%, the degree of orientation was 0.3093, and the number of carbon nanotubes arranged per unit width was about 134800.
Example 6
1. The carbon nano tube flat belt is prepared by a floating catalysis method, the width of the flat belt is 1mm, the thickness of the flat belt is 100um, and the porosity of the flat belt is 90%. The length of the carbon nano-tube is 500um, the diameter is 20nm, and the number of the carbon nano-tubes contained in each meter is 107And (4) root. The single bundle contains 10-100 carbon nanotubes. The pores in the network are open pore structures, with dimensions between 20nm and 200um, and are irregularly shaped surrounded by overlapping bundles of tubes. The flat belt is wound on the winding shaft.
2. And (3) penetrating the winding shaft A containing the flat belt on the stepping motor A, pulling out the flat belt from the winding shaft A, winding the flat belt on the winding shaft B, and penetrating the winding shaft B on the stepping motor B. A water tank is arranged at the lower position, the length of the water tank is 50cm, the depth is 5cm, the width is 3cm, and deionized water is poured into the water tank to reach the depth of 3 cm.
3. The flat belt is pressed into the water. And pressing a part of the flat belt suspended on the water tank into water by using two glass shafts, wherein the water entry depth is more than 2cm, and the part which is not immersed in water is still suspended in the air and is not scraped against the edge of the water tank.
4. And erecting high-energy ultrasound. And (3) erecting high-energy ultrasound, immersing the amplitude transformer into water, wherein the diameter of the amplitude transformer is 5mm, and the projection of the amplitude transformer covers the flat belt and is 1cm away from the flat belt.
5. High-energy ultrasonic treatment of the flat band. And sequentially opening the stepping motor B and the stepping motor A to enable the flat belt to move from the winding shaft A to the winding shaft B, wherein the speed of the winding shaft A, B is 1 m/min. And the part of the moving flat belt in the water tank is always kept in the projection plane of the amplitude transformer, and immediately, the ultrasonic is started, wherein the ultrasonic power is 500W, and the frequency is 22Hz, so that the flat belt is treated.
6. A treated sample was obtained. Thirdly, obtaining the high-density oriented carbon tube sample from the treated narrow band on the winding shaft B. The bandlet porosity before treatment was 78.3%, the degree of orientation was 0.2408, the number of carbon nanotubes per unit width was 65000, the porosity of the sample after treatment was 44.2%, the degree of orientation was 0.4025, and the number of carbon nanotubes per unit width was about 279000.
Examples 7 to 8: the release and collection speed is used as a variable, the slower the speed, the better the effect
Example 7
1. The carbon nano tube flat belt is prepared by a floating catalysis method, the width of the flat belt is 1mm, the thickness of the flat belt is 100um, and the porosity of the flat belt is 90%. The length of the carbon nano-tube is 500um, the diameter is 20nm, and the number of the carbon nano-tubes contained in each meter is 107And (4) root. The single bundle contains 10-100 carbon nanotubes. The pores in the network are open pore structures, with dimensions between 20nm and 200um, and are irregularly shaped surrounded by overlapping bundles of tubes. The flat belt is wound on the winding shaft.
2. And (3) penetrating the winding shaft A containing the flat belt on the stepping motor A, pulling out the flat belt from the winding shaft A, winding the flat belt on the winding shaft B, and penetrating the winding shaft B on the stepping motor B. A water tank is arranged at the lower position, the length of the water tank is 50cm, the depth is 5cm, the width is 3cm, and deionized water is poured into the water tank to reach the depth of 3 cm.
3. The flat belt is pressed into the water. And pressing a part of the flat belt suspended on the water tank into water by using two glass shafts, wherein the water entry depth is more than 2cm, and the part which is not immersed in water is still suspended in the air and is not scraped against the edge of the water tank.
4. And erecting high-energy ultrasound. And (3) erecting high-energy ultrasound, immersing the amplitude transformer into water, wherein the diameter of the amplitude transformer is 5mm, and the projection of the amplitude transformer covers the flat belt and is 1cm away from the flat belt.
