CN113600074A - Preparation method of uniform carbon nanotube solution - Google Patents
Preparation method of uniform carbon nanotube solution Download PDFInfo
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- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 99
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 97
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000002270 dispersing agent Substances 0.000 claims abstract description 48
- 238000003756 stirring Methods 0.000 claims abstract description 34
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 27
- 238000000227 grinding Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 12
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 10
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 8
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 claims description 2
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 claims description 2
- 229960003237 betaine Drugs 0.000 claims description 2
- DVEKCXOJTLDBFE-UHFFFAOYSA-N n-dodecyl-n,n-dimethylglycinate Chemical compound CCCCCCCCCCCC[N+](C)(C)CC([O-])=O DVEKCXOJTLDBFE-UHFFFAOYSA-N 0.000 claims description 2
- 238000007789 sealing Methods 0.000 description 10
- 239000002131 composite material Substances 0.000 description 7
- 239000011156 metal matrix composite Substances 0.000 description 7
- 239000006185 dispersion Substances 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 239000011229 interlayer Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 230000002787 reinforcement Effects 0.000 description 5
- 238000003917 TEM image Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000002035 prolonged effect Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000004098 selected area electron diffraction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
- C22C2026/002—Carbon nanotubes
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Abstract
The invention discloses a preparation method of a uniform carbon nanotube solution, which is implemented according to the following steps: step 1, weighing a multi-walled carbon nanotube, a zwitterionic dispersant, an isopropanol solution and a zirconia grinding ball; step 2, adding the zwitterion dispersing agent weighed in the step 1 into a container, then adding an isopropanol solution, and stirring to obtain a zwitterion dispersing solution A; step 3, adding the multiwalled carbon nanotubes weighed in the step 1 into the zwitterion dispersible solution A, and stirring to obtain a solution B; step 4, performing ultrasonic dispersion on the solution B to obtain a solution C; and 5, adding the zirconium oxide grinding balls weighed in the step 1 into the solution C, and then vibrating through a vibrating powder mixer to obtain a uniform carbon nano tube solution. The method solves the problems that the CNTs in the prior art are agglomerated and are easy to form weak phases.
Description
Technical Field
The invention belongs to the technical field of solution preparation, and relates to a preparation method of a uniform carbon nanotube solution.
Background
Metal Matrix Composites (MMCs) are Composites in which the Matrix component is a Metal. Early MMCs generally employed continuous long fibers as reinforcement, such as carbon fibers, boron fibers, SiC fibers, and the like. The addition of the long fiber can improve the properties of the composite material in various aspects such as strength, modulus, wear resistance, heat conduction, fatigue resistance, high temperature resistance and the like, and becomes a very critical special material in the fields of advanced weapons, aerospace and the like. However, long fiber-reinforced MMCs have little plastic deformability, and the high manufacturing costs, excessive processing difficulties, and significant anisotropy make them useful only in certain applications. The Carbon Nanotubes (CNTs) are fullerene tubes with diameters of 0.3nm to dozens of nanometers and lengths of dozens of micrometers, the tube walls are made of carbon with a hexagonal structure, and the CNTs are single-layer (single-wall carbon nanotubes) or multi-layer (multi-wall carbon nanotubes). The carbon nano tube has excellent mechanical property and physical property. However, the carbon nano tube has a nano-scale tube diameter, a large specific surface area and a high specific surface energy, so that the carbon nano tube has a strong agglomeration tendency, and in the process of preparing the carbon nano tube reinforced metal matrix composite material, the key step is to uniformly and dispersedly disperse the carbon nano tube in a metal matrix or to distribute the carbon nano tube in a bundle shape, so that the reinforcing phase is prevented from agglomerating in the matrix to form a weak phase.
Disclosure of Invention
The invention aims to provide a preparation method of a uniform carbon nanotube solution, which solves the problems that CNTs in the prior art are agglomerated and are easy to form weak phases.
