KR102018289B1 - Method for preparation of high concentrated carbon nanotube/graphene dispersion - Google Patents
Method for preparation of high concentrated carbon nanotube/graphene dispersion Download PDFInfo
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- KR102018289B1 KR102018289B1 KR1020150066577A KR20150066577A KR102018289B1 KR 102018289 B1 KR102018289 B1 KR 102018289B1 KR 1020150066577 A KR1020150066577 A KR 1020150066577A KR 20150066577 A KR20150066577 A KR 20150066577A KR 102018289 B1 KR102018289 B1 KR 102018289B1
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Abstract
According to the method for producing a CNT / graphene hybrid carbonaceous material according to the present invention, the graphite is separated into graphene by the high pressure homogenization, and the carbon nanotubes are in an unwrapped form, and at the same time, the carbon nanotubes are uniformly dispersed. As a result, a three-dimensional network is formed between graphene and carbon nanotubes structurally, π-π interaction is reduced between graphene or carbon nanotubes due to structural hindrance, thereby reducing reaggregation. In addition, carbon nanotubes act as a bridge between graphenes, thereby affecting electron migration paths, thereby reducing sheet resistance of graphene, thereby increasing the electrical conductivity of graphene.
Description
According to the present invention, high pressure homogenization is performed to treat carbon nanotubes and graphite together in situ to simultaneously release graphite and unwind carbon nanotubes, and the exfoliated graphene and carbon nanotubes are uniformly dispersed, thereby excellent characteristics. The present invention relates to a method for producing a hybrid carbon nanotube / graphene mixed dispersion.
Carbon-based materials such as graphene and carbon nanotubes have excellent physical properties and are being applied to various fields. In recent years, the development of a hybrid carbon-based material in which the properties of each carbon-based material are combined with each other has been made, and in particular, carbon nanotubes / graphene materials have attracted attention as hybrid-based carbon-based materials.
Graphene is a semimetallic material having a thickness corresponding to a carbon atom layer in an arrangement in which carbon atoms are connected in a hexagonal shape by sp2 bonds in two dimensions. Recently, as a result of evaluating the characteristics of the graphene sheet having one layer of carbon atoms, it has been reported that the electron mobility may exhibit very good electrical conductivity of about 50,000
Carbon nanotube / graphene hybrid carbon-based material, to improve the characteristics of the graphene as described above, carbon nanotubes that can act as a bridge between the graphene has a form that is sufficiently adsorbed on the graphene surface, The electrical conductivity of graphene can be further improved.
The carbon nanotube / graphene hybrid carbon-based material is primarily a mixture of two or more carbon-based materials, but various factors are considered in order for each characteristic to be fully expressed due to the physical and chemical properties of the carbon-based material. Should be. In particular, in the case of a carbon nanotube / graphene hybrid carbon-based material, it is necessary to adsorb the carbon nanotubes uniformly and sufficiently on the graphene surface.
Conventional methods for producing such carbon nanotube / graphene hybrid carbon-based materials include a solution phase method and a solid phase method. In the former case, in order to solve the solubility of each material, there are harsh methods such as acid treatment of strong acids such as Hummner's method and ultrasonic treatment after thermal reduction. However, the method again suffers a restacking problem after the reduction process. In the latter case, the growth conditions are typically controlled by CVD to control the shape and properties of the carbon nanotube / graphene hybrid carbonaceous material. However, this method is not suitable for mass production.
In addition to the entanglement of the carbon nanotubes (entanglement) in addition to the characteristics of the carbon nanotubes are not expressed, carbon nanotubes of the carbon nanotubes / graphene hybrid carbon-based material should be disentangled (disentanglement).
As a conventional method for manufacturing carbon nanotubes in a loose form, there is a method of ball-milling, jet-milling, or ultrasonically treating carbon nanotubes with graphene. However, in the case of the above method, the carbon nanotubes have a small length, but there is a problem in that they are limited in production in a loose form or require too long time.