5. High-energy ultrasonic treatment of the flat band. And sequentially opening the stepping motor B and the stepping motor A to enable the flat belt to move from the winding shaft A to the winding shaft B, wherein the speed of the winding shaft A, B is 5 m/min. The part of the moving flat belt in the water tank is always kept in the projection plane of the amplitude transformer, and immediately the ultrasonic is started, wherein the ultrasonic power is 500W, and the frequency is 22Hz, so that the flat belt is processed.
6. A treated sample was obtained. Thirdly, obtaining the high-density oriented carbon tube sample from the treated narrow band on the winding shaft B. The porosity of the ribbons before treatment was 78.3%, the degree of orientation was 0.2408, the number of carbon nanotubes per unit width was 65000, the porosity of the samples after treatment was 66.4%, the degree of orientation was 0.2878, and the number of carbon nanotubes per unit width was approximately 74600.
Example 8
1. The carbon nano tube flat belt is prepared by a floating catalysis method, the width of the flat belt is 1mm, the thickness of the flat belt is 100um, and the porosity of the flat belt is 90%. The length of the carbon nano-tube is 500um, the diameter is 20nm, and the number of the carbon nano-tubes contained in each meter is 107And (4) root. The single bundle contains 10-100 carbon nanotubes. The pores in the network are open pore structures, with dimensions between 20nm and 200um, and are irregularly shaped surrounded by overlapping bundles of tubes. The flat belt is wound on the winding shaft.
2. And (3) penetrating the winding shaft A containing the flat belt on the stepping motor A, pulling out the flat belt from the winding shaft A, winding the flat belt on the winding shaft B, and penetrating the winding shaft B on the stepping motor B. A water tank is arranged at the lower position, the length of the water tank is 50cm, the depth is 5cm, the width is 3cm, and deionized water is poured into the water tank to reach the depth of 3 cm.
3. The flat belt is pressed into the water. And pressing a part of the flat belt suspended on the water tank into water by using two glass shafts, wherein the water entry depth is more than 2cm, and the part which is not immersed in water is still suspended in the air and is not scraped against the edge of the water tank.
4. And erecting high-energy ultrasound. And (3) erecting high-energy ultrasound, immersing the amplitude transformer into water, wherein the diameter of the amplitude transformer is 5mm, and the projection of the amplitude transformer covers the flat belt and is 1cm away from the flat belt.
5. High-energy ultrasonic treatment of the flat band. And sequentially opening the stepping motor B and the stepping motor A to enable the flat belt to move from the winding shaft A to the winding shaft B, wherein the speed of the winding shaft A, B is 50 m/min. The part of the moving flat belt in the water tank is always kept in the projection plane of the amplitude transformer, and immediately the ultrasonic is started, wherein the ultrasonic power is 500W, and the frequency is 22Hz, so that the flat belt is processed.
6. A treated sample was obtained. Thirdly, obtaining the high-density oriented carbon tube sample from the treated narrow band on the winding shaft B. The porosity of the ribbons before treatment was 78.3%, the degree of orientation was 0.2408, the number of carbon nanotubes aligned per unit width was 65000, the porosity of the samples after treatment was 77.6%, the degree of orientation was 0.2415, and the number of carbon nanotubes aligned per unit width was about 67000.
Examples 9 to 10: the collection speed is greater than the release speed, the larger the speed difference is, the better the effect is
Example 9
1. The carbon nano tube flat belt is prepared by a floating catalysis method, the width of the flat belt is 1mm, the thickness of the flat belt is 100um, and the porosity of the flat belt is 90%. The length of the carbon nano-tube is 500um, the diameter is 20nm, and the number of the carbon nano-tubes contained in each meter is 107And (4) root. The single bundle contains 10-100 carbon nanotubes. The pores in the network are open pore structures, with dimensions between 20nm and 200um, and are irregularly shaped surrounded by overlapping bundles of tubes. The flat belt is wound on the winding shaft.
