CN103896249A - Spherical carbon nanotube group and preparation method and use thereof - Google Patents
Spherical carbon nanotube group and preparation method and use thereof Download PDFInfo
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- CN103896249A CN103896249A CN201410114240.4A CN201410114240A CN103896249A CN 103896249 A CN103896249 A CN 103896249A CN 201410114240 A CN201410114240 A CN 201410114240A CN 103896249 A CN103896249 A CN 103896249A
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Abstract
The invention discloses a spherical carbon nanotube group and a preparation method and use thereof. The spherical carbon nanotube group is formed by the following processes: putting carbon nano tubes into a rotary device, and agglomerating disorderly wound carbon nano tubes into an orderly interwoven group in a rotating manner; the particle size of the group is 0.1-3 micrometers; the group is spherical or bar-shaped. The preparation method comprises the following steps: grinding the carbon nano tubes with a grinding medium in a grinding miller to grind and forming powder formed by the spherical carbon nano tube group, or grinding by grinding equipment free of grinding medium, so as to form the powder formed by the carbon nano tube group; or carrying out high-pressure gas impact crushing on the carbon nano tubes by a jet mill, so as to form the powder formed by the carbon nano tube group. The spherical carbon nanotube group can be used as a conductive agent or heat-conducting agent of a lithium battery, a high polymer material and paint. The spherical carbon nanotube group disclosed by the invention is simple in preparation process, stable and uniform in property, and easy to form a conductive network, has excellent dispersing performance, and can be directly added to a matrix material.
Description
[technical field]
The present invention relates to carbon nanotube, particularly relate to a kind of Spherical Carbon nanotube group and its production and use.
[background technology]
Carbon nanotube is outstanding conductive agent, and its size is generally 2～100 nanometers, and length can reach 10～50 microns.Carbon nanotube not only can play the effect of wire in conductive network, but also has the high magnification characteristic of electrostatic double layer effect and ultracapacitor.Meanwhile, the heat radiation when heat conductivility that carbon nanotube is good is conducive to battery charging and discharging, reduces the polarization of battery, improves the high temperature performance of battery, extends the life of a cell.In macromolecular material and coating, paint, add 1/10 carbon nanotube of amounts of carbon black, can reach the conduction state of carbon black.
The people such as Sheem (Journal of Power Sources2006,158,1425-1430) contrast multi-walled carbon nano-tubes and the impact on lithium ion battery of traditional graphitized carbon black, found that, no matter, in electrical capacity and cycle index, multi-walled carbon nano-tubes is all significantly better than graphitized carbon black.But, due to carbon nanotube stronger Van der Waals force each other, make to be mutually intertwined between carbon nanotube, be difficult to be distributed in material equably, thereby affected the performance of the physicals of carbon nanotube own.Therefore, how to prepare the carbon nanotube product that is easy to disperse and become a major obstacle that limits its commercial application.At present, the scattering problem of solution carbon nanotube mainly contains chemistry and two kinds of methods of physics.Wherein, mostly chemical process is to be oxidized by strong acid.Due to this body structure of strong acid meeting destroying carbon nanometer tube, make the performance of carbon nanotube weaken or lose efficacy, and due to complicated operation, easily to factors such as environments, make it to be difficult to realize suitability for industrialized production.The materials such as current macromolecular material, coating, paint are mainly applied this type of carbon nanotube.Physical method is to carry out wet grinding processing by sand mill, is prepared into electrocondution slurry, although dispersion effect is better, but the amount of the dispersion agent wherein adding affects greatly the performance of conductivity, make it resistance and become large, and the quality guaranteed period is short, lithium cell is produced main this series products of application at present.
[summary of the invention]
The present invention is intended to address the above problem, and provides a kind of preparation process simple, has good dispersing property, can directly add in body material and without adding dispersion agent, and stable in properties homogeneous, easily forms the Spherical Carbon nanotube group of network.
The present invention also aims to provide a kind of preparation method of Spherical Carbon nanotube group.
The present invention also aims to provide the purposes of described Spherical Carbon nanotube group.
For achieving the above object, the invention provides a kind of Spherical Carbon nanotube group, this Spherical Carbon nanotube group is that carbon nanotube dust is placed in to rotating equipment, making the carbon nanotube of unordered winding be agglomerated into the group interweaving in order by rotation forms, the particle diameter of described group is 0.1～3 micron, is shaped as spherical or clavate.
Described spherical carbon nanotube group is spheroidal or elliposoidal.
Described rotating equipment is shredder or micronizer mill.
Described shredder is ball mill or sand mill.