Therefore, there is a demand for a method capable of producing a carbon nanotube / graphene hybrid carbon-based material with high yield and a simple method. Particularly, in situ, carbon nanotubes and graphite may be treated together to remove graphite and carbon nanotubes. Simultaneous annealing is required to produce a carbon nanotube / graphene mixed dispersion having excellent properties.
The present invention uses a high pressure homogenization, in the process of treating carbon nanotubes and graphite together in situ to proceed with the separation of graphite and unwinding of carbon nanotubes at the same time to produce a carbon nanotube / graphene mixture dispersion having excellent characteristics It is to provide.
In order to solve the above problems, the present invention provides a method for producing a carbon nanotube / graphene mixed dispersion comprising the following steps:
1) preparing a feed solution by mixing graphite and carbon nanotubes; And
2) passing the feed solution through an inlet, an outlet, and a high pressure homogenizer comprising a microchannel connecting the inlet and the outlet and having a diameter of micrometer scale.
The term 'graphite' used in the present invention is a substance also called graphite or quartz, which is a mineral belonging to a hexagonal system having a crystal structure such as crystal, and is black and has a metallic luster. Graphite has a plate-like structure, and one layer of graphite is referred to as 'graphene' to be manufactured in the present invention, and thus graphite becomes a main raw material of graphene production.
In order to peel the graphene from the graphite, it is necessary to apply energy to overcome the π-π interaction between the stacked graphenes. In the present invention, a high pressure homogenization method is used as in
Therefore, in the present invention, as shown in
In addition, in order to express characteristics of the carbon nanotube / graphene hybrid carbon-based material, carbon nanotubes should be uniformly adsorbed on the graphene surface in a disentanglement form. In the present invention, by homogenizing the carbon nanotubes together under high pressure, It is characterized in that the carbon nanotubes are in a loose form and uniformly dispersed carbon nanotubes / graphene mixed dispersion is prepared. Accordingly, when the carbon nanotubes / graphene mixed dispersions are applied to other uses, for example, Carbon nanotubes may be uniformly adsorbed on the graphene surface.
Hereinafter, the present invention will be described in detail step by step.
Graphite And by mixing carbon nanotubes Feed Step of preparing a solution (step 1)
The step is to prepare a feed solution to be applied to the high pressure homogenization of
The carbon nanotubes form a three-dimensional network together with the exfoliated graphene by
In addition to the above, by applying high pressure homogenization of the carbon nanotubes and graphite together, the carbon nanotubes become disentangled, and at the same time, the carbon nanotube / graphene mixed dispersion in which the carbon nanotubes are uniformly dispersed It can manufacture. Accordingly, when the carbon nanotube / graphene mixed dispersion is applied to another application, for example, carbon nanotubes may be uniformly adsorbed onto the graphene surface when dried.
The weight ratio of the graphite and the carbon nanotubes is preferably used in the range of 20: 1 to 1: 1, in which case the dispersion effect and the surface resistance reduction effect of the carbon nanotube / graphene mixed dispersion prepared in
In addition, it is preferable to use a dispersant in order to increase the dispersion of graphite and carbon nanotubes in the feed solution. The dispersant serves to maintain their dispersed state through hydrophobic graphite, interlayer exfoliated graphite, or graphene due to amphiphilicity, and is also called a surfactant in other terms. The dispersant may be used without particular limitation as long as it is used for graphene peeling, and anionic surfactants, nonionic surfactants and cationic surfactants may be used. Specific examples thereof include a low molecular weight pyrene derivative; Cellulose based polymers; Cationic surfactants; Anionic surfactants; Gum arabic; n-dodecyl bD-maltoside; Amphoteric surfactants; Polyvinylpyrrolidone-based polymers; Polyethylene oxide polymers; Ethylene oxide-propylene oxide copolymers; Tannic acid; Or as a mixture of a plurality of polyaromatic hydrocarbon oxides, a mixture containing a polyaromatic hydrocarbon oxide having a molecular weight of 300 to 1000 in an amount of 60% by weight or more.