The technical scheme adopted by the invention is that the preparation method of the uniform carbon nanotube solution is implemented according to the following steps:
step 1, weighing a multi-walled carbon nanotube, a zwitterionic dispersant, an isopropanol solution and a zirconia grinding ball;
step 2, adding the zwitterion dispersing agent weighed in the step 1 into a container, then adding an isopropanol solution, and stirring to obtain a zwitterion dispersing solution A;
step 3, adding the multiwalled carbon nanotubes weighed in the step 1 into the zwitterion dispersible solution A, and stirring to obtain a solution B;
step 4, performing ultrasonic dispersion on the solution B to obtain a solution C;
and 5, adding the zirconium oxide grinding balls weighed in the step 1 into the solution C, and then vibrating through a vibrating powder mixer to obtain a uniform carbon nano tube solution.
The invention is also characterized in that:
the mass ratio of the multiwalled carbon nanotube, the zwitterionic dispersant and the isopropanol solution weighed in the step 1 is 0.1-2.0:0-2.5:50-500, and the number of the zirconia grinding balls is 5-10.
The zwitterionic dispersant in the step 1 is dodecyl dimethyl betaine or betaine type zwitterionic dispersant.
And in the step 2, stirring, namely, placing the container on a magnetic stirrer, and stirring the solution by using a magnetic rod.
In the step 2, the rotating speed of the magnetic stirrer is 400-.
And 3, stirring by using a magnetic stirrer, wherein the rotating speed of the magnetic stirrer is 300-.
In the step 4, the temperature of ultrasonic dispersion is 5-18 ℃, the time is 0.5-1.5h, and the frequency is 39-45 KHz.
In the step 5, the vibration frequency of the vibration powder mixer is 40-50Hz, and the time is 0.5-1 h.
The invention has the beneficial effects that: the method prepares the uniform CNTs solution by uniformly dispersing the CNTs in the isopropanol solution, the solution can be directly used for wet ball milling (SBM) in the preparation process of the MMCs, and the dispersed CNTs still have higher strength (60-110 GPa) and rigidity and lower density (2.1 g/cm)3) The metal matrix has higher strength, larger length-diameter ratio (100-1000) and higher heat conduction capacity (3000-6000W/m.K), so that the density can be reduced while the metal matrix is enhanced, the weight reduction effect is further improved, and the CNTs are more widely applied to MMCs.
Drawings
FIG. 1 is a flow chart of a method for preparing a uniform Carbon Nanotube (CNTs) solution according to the present invention;
FIG. 2 is a bright field TEM image of a sample obtained in example 1 of the present invention;
FIG. 3 is a bright field TEM image of a sample obtained in example 2 of the present invention;
FIG. 4 is a bright field TEM image of a sample obtained in example 3 of the present invention;
FIG. 5 is a bright field TEM image of a sample obtained in example 4 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of a uniform carbon nanotube CNTs solution, which is specifically implemented according to the following steps as shown in figure 1:
step 1, weighing multi-wall CNTs, a zwitterionic dispersant, an isopropanol solution and zirconia grinding balls, wherein the mass ratio of the multi-wall CNTs to the zwitterionic dispersant to the isopropanol solution is 0.1-2.0:0-2.5:50-500, and the number of the zirconia grinding balls is 5-10;
step 2, adding the zwitterionic dispersing agent weighed in the step 1 into a clean beaker, wherein the beaker needs to be clean and free of moisture, adding the isopropanol solution weighed in the step 1, the purity of the isopropanol solution is more than 99.9%, placing the beaker on a magnetic stirrer, setting operation parameters of the magnetic stirrer, wherein the rotating speed is 400-600r/min, the operation time is 10-20min, fully stirring the solution by using a magnetic rod to completely dissolve the zwitterionic dispersing agent, and if the dispersing agent is not completely dissolved, prolonging the stirring time until all the dispersing agent is completely dissolved to obtain a zwitterionic dispersing solution A;
step 3, adding the multi-wall CNTs weighed in the step 1 into the zwitter-ion dispersible solution A obtained in the step 2, setting operation parameters for a magnetic stirrer, wherein the operation speed is 300-;
step 4, putting the solution B obtained in the step 3 into an ultrasonic machine, setting working parameters of the ultrasonic machine to be 5-18 ℃, setting the time to be 0.5-1.5h and setting the working frequency to be 39-45KHz, and performing ultrasonic dispersion on the solution B to obtain a solution C;
and 5, transferring the solution C obtained in the step 4 into a bottle sealing bottle special for a vibration powder mixer, adding 5-10 zirconium oxide grinding balls with the diameter of 10mm weighed in the step 1, sealing the bottle, mounting the sealed bottle on a three-dimensional vibration powder mixer for inputting vibration energy, wherein the vibration powder mixer has the working parameters of vibration frequency of 40-50Hz and working time of 0.5-1h, and obtaining a solution D after vibration is finished, namely the uniform CNTs solution.
