KR20160133711A - Method for preparation of high concentrated carbon nanotube/graphene dispersion - Google Patents
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Abstract
Description
The present invention relates to a method for producing a carbon nanotube by treating carbon nanotubes and graphite together in situ using high pressure homogenization to peel graphite and unwinding carbon nanotubes simultaneously, To a method for producing a hybrid carbon nanotube / graphene mixed dispersion.
Carbon materials such as graphene and carbon nanotubes have excellent physical properties and are applied to various fields. In recent years, hybrid carbon-based materials have been developed in which carbon-based materials are combined with each other, and carbon nanotubes / graphene materials are attracting attention as hybrid carbon-based materials.
Graphene is a semimetallic material with a thickness corresponding to the carbon atomic layer, with the carbon atoms forming a hexagonally connected arrangement in two dimensions on the sp2 bond. Recently, evaluation of the properties of a graphene sheet having one carbon atom layer has revealed that the electron mobility is about 50,000
The carbon nanotube / graphene hybrid carbon-based material is intended to further improve the characteristics of graphene as described above. Carbon nanotubes capable of acting as a bridge between graphenes are sufficiently adsorbed on the graphene surface, The electrical conductivity of graphene can be further improved.
Carbon nanotubes / graphene hybrid carbon-based materials are primarily mixed with two or more carbon-based materials, but due to the physicochemical properties inherent to the carbon-based materials, various factors are considered to be maximized. . In particular, in the case of a carbon nanotube / graphene hybrid carbon-based material, it is necessary that the carbon nanotubes are uniformly and sufficiently adsorbed on the graphene surface.
Conventional manufacturing methods for such carbon nanotube / graphene hybrid carbon-based materials include a solution-phase method and a solid-phase method. In the former case, the solubility of each material is processed in the harsh condition. For example, there is a method of acid treatment of a strong acid such as Hummner's method and ultrasonic treatment after thermal reduction. However, the above method causes a restacking problem again after the reduction process. In the latter case, the shape and characteristics of the carbon nanotube / graphene hybrid carbon-based material are controlled by controlling the growth conditions by a typical CVD method. However, the method is not suitable for mass production.
In addition, carbon nanotubes of the carbon nanotube / graphene hybrid carbon-based material must be disentanglement because the intrinsic nature of the carbon nanotubes is not expressed by the entanglement of the carbon nanotubes.
As a conventional method for producing carbon nanotubes in a loose form, ball-milling, jet-milling, or ultrasonic treatment of carbon nanotubes together with graphene is available. However, in the case of the above method, the length of the carbon nanotubes is small, but there is a problem in that the carbon nanotubes are limited to be manufactured in a loose form or require a long time.
Accordingly, there is a need for a method of manufacturing a carbon nanotube / graphene hybrid carbon based material with high yield and simple method. In particular, carbon nanotubes and graphite are treated in situ to remove graphite and carbon nanotubes There is a need for a method for producing a carbon nanotube / graphene mixed dispersion having excellent properties.
The present invention relates to a process for producing a carbon nanotube / graphene mixed dispersion having excellent properties by simultaneously treating carbon nanotubes and graphite in situ using high pressure homogenization and peeling of graphite and annealing of carbon nanotubes simultaneously .
In order to solve the above-mentioned problems, the present invention provides a method for producing a carbon nanotube / graphene mixed dispersion comprising the steps of:
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 including a microfluidic channel having a micrometer scale diameter connecting between the inlet and outlet.
The term "graphite" used in the present invention refers to a material which is also called graphite or talc and belongs to a hexagonal system having a crystal structure such as quartz, and is a material having a black color and metallic luster. The graphite has a plate-like structure. A single layer of graphite is called "graphene" to be produced in the present invention, and thus graphite becomes the main raw material for the production of graphene.
In order to peel off graphene from graphite, it is necessary to apply energy to overcome the pi-pi interactions between the stacked graphenes. In the present invention, the high-pressure homogenization method is used as in
Accordingly, in the present invention, by homogenizing the feed solution containing carbon nanotubes in addition to graphite, the aggregation of the graphene peeled is suppressed, and at the same time, the graphene and carbon nanotubes peeled off are three- The network can be formed to lower the sheet resistance of graphene.