Preferably, polyvinylpyrrolidone may be used as the dispersant. The "polyvinylpyrrolidone" is a polymer prepared by polymerizing N-vinylpyrrolidone, and refers to a polymer having a weight average molecular weight of 6,000 to 1,300,000 g / mol, and particularly serves as a dispersant of graphene in the present invention. . After graphene is separated from graphite, graphene tends to agglomerate again. The polyvinylpyrrolidone may be attached to the surface of graphene to prevent the graphene from agglomerating again.
The amount of the dispersant is determined by the content of graphite and carbon nanotubes in the feed solution. Preferably, the total weight of graphite and carbon nanotubes and the weight ratio of the dispersant ((graphite + carbon nanotube) / dispersant) is 2.5 It is preferable that it is to 20. Less than 2.5, the content of graphite / carbon nanotubes is too low to reduce the peeling efficiency. If the content of dispersant is too low, the dispersion effect of graphite / carbon nanotubes is less than 20. More preferably, the weight ratio of the total weight of the graphite and carbon nanotubes and the dispersant is 2.5 to 5.
In addition, the concentration of graphite in the feed solution is preferably 0.5 to 10% by weight. Less than 0.5% by weight of the graphite content is too low to reduce the yield on the peeling process, more than 10% by weight of graphite content is so high that the effect of the high pressure homogenization of
In addition, the concentration of carbon nanotubes in the feed solution is preferably 0.1 to 5% by weight. If the concentration of carbon nanotubes is less than 0.1% by weight, the effect of improving the properties of graphene is inferior. If the content is more than 5% by weight, the content of carbon nanotubes is too high, which may inhibit the expression of graphene. Becomes high and the high pressure homogenization effect is inferior.
The solvent of the feed solution is water, N-Methyl-2-pyrrolidone (NMP), acetone, DMF (N, N-dimethylformamide), DMSO (dimethyl sulfoxide), CHP (Cyclohexyl-pyrrolidinone), N12P (N-dodecyl-pyrrolidone) ), Benzyl benzoate, N-Octyl-pyrrolidone (N8P), dimethyl-imidazolidinone (DMEU), cyclohexanone, dimethylacetamide (DMA), N-Methyl Formamide (NMF), bromobenzene, chloroform, chlorobenzene, benzonitrile , Quinoline, benzyl ether, ethanol, isopropyl alcohol, methanol, butanol, 2-ethoxy ethanol, 2-butoxy ethanol, 2-methoxy propanol, THF (tetrahydrofuran), ethylene glycol, pyridine, N-vinylpyrrolidone , Methyl ethyl ketone (butanone), alpha-terpinol, formic acid, ethyl acetate and acrylonitrile may be used.
On the other hand, in order to increase the dispersion of the graphite and carbon nanotubes in the feed solution, it is preferable to prepare a feed solution by mixing the graphite and carbon nanotubes and then homogenizing at high speed.
The high speed homogenization means agitation of the feed solution, and preferably, the dispersion solution is stirred at 3000 to 8000 rpm. The high speed homogenization is preferably performed for 0.5 to 3 hours. In less than 0.5 hours, there is a limit that the degree of dispersion falls, and in more than 3 hours, the degree of dispersion does not increase any more.
The agitation can be performed using a high speed homogenizer, by mixing based on a high shear rate (> 10 4 sec -1 ) between the rotor and the stator of the high speed homogenizer. , The dispersibility in the feed solution is increased, and when used as a feed solution of the high pressure homogenization of
remind Feed Solution Inlet and , With the outlet , Inlet and Outlet Between the micrometer scale Diameter High pressure containing fine flow path having In homogenizer Passing Step (Step 2)
The step is a high pressure homogenization of the feed solution prepared in 1 to peel off the graphene from the graphite in the feed solution, and at the same time to make the carbon nanotubes disentangled (disentanglement) and to effectively disperse the carbon nanotubes.
The term 'high pressure homogenization' means applying a high pressure to a microchannel having a diameter of a micrometer scale and applying a strong shear force to a material passing therethrough. In general, high pressure homogenization is performed using a high pressure homogenizer comprising an inlet, an outlet, and a microchannel having a diameter of micrometer scale that connects between the inlet and the outlet.