The present invention also provides the preparation method of described Spherical Carbon nanotube group, and the method comprises the steps:
A, carbon nanotube and grinding medium are placed in to shredder in the ratio of 0.1～1:0.1～10;
B, CNT (carbon nano-tube) is ground 1 minute～20 hours with the linear velocity of 2～50 meter per seconds with the shredder that has a grinding medium, forming is 0.1～3 micron by multiple particle diameters, is shaped as the powder that the carbon nanotube group of spherical or clavate forms.
In another program of the present invention, the preparation method of described Spherical Carbon nanotube group comprises the steps:
C, the carbon nanotube that accounts for grinding plant volume 30～90% is placed in to the shredder of non-grinding medium;
D, CNT (carbon nano-tube) is ground 1 minute～20 hours with the shredder of non-grinding medium, the linear velocity of described shredder is 5～50 meter per seconds, and forming is 0.1～3 micron by multiple particle diameters, is shaped as the powder that the carbon nanotube group of spherical or clavate forms.
In another scheme of the present invention, the preparation method of described Spherical Carbon nanotube group comprises the steps
E, carbon nanotube is sent into micronizer mill, the input speed of carbon nanotube is 1～100 kg/hour, and charging air pressure is 0.7～1.0Mpa;
F, carbon nanotube is carried out to discharging after impact grinding with the high pressure gas of the airshed of 2～10 cubes ms/h in micronizer mill, obtaining by multiple particle diameters is 0.1～3 micron, is shaped as the powder that the carbon nanotube group of spherical or clavate forms.
Described grinding medium is material and measure-alike Single Medium, or material and the different blending agent of size, and wherein, the particle diameter of described Single Medium is 0.1～50mm.
Grinding medium is one or more the combination in zirconium silicate pearl, zirconium dioxide pearl, titanium dioxide aluminium pill or steel ball.
The purposes of the Spherical Carbon nanotube group described in the present invention also provides, this Spherical Carbon nanotube group can be used as conductive agent, the thermal conducting agent of lithium cell, macromolecular material, coating, paint.
Contribution of the present invention is, it is poor that it efficiently solves the carbon nanotube dispersed existing in prior art, needs strong acid oxidation and uses the problems such as dispersion agent dispersion.Spherical Carbon nanotube group material of the present invention is owing to being agglomerated into spherule, thereby there is good dispersing characteristic, it can directly add in body material, thereby reduce or without add dispersion agent, thereby greatly expand its range of application, optimize and improved production technique, and remarkable save energy.The ball-like structure of carbon nanotube group of the present invention is easy to form conductive network, therefore can better bring into play the performance of carbon nanotube.In actual applications, this carbon nanotube group directly can be made lithium cell electrocondution slurry through short period of time high-speed stirring, has therefore greatly reduced jitter time.Preparation method's technique of the present invention is simple, easy to implement and large-scale promotion application, and low production cost.Carbon nanotube group of the present invention is of many uses, and it can be applicable in lithium cell, macromolecular material, coating, paint, as can homodisperse conductive agent and thermal conducting agent.
[accompanying drawing explanation]
Fig. 1 is the powder microscan figure by there being the prepared carbon nanotubes group of medium milling equipment.
Fig. 2 is by the powder microscan figure without the prepared carbon nanotubes group of medium milling equipment.
Fig. 3 is the powder microscan figure by the prepared carbon nanotubes group of micronizer mill.
Fig. 4 is the electrocondution slurry microscan figure being made up of carbon nanotube group.
[embodiment]
The following example is further explanation of the present invention, and the present invention is not constituted any limitation.
Carbon nanotube in the present invention can be any in known Single Walled Carbon Nanotube or multi-walled carbon nano-tubes.
Embodiment 1
It is 600 grams by the multi-walled carbon nano-tubes of 160 grams and weight, diameter is that zirconium pearl and the weight of 5 millimeters is 600 grams, diameter is that the blending agent of the zirconium pearl of 1 millimeter is put into the planetary ball mill tank of 3 liters simultaneously, the linear velocity of ball mill is 5 meter per seconds, milling time 5 hours, obtaining containing multiple diameters is 1～3 micron, is shaped as the powder of axiolitic carbon nanotube group, in powder, the volume content of carbon nanotube group is 30～40%, and the microscan figure of this carbon nanotube-based cooking starch body as shown in Figure 1.