2. And (3) penetrating the winding shaft A containing the flat belt on the stepping motor A, pulling out the flat belt from the winding shaft A, winding the flat belt on the winding shaft B, and penetrating the winding shaft B on the stepping motor B. A water tank is arranged at the lower position, the length of the water tank is 50cm, the depth is 5cm, the width is 3cm, and deionized water is poured into the water tank to reach the depth of 3 cm.
3. The flat belt is pressed into the water. And pressing a part of the flat belt suspended on the water tank into water by using two glass shafts, wherein the water entry depth is more than 2cm, and the part which is not immersed in water is still suspended in the air and is not scraped against the edge of the water tank.
4. And erecting high-energy ultrasound. And (3) erecting high-energy ultrasound, immersing the amplitude transformer into water, wherein the diameter of the amplitude transformer is 5mm, and the projection of the amplitude transformer covers the flat belt and is 1cm away from the flat belt.
5. High-energy ultrasonic treatment of the flat band. And sequentially opening the stepping motor B and the stepping motor A to enable the flat belt to move from the winding shaft A to the winding shaft B, wherein the speed of the winding shaft A is 1m/min, and the speed of the winding shaft B is 1.5 m/min. The part of the moving flat belt in the water tank is always kept in the projection plane of the amplitude transformer, and immediately the ultrasonic is started, wherein the ultrasonic power is 500W, and the frequency is 22Hz, so that the flat belt is processed.
6. A treated sample was obtained. Thirdly, the processed narrow band is removed from the bobbin B, and the high-density oriented carbon tube sample is obtained. The porosity of the ribbons before treatment was 78.3%, the degree of orientation was 0.2408, the number of carbon nanotubes per unit width was 65000, the porosity of the samples after treatment was 67.2%, the degree of orientation was 0.3127, and the number of carbon nanotubes per unit width was about 118700.
Example 10
1. The carbon nano tube flat belt is prepared by a floating catalysis method, the width of the flat belt is 1mm, the thickness of the flat belt is 100um, and the porosity of the flat belt is 90%. The length of the carbon nano-tube is 500um, the diameter is 20nm, and the number of the carbon nano-tubes contained in each meter is 107And (4) root. The single bundle contains 10-100 carbon nanotubes. The pores in the network are open pore structures, with dimensions between 20nm and 200um, and are irregularly shaped surrounded by overlapping bundles of tubes. The flat belt is wound on the winding shaft.
2. And (3) penetrating the winding shaft A containing the flat belt on the stepping motor A, pulling out the flat belt from the winding shaft A, winding the flat belt on the winding shaft B, and penetrating the winding shaft B on the stepping motor B. A water tank is arranged at the lower position, the length of the water tank is 50cm, the depth is 5cm, the width is 3cm, and deionized water is poured into the water tank to reach the depth of 3 cm.
3. The flat belt is pressed into the water. And pressing a part of the flat belt suspended on the water tank into water by using two glass shafts, wherein the water entry depth is more than 2cm, and the part which is not immersed in water is still suspended in the air and is not scraped against the edge of the water tank.
4. And erecting high-energy ultrasound. And (3) erecting high-energy ultrasound, immersing the amplitude transformer into water, wherein the diameter of the amplitude transformer is 5mm, and the projection of the amplitude transformer covers the flat belt and is 1cm away from the flat belt.
5. High-energy ultrasonic treatment of the flat band. And sequentially opening the stepping motor B and the stepping motor A to enable the flat belt to move from the winding shaft A to the winding shaft B, wherein the speed of the winding shaft A is 1m/min, and the speed of the winding shaft B is 2 m/min. The part of the moving flat belt in the water tank is always kept in the projection plane of the amplitude transformer, and immediately the ultrasonic is started, wherein the ultrasonic power is 500W, and the frequency is 22Hz, so that the flat belt is processed.
6. A treated sample was obtained. Thirdly, obtaining the high-density oriented carbon tube sample from the treated narrow band on the winding shaft B. The porosity of the ribbons before treatment was 78.3%, the degree of orientation was 0.2408, the number of carbon nanotubes per unit width was 65000, the porosity of the samples after treatment was 47.1%, the degree of orientation was 0.4002, and the number of carbon nanotubes per unit width was approximately 206000.