As described above, since the carbon nanotubes are included in addition to the graphite in the feed solution, the graphite is separated into graphene by high pressure homogenization, and the carbon nanotubes are in the unwrapped form, and at the same time, the carbon nanotubes are dispersed. As a result, a three-dimensional network is formed between graphene and carbon nanotubes structurally, π-π interaction is reduced between graphene or carbon nanotubes due to structural hindrance, thereby reducing reaggregation.
It is preferable that the fine flow path has a diameter of 10 to 800 µm. In addition, the feed solution is preferably introduced into the inlet of the high pressure homogenizer under pressure application of 100 to 3000 bar to pass through the fine flow path.
In addition, the feed solution passed through the micro-path can be re-introduced into the inlet of the high pressure homogenizer, thereby further processing carbon nanotubes / graphene.
The re-insertion process may be performed by repeating 2 to 10 times. The re-insertion process may be performed by using the high pressure homogenizer repeatedly used, or using a plurality of high pressure homogenizers. In addition, the re-insertion process may be performed separately for each process, or may be performed continuously.
Carbon Nanotubes / Graphene Mixed Dispersion
The carbon nanotubes / graphenes in the carbon nanotube / graphene mixed dispersion prepared according to the present invention have a uniform graphene size, and when applied to an application field, for example, in the form of unwrapped on the surface of graphene during drying Is characterized in that the carbon nanotubes are uniformly adsorbed.
Accordingly, a three-dimensional network is formed between the graphene and the carbon nanotubes structurally, and the carbon nanotubes act as a bridge between the graphenes, thereby affecting the electron migration path and reducing the sheet resistance of the graphene. In this way, it is possible to increase the electrical conductivity of the graphene more.
In addition, in the application process of the graphene is generally used to prepare the graphene in the form of a dispersion (slurry), the carbon nanotube / graphene mixed dispersion prepared according to the present invention is a high concentration in itself, for example, for secondary batteries In the slurry manufacturing process, there is an advantage that it can be directly applied without additional processes, and excellent capacity characteristics, electrical characteristics, and lifetime characteristics at high concentrations can be expected.
In addition, the carbon nanotube / graphene mixed dispersion according to the present invention can be applied to the existing graphene applications, such as conductive paste composition, conductive ink composition, heat radiation substrate forming composition, electroconductive composite, EMI shielding composite Or it can be utilized for various uses, such as a battery electrically conductive material or a slurry.
According to one embodiment of the present invention, as shown in Figure 1 by the manufacturing method according to the present invention was able to confirm the well-released graphene flakes and disentangled carbon nanotubes, and also on the surface of the graphene carbon nano It was confirmed that the tube was formed uniformly to form a three-dimensional network. In addition, the carbon nanotube / graphene hybrid carbon-based material was confirmed that the electrical resistance is significantly improved by reducing the surface resistance.
In the method for producing a high concentration carbon nanotube / graphene mixed dispersion according to the present invention, the carbon nanotube / graphene mixture forming a three-dimensional network with carbon nanotubes by high pressure homogenization of a feed solution containing graphite and carbon nanotubes Dispersions can be prepared. Accordingly, the manufacturing efficiency is superior to that of the conventional process, and the electrical characteristics of the carbon nanotube / graphene hybrid carbon based on the three-dimensional network formed between the graphene and the carbon nanotubes are remarkably improved.
Figure 1 shows the results of observing the carbon nanotube / graphene mixed dispersion prepared in Example of the present invention by SEM image (Fig. 1 (a): Example 1, Figure 1 (b): Example 2 ).
Figure 2 shows the results of visual observation of the carbon nanotube / graphene mixture dispersion prepared in the embodiment of the present invention.
Figure 3 shows the surface resistance measurement results of the PET film coated with the carbon nanotube / graphene mixed dispersion of the embodiment of the present invention.
Figure 4 shows the surface resistance measurement results of the PET film coated with a graphene dispersion of the comparative example of the present invention.
Hereinafter, preferred embodiments are presented to help understand the invention. However, the following examples are only for illustrating the present invention, and the present invention is not limited thereto.