Embodiment 2
It is 600 grams by the multi-walled carbon nano-tubes of 160 grams and weight, diameter is that zirconium pearl and the weight of 5 millimeters is 600 grams, diameter is that the blending agent of the zirconium pearl of 1 millimeter is put into the planetary ball mill tank of 3 liters simultaneously, the linear velocity of ball mill is 5 meter per seconds, milling time 19 hours, obtaining containing multiple diameters is 1～3 micron, is shaped as the powder of axiolitic carbon nanotube group, and in powder, the volume content of carbon nanotube group is 50～60%.
Embodiment 3
The multi-walled carbon nano-tubes and the weight that are 300 milliliters by volume are 400 grams, diameter is that the zirconium pearl of the Single Medium of 1 millimeter is put into the sand mill tank of 1 liter, wherein the dispersion impeller of sand mill and the gap of cylindrical shell are 5 millimeters, the linear velocity of dispersion impeller is 15 meter per seconds, milling time 1 hour, obtaining containing multiple diameters is 1～3 micron, be shaped as the powder of axiolitic carbon nanotube group, in powder, the volume content of carbon nanotube group is 30～40%, and the microscan figure of this carbon nanotube-based cooking starch body as shown in Figure 2.
The multi-walled carbon nano-tubes and the weight that are 300 milliliters by volume are 400 grams, diameter is that the zirconium pearl of the Single Medium of 1 millimeter is put into the sand mill tank of 1 liter, wherein the dispersion impeller of sand mill and the gap of cylindrical shell are 5 millimeters, dispersion impeller linear velocity is 25 meter per seconds, milling time 6 hours, obtaining containing multiple diameters is 1～3 micron, is shaped as the powder of axiolitic carbon nanotube group, and in powder, the volume content of carbon nanotube group is 60～70%.
Embodiment 5
The multi-walled carbon nano-tubes that is 800 milliliters by volume put into 1 liter without medium sand mill tank, wherein the dispersion impeller of sand mill and the gap of cylindrical shell are 3 millimeters, dispersion impeller linear velocity is 50 meter per seconds, milling time 3 minutes, obtaining containing multiple diameters is 1～3 micron, be shaped as the powder of axiolitic carbon nanotube group, in powder, the volume content of carbon nanotube group is 70～80%.
Embodiment 6
The multi-walled carbon nano-tubes that is 800 milliliters by volume put into 1 liter without medium sand mill tank, wherein the dispersion impeller of sand mill and the gap of cylindrical shell are 5 millimeters, dispersion impeller linear velocity is 50 meter per seconds, milling time 10 minutes, obtaining containing multiple diameters is 1～3 micron, be shaped as the powder of axiolitic carbon nanotube group, in powder, the volume content of carbon nanotube group is 80～90%.
Embodiment 7
Multi-walled carbon nano-tubes is sent in the micronizer mill of stream pressure 0.8Mpa, the input speed of micronizer mill is 40 kgs/hour; By carbon nanotube in micronizer mill with, airshed is that the high pressure gas of 10 cubes ms/h carry out impact grinding 0.5 hour, obtaining containing multiple diameters is 1～3 micron, be shaped as the powder of axiolitic carbon nanotube group, in powder, the volume content of carbon nanotube group is 40～50%, and the microscan figure of this carbon nanotube-based cooking starch body as shown in Figure 3.
Embodiment 8
Prepared carbon nanotube group in embodiment 1,2,3,4,5,6,7 is mixed mutually by the weight ratio of 5:95 with solvent N～methyl-2-pyrrolidone respectively in stirred vessel, the linear velocity of stirred vessel is 5 meter per seconds, at the uniform velocity stir 5 minutes, make respectively sequence number and be 1,2,3,4,5,6,7 electrocondution slurry, coating is prepared into electrode slice, then survey its resistivity, and relatively resistance size and dispersing uniformity, data are as table 1:
Table 1
Comparative example 1
Common carbon nanotube without this law processing is mixed mutually by the weight ratio of 5:95 with solvent N～methyl-2-pyrrolidone in stirred vessel, and the linear velocity of stirred vessel is 5 meter per seconds, at the uniform velocity stirs 5 minutes, make electrocondution slurry, coating is prepared into electrode slice, then surveys its resistivity, the results are shown in Table 1.
Above-mentioned test result shows, the in the situation that of same dispersing technology, the little and narrow range of the resistivity of carbon nanotube group of the present invention, illustrate that dispersion state is even, is easier to dispersion than untreated carbon nanotube.
Comparative example 2:
Common carbon nanotube without this law processing is mixed mutually by the weight ratio of 3:97 with base material polyethylene in stirred vessel, and through mill the temperature of 165 ℃ mixing 5 minutes, pulling-on piece was surveyed surface resistivity, the results are shown in Table 2.