Example 1
A preparation method of a uniform Carbon Nanotube (CNTs) solution specifically comprises the following steps:
step 1, weighing required raw materials
Weighing 0.3g of multi-wall CNTs, 0.3g of zwitterionic dispersant, 30g of isopropanol solution and 5 zirconia grinding balls, wherein the mass ratio of the multi-wall CNTs to the zwitterionic dispersant to the isopropanol solution is 1: 1: 100, the number of zirconia grinding balls is 5;
step 2, dissolving the zwitterionic dispersant
And (2) adding 0.3g of the zwitterionic dispersant weighed in the step (1) into a clean beaker, wherein the beaker needs to be clean and free of moisture, and then adding 30g of the isopropanol solution weighed in the step (1), wherein the purity of the isopropanol solution is more than 99.9%. And (3) placing the beaker on a magnetic stirrer, setting the operating parameters of the magnetic stirrer, wherein the rotating speed is 500r/min, the operating time is 10min, and fully stirring the solution by using a magnetic rod to completely dissolve the zwitterion dispersing agent. If the dispersant is not completely dissolved, the stirring time is prolonged until all the dispersant is completely dissolved. Obtaining a zwitterion dispersing solution A;
step 3, adding and dispersing CNTs
And (2) adding 0.3g of multi-wall CNTs weighed in the step (1) into the zwitter-ion dispersible solution A obtained in the step (2), setting operation parameters for a magnetic stirrer, wherein the operation speed is 400r/min, the operation time is 30min, and the cup mouth of a beaker needs to be sealed in the process so as to prevent the solution from volatilizing in the stirring process. Fully stirring to obtain a solution B;
step 4, ultrasonically dispersing the CNTs solution
Putting the solution B obtained in the step (3) into an ultrasonic machine, setting working parameters of the ultrasonic machine to be 10 ℃, 30min and 39KHz of working frequency, and performing ultrasonic dispersion on the solution B to obtain a solution C;
step 5, inputting energy of the vibrating powder mixer
And (3) transferring the solution C obtained in the step (4) into a bottle sealing bottle special for a vibration powder mixer, adding 5 zirconium oxide grinding balls with the diameter of 10mm weighed in the step (1), sealing the bottle, mounting the bottle on a three-dimensional vibration powder mixer for inputting vibration energy, wherein the working parameters of the vibration powder mixer are vibration frequency of 40Hz and working time of 30min, and obtaining a solution D which is a uniform CNTs solution after vibration is finished.
The high-resolution Transmission Electron Microscope (TEM) bright field observation of the uniform Carbon Nanotube (CNTs) solution prepared in the embodiment 1 of the invention is shown in FIG. 2, and the result shows that CNTs are multi-wall carbon nanotubes, an obvious tube wall hollow structure can be seen, no obvious defect is seen, the diameter is about 10-30 nm, and the interlayer spacing is 0.36 nm. The TEM selected area electron diffraction pattern presents amorphous ring characteristics, which shows that the carbon nano tube has complete structure and uniform dispersion and meets the requirement of preparing composite materials as a reinforcement.