Examples 11 to 12: the flat belt is used as a variable, the smaller the flat belt is, the better the effect is
Example 11
1. The carbon nano tube flat belt is prepared by a floating catalysis method, the width of the flat belt is 0.3mm, the thickness of the flat belt is 500 mu m, and the porosity is 78%. The length of the carbon nano-tube is 800um, the diameter is 20nm, and the number of the carbon nano-tubes in each meter is 108. The single bundle contains 10-100 carbon nanotubes. The pores in the network are open pore structures, with dimensions between 20nm and 200um, and are irregularly shaped surrounded by overlapping bundles of tubes. The flat belt is wound on the winding shaft.
2. And (3) penetrating the winding shaft A containing the flat belt on the stepping motor A, pulling out the flat belt from the winding shaft A, winding the flat belt on the winding shaft B, and penetrating the winding shaft B on the stepping motor B. A water tank is arranged at the lower position, the length of the water tank is 50cm, the depth is 5cm, the width is 3cm, deionized water is poured into the water tank, and the water depth is 3 cm.
3. The flat belt is pressed into the water. And pressing a part of the flat belt suspended on the water tank into water by using two glass shafts, wherein the water entry depth is more than 2cm, and the part which is not immersed in water is still suspended in the air and is not scraped against the edge of the water tank.
4. And erecting high-energy ultrasound. And (3) erecting high-energy ultrasound, immersing the amplitude transformer into water, wherein the diameter of the amplitude transformer is 5mm, and the projection of the amplitude transformer covers the flat belt and is 1cm away from the flat belt.
5. High-energy ultrasonic treatment of the flat band. And sequentially opening the stepping motor B and the stepping motor A to enable the flat belt to move from the winding shaft A to the winding shaft B, wherein the speed of the winding shaft A, B is 1 m/min. The part of the moving flat belt in the water tank is always kept in the projection plane of the amplitude transformer, and immediately the ultrasonic is started, wherein the ultrasonic power is 500W, and the frequency is 22Hz, so that the flat belt is processed.
6. A treated sample was obtained. Thirdly, obtaining the high-density oriented carbon tube sample from the treated narrow band on the winding shaft B. The bandlet porosity before treatment was 78.3%, the degree of orientation was 0.2408, the number of carbon nanotubes per unit width was 65000, the porosity of the sample after treatment was 47.1%, the degree of orientation was 0.3957, and the number of carbon nanotubes per unit width was about 183000.
Example 12
1. The carbon nano tube flat belt is prepared by a floating catalysis method, the width of the flat belt is 2mm, the thickness of the flat belt is 500 mu m, and the porosity is 94%. The length of the carbon nano-tube is 300um, the diameter is 20nm, and the number of the carbon nano-tubes contained in each meter is 109. The single bundle contains 10-100 carbon nanotubes. The pores in the network are open pore structures, with dimensions between 20nm and 200um, and are irregularly shaped surrounded by overlapping bundles of tubes. The flat belt is wound on the winding shaft.
2. And (3) penetrating the winding shaft A containing the flat belt on the stepping motor A, pulling out the flat belt from the winding shaft A, winding the flat belt on the winding shaft B, and penetrating the winding shaft B on the stepping motor B. A water tank is arranged at the lower position, the length of the water tank is 50cm, the depth is 5cm, the width is 3cm, and deionized water is poured into the water tank to reach the depth of 3 cm.
3. The flat belt is pressed into the water. And pressing a part of the flat belt suspended on the water tank into water by using two glass shafts, wherein the water entry depth is more than 2cm, and the part which is not immersed in water is still suspended in the air and is not scraped against the edge of the water tank.
4. And erecting high-energy ultrasound. And (3) erecting high-energy ultrasound, immersing the amplitude transformer into water, wherein the diameter of the amplitude transformer is 5mm, and the projection of the amplitude transformer covers the flat belt and is 1cm away from the flat belt.