Further, in order to manifest the characteristics of the carbon nanotube / graphene hybrid carbon-based material, the carbon nanotubes must be homogeneously adsorbed on the surface of the graphene by disentanglement. In the present invention, by homogenizing the carbon nanotubes together under high pressure, When the carbon nanotube / graphene mixed dispersion is applied for other purposes, the carbon nanotube / graphene mixed dispersion is used as the carbon nanotube / The carbon nanotubes can be uniformly adsorbed on the surface of the graphene.
Hereinafter, the present invention will be described step by step.
Graphite And carbon nanotubes were mixed Feed The step of preparing the solution (step 1)
This step is a step of preparing a feed solution to be applied to high pressure homogenization of
The carbon nanotubes form a three-dimensional network together with the graphene peeled in
In addition to the above, the carbon nanotubes are disentanglement by applying the high pressure homogenization together with the carbon nanotubes and the graphite, and at the same time, the carbon nanotubes / graphene mixed dispersion in which the carbon nanotubes are uniformly dispersed Can be manufactured. Accordingly, when the carbon nanotube / graphene mixed dispersion is applied for other purposes, carbon nanotubes can be uniformly adsorbed on the surface of graphene, for example, when dried.
The weight ratio of the graphite to the carbon nanotubes is preferably in the range of 20: 1 to 1: 1. In this case, the dispersion effect and the surface resistance reduction effect of the carbon nanotube / It is remarkable.
In order to increase the degree of dispersion of graphite and carbon nanotubes in the feed solution, it is preferable to use a dispersant. The dispersants act to maintain their dispersed state mediated by hydrophobic graphite, delaminated graphite or graphene due to their amphiphilic nature, and are also referred to as surfactants in other terms. As the dispersing agent, any dispersant may be used as long as it is used for graphene peeling, and an anionic surfactant, a nonionic surfactant, and a cationic surfactant can be used. Specific examples thereof include pyrene-based low molecular weight derivatives; Cellulosic polymers; Cationic surfactants; Anionic surfactants; Gum arabic; n-Dodecyl bD-maltoside; Amphoteric surfactants; Polyvinylpyrrolidone type polymers; Polyethylene oxide type polymers; Ethylene oxide-propylene oxide copolymer; Tannic acid; Or a mixture of plural kinds of polyaromatic hydrocarbon oxides, which contains a polyaromatic hydrocarbon oxide having a molecular weight of 300 to 1000 in an amount of 60 wt% or more.
Preferably, polyvinylpyrrolidone may be used as the dispersing agent. The above-mentioned "polyvinylpyrrolidone" is a polymer prepared by polymerizing N-vinylpyrrolidone, and means a polymer having a weight average molecular weight of 6,000 to 1,300,000 g / mol. In particular, . After the graphene is peeled off from the graphite, the graphene tends to be reunited, and the polyvinylpyrrolidone may be attached to the surface of the graphene to inhibit the graphene from re-aggregating.
The amount of the dispersant to be used is determined by the content of graphite and carbon nanotube in the feed solution, and preferably the total weight of the graphite and the carbon nanotube and the weight ratio of the dispersant (graphite + carbon nanotube) / dispersant) To 20% by weight. If the content is less than 2.5, the content of graphite / carbon nanotubes is too low to detach the peeling efficiency. If the content exceeds 20, the content of the dispersant is too low, thereby deteriorating the dispersing effect of graphite / carbon nanotubes. More preferably, the total weight of the graphite and the carbon nanotube and the weight ratio of the dispersant is 2.5 to 5. [
The concentration of the graphite in the feed solution is preferably 0.5 to 10% by weight. If the amount is less than 0.5% by weight, the amount of graphite is too low and the yield in the peeling step is low. If the amount is more than 10% by weight, the content of graphite is too high.
The concentration of carbon nanotubes in the feed solution is preferably 0.1 to 5% by weight. When the content is less than 0.1% by weight, the concentration of the carbon nanotubes is too low to improve the properties of the graphene. When the content exceeds 5% by weight, the content of the carbon nanotubes is too high, And the effect of high-pressure homogenization deteriorates.