Example 2
A preparation method of a uniform Carbon Nanotube (CNTs) solution specifically comprises the following steps:
step 1, weighing required raw materials
Weighing 0.6g of multi-wall CNTs, 0.3g of zwitterionic dispersant, 60g of isopropanol solution and 7 zirconia grinding balls, wherein the mass ratio of the multi-wall CNTs to the zwitterionic dispersant to the isopropanol solution is 2: 1: 200, the number of the zirconia grinding balls is 7;
step 2, dissolving the zwitterionic dispersant
And (2) adding 0.3g of the zwitterionic dispersant weighed in the step (1) into a clean beaker, wherein the beaker needs to be clean and free of moisture, and then adding 60g of the isopropanol solution weighed in the step (1), wherein the purity of the isopropanol solution is more than 99.9%. And (3) placing the beaker on a magnetic stirrer, setting the operating parameters of the magnetic stirrer, wherein the rotating speed is 500r/min, the operating time is 15min, and fully stirring the solution by using a magnetic rod to completely dissolve the zwitterion dispersing agent. If the dispersant is not completely dissolved, the stirring time is prolonged until all the dispersant is completely dissolved. Obtaining a zwitterion dispersing solution A;
step 3, adding and dispersing CNTs
And (2) adding 0.6g of multi-wall CNTs weighed in the step (1) into the zwitter-ion dispersible solution A obtained in the step (2), setting operation parameters for a magnetic stirrer, wherein the operation speed is 400r/min, the operation time is 45min, and the cup mouth of a beaker needs to be sealed in the process so as to prevent the solution from volatilizing in the stirring process. Fully stirring to obtain a solution B;
step 4, ultrasonically dispersing the CNTs solution
Putting the solution B obtained in the step (3) into an ultrasonic machine, setting the working parameters of the ultrasonic machine to be 10 ℃, 80min and 40KHz of working frequency, and performing ultrasonic dispersion on the solution B to obtain a solution C;
step 5, inputting energy of the vibrating powder mixer
And (3) transferring the solution C obtained in the step (4) into a bottle sealing bottle special for a vibration powder mixer, adding 7 zirconium oxide grinding balls with the diameter of 10mm weighed in the step (1), sealing the bottle, mounting the bottle on a three-dimensional vibration powder mixer for inputting vibration energy, wherein the working parameters of the vibration powder mixer are vibration frequency of 40Hz and working time of 50min, and obtaining a solution D which is a uniform CNTs solution after vibration is finished.
The high-resolution Transmission Electron Microscope (TEM) bright field observation of the uniform Carbon Nanotube (CNTs) solution prepared in example 2 of the invention is shown in FIG. 3, and the result shows that CNTs are multi-walled carbon nanotubes, and can be seen to have an obvious tube wall hollow structure without obvious defects, the diameter is about 10-30 nm, and the interlayer spacing is 0.28 nm. The TEM selected area electron diffraction pattern presents amorphous ring characteristics, which shows that the carbon nano tube has complete structure and uniform dispersion and meets the requirement of preparing composite materials as a reinforcement.
Example 3
A preparation method of a uniform Carbon Nanotube (CNTs) solution specifically comprises the following steps:
step 1, weighing required raw materials
Weighing 0.6g of multi-wall CNTs, 0.6g of zwitterionic dispersant, 90g of isopropanol solution and 8 zirconia grinding balls, wherein the mass ratio of the multi-wall CNTs to the zwitterionic dispersant to the isopropanol solution is 1: 1: 150, the number of the zirconia grinding balls is 8;
step 2, dissolving the zwitterionic dispersant
And (2) adding 0.6g of the zwitterionic dispersant weighed in the step (1) into a clean beaker, wherein the beaker needs to be clean and free of moisture, and then adding 90g of the isopropanol solution weighed in the step (1), wherein the purity of the isopropanol solution is more than 99.9%. And (3) placing the beaker on a magnetic stirrer, setting the operating parameters of the magnetic stirrer, wherein the rotating speed is 500r/min, the operating time is 15min, and fully stirring the solution by using a magnetic rod to completely dissolve the zwitterion dispersing agent. If the dispersant is not completely dissolved, the stirring time is prolonged until all the dispersant is completely dissolved. Obtaining a zwitterion dispersing solution A;
step 3, adding and dispersing CNTs
And (2) adding 0.6g of multi-wall CNTs weighed in the step (1) into the zwitter-ion dispersible solution A obtained in the step (2), setting operation parameters for a magnetic stirrer, wherein the operation speed is 400r/min, the operation time is 50min, and the cup mouth of a beaker needs to be sealed in the process so as to prevent the solution from volatilizing in the stirring process. Fully stirring to obtain a solution B;
step 4, ultrasonically dispersing the CNTs solution
Putting the solution B obtained in the step (3) into an ultrasonic machine, setting working parameters of the ultrasonic machine to be 10 ℃, 60min and 42KHz of working frequency, and performing ultrasonic dispersion on the solution B to obtain a solution C;
step 5, inputting energy of the vibrating powder mixer
And (3) transferring the solution C obtained in the step (4) into a bottle sealing bottle special for a vibration powder mixer, adding 8 zirconium oxide grinding balls with the diameter of 10mm weighed in the step (1), sealing the bottle, mounting the bottle on a three-dimensional vibration powder mixer for inputting vibration energy, wherein the working parameters of the vibration powder mixer are vibration frequency of 50Hz and working time of 30min, and obtaining a solution D which is a uniform CNTs solution after vibration is finished.