Example One
A solution comprising 35 g of graphite (BNB90), 7 g of PVP (Mw = 58,000) and 500 mL of N-Methyl-2-pyrrolidone (NMP) was prepared. Separately, a solution including 3.5 g of carbon nanotubes (ACN's multiwall CNT (1 μm)) and 200 mL of NMP was prepared. After the two solutions were stirred at 6,000 rpm and 30 minutes in a high speed homogenizer (Silverson model L5M mixer), respectively, the two solutions were mixed and again stirred at 6,000 rpm and 10 minutes in order to prepare a feed solution.
The feed solution was fed to the inlet of the high pressure homogenizer. The high pressure homogenizer has a structure including a microchannel having a diameter of a micrometer and connecting the inlet of the raw material, the outlet of the separation result, and the inlet and the outlet. The feed solution was introduced while applying a high pressure of 1600 bar through the inlet, and a high shear force was applied while passing through a microchannel having a diameter of 75 μm. The high pressure homogenization process was repeated by re-injecting the dispersion liquid recovered from the outlet part into the inlet part of the high pressure homogenizer, and the carbon nanotube / graphene mixed dispersion was prepared until the high pressure homogenization process was repeated five times. .
Example 2
A solution comprising 35 g of graphite (3
The feed solution was fed to the inlet of the high pressure homogenizer. The high pressure homogenizer has a structure including a microchannel having a diameter of a micrometer and connecting the inlet of the raw material, the outlet of the separation result, and the inlet and the outlet. The feed solution was introduced while applying a high pressure of 1600 bar through the inlet, and a high shear force was applied while passing through a microchannel having a diameter of 75 μm. The high pressure homogenization process was repeated by re-injecting the dispersion liquid recovered from the outlet to the inlet of the high pressure homogenizer, and the carbon nanotube / graphene mixed dispersion was prepared until the high pressure homogenization process was repeated 10 times in total. (Graphene concentration: 5 wt%, carbon nanotube concentration: 2 wt%).
Experimental Example 1: carbon nanotubes / Graphene Mixed dispersion observation
The surface of graphene in the carbon nanotube / graphene mixed dispersion prepared in the above example was confirmed by SEM image, and the results are shown in FIG. 1. As shown in FIG. 1, the exfoliated graphene flakes and disentangled carbon nanotubes were confirmed, and in particular, carbon nanotubes were formed on the surface of graphene to form a three-dimensional network. there was.
In addition, in Example 2, the degree of dispersion was visually observed and the results are shown in FIG. 2. As shown in Figure 2, it was confirmed that the graphene and carbon nanotubes are well dispersed without reaggregation.
Experimental Example 2: surface resistance rating
Step 1) Preparation of Anode Paste
A positive electrode paste was prepared from the carbon nanotube / graphene mixed dispersion prepared in Example to evaluate its properties.
Specifically, 8.47 g of KF 1100 binder (11.8 wt% in NMP), 0.75 g of super-C65, 2.5 g of carbon nanotube / graphene dispersion prepared in Example 2 and 2 g of NMP were placed in a paste mixer-only container, and 1,500. Mix for 5 minutes at rpm. 23.11 g of NMC-based cathode active material and 5 g of NMP were added thereto, and the mixture was mixed at 1,500 rpm for 5 minutes to prepare a slurry.
A certain amount of the slurry was sprayed on a PET film (thickness: 18.6 μm), coated using a Mayer bar (wire size: # 9), and then dried at 100 ° C. in a convection oven for 2 hours. The coating thickness on the PET film was measured, and sheet resistance was measured at 5.5 × 4.5 size using four-point-probe, and the results are shown in Table 1 below.
Step 2) Preparation of Anode Paste (Comparative Example)
For comparison, a positive electrode paste was prepared in the same manner as in
After coating on the PET film in the same manner as in
(average: 25-point)
(25-point)
As shown in Table 1, in the embodiment according to the present invention, the surface resistance and the deviation was significantly lower than the comparative example, which is due to the formation of a three-dimensional network with the graphene carbon nanotubes peeled off.