5. High-energy ultrasonic treatment of the flat band. And sequentially opening the stepping motor B and the stepping motor A to enable the flat belt to move from the winding shaft A to the winding shaft B, wherein the speed of the winding shaft A, B is 1 m/min. The part of the moving flat belt in the water tank is always kept in the projection plane of the amplitude transformer, and immediately the ultrasonic is started, wherein the ultrasonic power is 500W, and the frequency is 22Hz, so that the flat belt is processed.
6. A treated sample was obtained. Thirdly, obtaining the high-density oriented carbon tube sample from the treated narrow band on the winding shaft B. The porosity of the ribbons before treatment was 78.3%, the degree of orientation was 0.2408, the number of carbon nanotube arrays per unit width was 65000, the porosity of the samples after treatment was 69.2%, the degree of orientation was 0.2571, and the number of carbon nanotube arrays per unit width was about 76900.
It should be clear that the embodiments in this specification are described in a progressive manner, and the same or similar parts in the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. The present invention is not limited to the specific steps and structures described above and shown in the drawings. Also, a detailed description of known process techniques is omitted herein for the sake of brevity.
The above are merely examples of the present application and are not intended to limit the present application. Various modifications and alterations to this application will become apparent to those skilled in the art without departing from the scope of this invention. Any modification, equivalent replacement, improvement or the like made within the spirit and principle of the present application shall be included in the scope of the claims of the present application.
Claims (10)
1. A method for high-density orientation of carbon nanotubes in a unit width, the method comprising the steps of:
preparing a carbon nano tube flat belt by adopting a floating catalysis method;
respectively erecting two ends of the carbon nano tube flat belt on a first winding shaft and a second winding shaft;
pressing the erected carbon nano tube flat belt into water;
and carrying out high-energy ultrasonic treatment on the carbon nano tube flat belt through an ultrasonic amplitude transformer immersed in water.
2. The method as claimed in claim 1, wherein the carbon nanotube ribbons have a porous network structure, and the pores of the network structure are open and have irregular shapes surrounded by overlapping bundles or tubes.
3. The method for high-density orientation of carbon nanotubes per unit width according to claim 1, wherein the two ends of the carbon nanotube ribbon are respectively mounted on a first winding shaft and a second winding shaft, specifically:
and two ends of the carbon nano tube flat belt are respectively wound on the first winding shaft and the second winding shaft, and the winding lengths are both greater than 1 cm.
4. The method of claim 1, wherein the ribbon of carbon nanotubes is pressed into water to a depth of 1 to 10 cm.
5. The method for high-density orientation of carbon nanotubes within a unit width according to claim 1, wherein the distance between one end of the ultrasonic horn facing the carbon nanotube ribbon and the carbon nanotube ribbon is 1-10 cm.
6. The method for the high-density orientation of carbon nanotubes in unit width according to claim 1, wherein the high-energy ultrasonic treatment of the carbon nanotube ribbons by an ultrasonic horn immersed in water comprises the following steps:
the carbon nano tube flat belt moves from the first winding shaft to the second winding shaft;
opening the amplitude transformer and processing the carbon nanotube flat belt;
wherein the part of the moving carbon nanotube flat belt in the water is always kept in the projection plane of the amplitude transformer.
7. The method of claim 6, wherein the rotation speeds of the first and second bobbins include a release speed and a collection speed, and the collection speed is greater than or equal to the release speed.
8. The method of claim 7, wherein the collecting speed is equal to the discharging speed, and the speed is in the range of 0.5 to 200 m/min.
9. The method of claim 7, wherein when the collecting speed is higher than the discharging speed, the speed is in the range of 0.5 to 200m/min and the speed difference is less than or equal to 1 m/min.
10. The method for high-density orientation of carbon nanotubes per unit width according to claim 1, wherein the ultrasonic power of the ultrasonic horn is 10 to 2000W.
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| CN101003418A (en) * | 2006-07-14 | 2007-07-25 | 上海兰度科技有限公司 | Composite Nano fiber of directional arranged Nano carbon tube, high-speed preparation device, and preparation method |
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