The high-resolution Transmission Electron Microscope (TEM) bright field observation of the uniform Carbon Nanotube (CNTs) solution prepared in the embodiment 3 of the invention is shown in FIG. 4, and the result shows that CNTs are multi-wall carbon nanotubes, an obvious tube wall hollow structure can be seen, no obvious defect is seen, the diameter is about 10-30 nm, and the interlayer spacing is 0.35 nm. The TEM selected area electron diffraction pattern presents amorphous ring characteristics, which shows that the carbon nano tube has complete structure and uniform dispersion and meets the requirement of preparing composite materials as a reinforcement.
Example 4
A preparation method of a uniform Carbon Nanotube (CNTs) solution specifically comprises the following steps:
step 1, weighing required raw materials
Weighing 0.3g of multi-wall CNTs, 0.6g of zwitterionic dispersant, 120g of isopropanol solution and 10 zirconia grinding balls, wherein the mass ratio of the multi-wall CNTs to the zwitterionic dispersant to the isopropanol solution is 1: 2: 400, the number of the zirconia grinding balls is 10;
step 2, dissolving the zwitterionic dispersant
And (2) adding 0.6g of the zwitterionic dispersant weighed in the step (1) into a clean beaker, wherein the beaker needs to be clean and free of moisture, and then adding 120g of the isopropanol solution weighed in the step (1), wherein the purity of the isopropanol solution is more than 99.9%. And (3) placing the beaker on a magnetic stirrer, setting the operating parameters of the magnetic stirrer, wherein the rotating speed is 500r/min, the operating time is 20min, and fully stirring the solution by using a magnetic rod to completely dissolve the zwitterion dispersing agent. If the dispersant is not completely dissolved, the stirring time is prolonged until all the dispersant is completely dissolved. Obtaining a zwitterion dispersing solution A;
step 3, adding and dispersing CNTs
And (2) adding 0.3g of multi-wall CNTs weighed in the step (1) into the zwitter-ion dispersible solution A obtained in the step (2), setting operation parameters for a magnetic stirrer, wherein the operation speed is 400r/min, the operation time is 60min, and the cup mouth of a beaker needs to be sealed in the process so as to prevent the solution from volatilizing in the stirring process. Fully stirring to obtain a solution B;
step 4, ultrasonically dispersing the CNTs solution
Putting the solution B obtained in the step (3) into an ultrasonic machine, setting the working parameters of the ultrasonic machine to be 10 ℃, the time to be 150min and the working frequency to be 45KHz, and performing ultrasonic dispersion on the solution B to obtain a solution C;
step 5, inputting energy of the vibrating powder mixer
And (3) transferring the solution C obtained in the step (4) into a bottle sealing bottle special for a vibration powder mixer, adding 10 zirconium oxide grinding balls with the diameter of 10mm weighed in the step (1), sealing the bottle, mounting the bottle on a three-dimensional vibration powder mixer for inputting vibration energy, wherein the working parameters of the vibration powder mixer are vibration frequency of 50Hz and working time of 40min, and obtaining a solution D which is a uniform CNTs solution after vibration is finished.
The high-resolution Transmission Electron Microscope (TEM) bright field observation of the uniform Carbon Nanotube (CNTs) solution prepared in the embodiment 4 of the invention is shown in FIG. 5, and the result shows that CNTs are multi-wall carbon nanotubes, an obvious tube wall hollow structure can be seen, no obvious defect is seen, the diameter is about 10-30 nm, and the interlayer spacing is 0.34 nm. The TEM selected area electron diffraction pattern presents amorphous ring characteristics, which shows that the carbon nano tube has complete structure and uniform dispersion and meets the requirement of preparing composite materials as a reinforcement.
The dispersion effect of the uniform Carbon Nanotube (CNTs) solution prepared by the present invention is further illustrated by experiments below.