Table 2
Above-mentioned test result shows, the in the situation that of same dispersing technology, the little and narrow range of the resistivity of carbon nanotube group of the present invention, illustrate that dispersion state is even, is easier to dispersion than untreated carbon nanotube.
Although the present invention is disclosed by above embodiment, protection scope of the present invention is not limited to this, is not departing under the condition of the present invention's design, and distortion, the replacement etc. that above each member is done all will fall within the scope of claim of the present invention.
Claims (10)
1. a Spherical Carbon nanotube group, it is characterized in that, this Spherical Carbon nanotube group is that carbon nanotube dust is placed in to rotating equipment, making the carbon nanotube of unordered winding be agglomerated into the group interweaving in order by rotation forms, the particle diameter of described group is 0.1～3 micron, is shaped as spherical or clavate.
2. Spherical Carbon nanotube group as claimed in claim 1, is characterized in that, described spherical carbon nanotube group is spheroidal or elliposoidal.
3. Spherical Carbon nanotube group as claimed in claim 1, is characterized in that, described rotating equipment is shredder or micronizer mill.
4. Spherical Carbon nanotube group as claimed in claim 3, is characterized in that, described shredder is ball mill or sand mill.
5. a method of preparing Spherical Carbon nanotube group described in claim 1, is characterized in that, the method comprises the steps:
A, carbon nanotube and grinding medium are placed in to shredder in the ratio of 0.1～1:0.1～10;
B, CNT (carbon nano-tube) is ground 1 minute～20 hours with the linear velocity of 2～50 meter per seconds with the shredder that has a grinding medium, forming is 0.1～3 micron by multiple particle diameters, is shaped as the powder that the carbon nanotube group of spherical or clavate forms.
6. a method of preparing Spherical Carbon nanotube group described in claim 1, is characterized in that, the method comprises the steps:
C, the carbon nanotube that accounts for grinding plant volume 30～90% is placed in to the shredder of non-grinding medium;
D, CNT (carbon nano-tube) is ground 1 minute～20 hours with the shredder of non-grinding medium, the linear velocity of described shredder is 5～50 meter per seconds, and forming is 0.1～3 micron by multiple particle diameters, is shaped as the powder that the carbon nanotube group of spherical or clavate forms.
7. a method of preparing Spherical Carbon nanotube group described in claim 1, is characterized in that, the method comprises the steps
E, carbon nanotube is sent into micronizer mill, the input speed of carbon nanotube is 1～100 kg/hour, and charging air pressure is 0.7～1.0Mpa;
F, carbon nanotube is carried out to discharging after impact grinding with the high pressure gas of the airshed of 2～10 cubes ms/h in micronizer mill, obtaining by multiple particle diameters is 0.1～3 micron, is shaped as the powder that the carbon nanotube group of spherical or clavate forms.
8. method as claimed in claim 5, is characterized in that, described grinding medium is material and measure-alike Single Medium, or material and the different blending agent of size, and wherein, the particle diameter of described Single Medium is 0.1～50mm.
9. method as claimed in claim 8, is characterized in that, described grinding medium is one or more the combination in zirconium silicate pearl, zirconium dioxide pearl, titanium dioxide aluminium pill or steel ball.
10. Spherical Carbon nanotube group claimed in claim 1 is as the conductive agent of lithium cell, macromolecular material, coating, paint, the application of thermal conducting agent.
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| CN107994232A (en) * | 2017-11-23 | 2018-05-04 | 深圳市清新电源研究院 | A kind of lithium-sulfur cell carrier material |
| CN110684392A (en) * | 2019-09-29 | 2020-01-14 | 佛山宜可居新材料有限公司 | Multi-wall carbon nano tube composite conductive material, preparation method and product thereof |
| CN114068933A (en) * | 2021-10-28 | 2022-02-18 | 诺瑞(深圳)新技术有限公司 | Carbon nano tube conductive agent and preparation method and application thereof |
| CN114361427A (en) * | 2021-12-28 | 2022-04-15 | 深圳市纳米港有限公司 | Method for coating silicon cathode material with carbon nano tube |
| CN115304056A (en) * | 2022-07-21 | 2022-11-08 | 青岛泰联新材料有限公司 | Granular carbon nano tube and preparation method thereof |
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| CN115304056A (en) * | 2022-07-21 | 2022-11-08 | 青岛泰联新材料有限公司 | Granular carbon nano tube and preparation method thereof |
| CN115304056B (en) * | 2022-07-21 | 2024-01-26 | 青岛泰联新材料有限公司 | Granular carbon nano tube and preparation method thereof |
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