Step 3) Evaluate sheet resistance as it bends
After applying silver paste to both ends of the diagonal of the coated PET film prepared in
As shown in Figure 3, in the embodiment according to the present invention, the average value of the flat state was 3.10 kΩ / □, the average value of the bending state was 3.23 kΩ / □. When the bending radius was measured at 15 mm, the tensile strain increased about 0.9% and the surface resistance increased about 4%.
On the other hand, as shown in Figure 4, in the comparative example the average value of the flat state was 16.60 kΩ / □, the average value of the bending state was 17.28 kΩ / □. When the bending radius was measured at 15 mm, the tensile strain increased about 0.9% and the surface resistance increased about 4%.
As described above, the sheet resistance of the embodiment according to the present invention was significantly smaller than the comparative example, in particular, even in the vending state, the sheet resistance value was small and the deviation was also remarkably small.
Claims (16)
2) passing the feed solution through a high pressure homogenizer comprising an inlet, an outlet, and a microchannel having a diameter of micrometer scale connecting the inlet and the outlet;
The fine flow path has a diameter of 50 to 300 ㎛,
The feed solution is introduced into the inlet of the high pressure homogenizer under pressure application of 500 to 3000 bar and passes through the microchannel,
Method for producing a carbon nanotube / graphene mixed dispersion.
The weight ratio of the graphite and carbon nanotubes is characterized in that 20: 1 to 1: 1,
Manufacturing method.
The concentration of graphite in the feed solution is characterized in that 0.5 to 5% by weight,
Manufacturing method.
The concentration of carbon nanotubes in the feed solution is characterized in that 0.1 to 5% by weight,
Manufacturing method.
The dispersant is a low molecular weight pyrene derivative; Cellulose based polymers; Cationic surfactants; Anionic surfactants; Gum arabic; n-dodecyl bD-maltoside; Amphoteric surfactants; Polyvinylpyrrolidone-based polymers; Polyethylene oxide polymers; Ethylene oxide-propylene oxide copolymers; Tannic acid; Or a mixture of a plurality of polyaromatic hydrocarbon oxides, the mixture comprising a polyaromatic hydrocarbon oxide having a molecular weight of 300 to 1000 in an amount of 60% by weight or more,
Manufacturing method.
The dispersant is characterized in that the polyvinylpyrrolidone,
Manufacturing method.
Characterized in that the weight ratio of the total weight of the graphite and carbon nanotubes and the dispersant is 2.5 to 20,
Manufacturing method.
Step 1, characterized in that for mixing the graphite, carbon nanotubes and dispersant and then high speed homogenization to prepare a feed solution,
Manufacturing method.
The high speed homogenization may be performed by stirring the dispersion solution at 3000 to 8000 rpm.
Manufacturing method.
The high speed homogenization is characterized in that performed for 0.5 to 3 hours,
Manufacturing method.
The solvent of the feed solution is water, N-Methyl-2-pyrrolidone (NMP), acetone, DMF (N, N-dimethylformamide), DMSO (dimethyl sulfoxide), CHP (Cyclohexyl-pyrrolidinone), N12P (N-dodecyl-pyrrolidone) ), Benzyl benzoate, N-Octyl-pyrrolidone (N8P), dimethyl-imidazolidinone (DMEU), cyclohexanone, dimethylacetamide (DMA), N-Methyl Formamide (NMF), bromobenzene, chloroform, chlorobenzene, benzonitrile , Quinoline, benzyl ether, ethanol, isopropyl alcohol, methanol, butanol, 2-ethoxy ethanol, 2-butoxy ethanol, 2-methoxy propanol, THF (tetrahydrofuran), ethylene glycol, pyridine, N-vinylpyrrolidone , Methyl ethyl ketone (butanone), alpha-terpinol, formic acid, ethyl acetate, and at least one member selected from the group consisting of acrylonitrile,
Manufacturing method.
Graphite in the feed solution is peeled while passing through the micro-channel under the application of shear force, characterized in that the graphene is produced,
Manufacturing method.
Characterized in that the step 2 additionally performed 2 to 10 times,
Manufacturing method.
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| KR102482505B1 (en) * | 2018-06-11 | 2022-12-30 | 주식회사 엘지화학 | Carbon nanotube dispersed solution and method for preparing the same |
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