Four samples were taken:
firstly, the uniform Carbon Nanotube (CNTs) solution prepared in example 1 of the present invention is sample 1;
(II) the difference from the embodiment 1 of the invention is only that in the step 1, 0.6g of CNTs is weighed, 60g of isopropanol is weighed, 7 grinding balls are weighed, the stirring time in the step 2 is 15min, the stirring time in the step 3 is 45min, the ultrasonic frequency in the step 4 is 40KHz, the ultrasonic time is 80min, the operation time of the vibration powder mixer in the step 5 is 30min, the other contents are the same as the embodiment 1 of the invention, no redundancy is provided, and the obtained uniform Carbon Nanotube (CNTs) solution sample 2 is prepared;
thirdly, the difference from the embodiment 1 of the present invention is only that in the step 1, 0.6g of CNTs, 0.6g of zwitterionic dispersant, 90g of isopropanol, 8 grinding balls, 50min of stirring time in the step 3, 42KHz of ultrasonic frequency in the step 4, 60min of ultrasonic time, 50Hz of vibration frequency of vibration powder mixer in the step 5, 30min of running time, the other contents are the same as those in the embodiment 1 of the present invention, and the description is omitted, so as to prepare the uniform Carbon Nanotube (CNTs) solution sample 3;
(IV) the difference from the embodiment 1 of the invention is only that 0.6g of zwitterionic dispersant, 120g of isopropanol, 10 grinding balls, 20min of stirring time in the step 2, 60min of stirring time in the step 3, 45KHz of ultrasonic frequency in the step 4, 150min of ultrasonic frequency, 50Hz of vibration frequency of a vibration powder mixer in the step 5 and 40min of running time are weighed in the step 1, the other contents are the same as those in the embodiment 1 of the invention, and the description is omitted, so that the obtained uniform Carbon Nanotube (CNTs) solution sample 4 is prepared;
the result shows that the density of CNTs in the TEM is changed along with the content change of the CNTs, the dispersed CNTs have complete structure, obvious tube wall hollow structure can be seen, obvious defects are not seen, the diameter is about 10-30 nm, the interlayer spacing is 0.28-0.36nm, the CNTs have the length of more than 200nm, the dispersion is uniform, and the preparation requirement of the composite material is met.
Claims (8)
1. A preparation method of a uniform carbon nanotube solution is characterized by comprising the following steps:
step 1, weighing a multi-walled carbon nanotube, a zwitterionic dispersant, an isopropanol solution and a zirconia grinding ball;
step 2, adding the zwitterion dispersing agent weighed in the step 1 into a container, then adding an isopropanol solution, and stirring to obtain a zwitterion dispersing solution A;
step 3, adding the multiwalled carbon nanotubes weighed in the step 1 into the zwitterion dispersible solution A, and stirring to obtain a solution B;
step 4, performing ultrasonic dispersion on the solution B to obtain a solution C;
and 5, adding the zirconium oxide grinding balls weighed in the step 1 into the solution C, and then vibrating through a vibrating powder mixer to obtain a uniform carbon nano tube solution.
2. The method for preparing a uniform carbon nanotube solution according to claim 1, wherein the mass ratio of the multiwall carbon nanotubes, the zwitterionic dispersant and the isopropanol solution weighed in the step 1 is 0.1-2.0:0-2.5:50-500, and the number of the zirconia grinding balls is 5-10.
3. The method as claimed in claim 1, wherein the zwitterionic dispersant in step 1 is dodecyl dimethyl betaine or betaine type zwitterionic dispersant.
4. The method of claim 1, wherein the stirring in step 2 is performed by placing the container on a magnetic stirrer and stirring the solution with a magnetic rod.
5. The method as claimed in claim 4, wherein the rotation speed of the magnetic stirrer in step 2 is 400-600r/min, and the operation time is 10-20 min.
6. The method as claimed in claim 1, wherein the step 3 is performed by using a magnetic stirrer, the rotation speed of the magnetic stirrer is 300-.
7. The method for preparing a uniform carbon nanotube solution according to claim 1, wherein the temperature of the ultrasonic dispersion in the step 4 is 5-18 ℃, the time is 0.5-1.5h, and the frequency is 39-45 KHz.
8. The method for preparing a uniform carbon nanotube solution according to claim 1, wherein the vibration frequency of the vibration powder mixer in the step 5 is 40 to 50Hz, and the time is 0.5 to 1 hour.
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