The solvent of the feed solution can be selected from the group consisting of water, N-methyl-2-pyrrolidone, acetone, N, N-dimethylformamide, DMSO, CHP, N-dodecyl-pyrrolidone ), Benzyl benzoate, N-octyl-pyrrolidone, dimethyl-imidazolidinone, cyclohexanone, dimethylacetamide, NMF (N-Methyl Formamide), bromobenzene, chloroform, chlorobenzene, benzonitrile , Quinoline, benzyl ether, ethanol, isopropyl alcohol, methanol, butanol, 2-ethoxyethanol, 2-butoxyethanol, 2-methoxypropanol, tetrahydrofuran (THF), ethylene glycol, , Methyl ethyl ketone (butanone), alpha-terpineol, formic acid, ethyl acetate and acrylonitrile may be used.
Meanwhile, in order to increase the degree of dispersion of graphite and carbon nanotubes in the feed solution, it is preferable to mix graphite and carbon nanotubes followed by high-speed homogenization to prepare a feed solution.
The high-speed homogenization means stirring the feed solution, preferably the dispersion solution is stirred at 3000 to 8000 rpm. The high-speed homogenization is preferably performed for 0.5 to 3 hours. When the time is less than 0.5 hour, there is a limit that the dispersion degree is lowered, and when the time exceeds 3 hours, the dispersion degree does not become substantially higher.
The stirring can be carried out using a high speed homogenizer and by mixing based on the high shear rate (> 10 4 sec -1 ) between the rotor and stator of the high speed homogenizer , The degree of dispersion in the feed solution is increased, and as a feed solution of high pressure homogenization in
remind Feed The solution The inlet , The outlet , The inlet Outlet And a micrometer-scale Diameter And a high-pressure In the homogenizer (Step 2)
In this step, the feed solution prepared in the
The term 'high pressure homogenization' means applying a high pressure to a micro-channel having a micrometer scale diameter to apply a strong shear force to the material passing through it. Typically, high pressure homogenization is performed using a high pressure homogenizer including an inlet, an outlet, and a microchannel connecting between the inlet and outlet and having a micrometer scale diameter.
As described above, since the carbon nanotubes are contained in addition to the graphite in the feed solution, the graphite is peeled off by graphene by high-pressure homogenization, and the carbon nanotubes are in a relaxed state, and at the same time, the carbon nanotubes are dispersed. Accordingly, a three-dimensional network is structurally formed between graphene and carbon nanotubes, and the steric hindrance reduces the reprecipitation phenomenon due to a decrease in the pi-pi interaction between graphenes or carbon nanotubes.
It is preferable that the fine flow path has a diameter of 10 to 800 탆. In addition, it is preferable that the feed solution flows into the inlet portion of the high pressure homogenizer through the micro flow path under a pressure of 100 to 3000 bar.
Further, the feed solution passing through the microchannel can be reintroduced into the inlet of the high-pressure homogenizer, and thus the carbon nanotube / graphene can be further treated.
The recycling may be carried out two to ten times. The reintroduction process can be carried out repeatedly using the high-pressure homogenizer used or using a plurality of high-pressure homogenizers. In addition, the re-inputting process may be performed separately or sequentially.
Carbon nanotubes / Grapina 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 application fields, for example, Of carbon nanotubes are uniformly adsorbed.
Therefore, a three-dimensional network is formed between graphene and carbon nanotube structurally, and carbon nanotube acts as a bridge between graphenes, thereby affecting the movement path of electrons and reducing the sheet resistance of graphene Thereby increasing the electrical conductivity of the graphene.
Generally, graphene is prepared in the form of a dispersion (slurry) in the process of application of graphene. The carbon nanotube / graphene mixed dispersion prepared according to the present invention has a high concentration in itself, It has an advantage of being directly applied without any additional process in the slurry production process, and excellent capacity characteristics, electrical characteristics and lifetime characteristics can be expected according to high concentration.
In addition, the carbon nanotube / graphene mixed dispersion according to the present invention can be applied to existing graphene applications, and can be applied to various applications such as a conductive paste composition, a conductive ink composition, a composition for forming a heat dissipation substrate, an electroconductive composite, Or a conductive material or a slurry for a battery.
According to an embodiment of the present invention, it is possible to identify graphene flakes and disentanglement carbon nanotubes that are well separated as shown in FIG. 1 by the manufacturing method according to the present invention, It can be seen that the tubes are formed uniformly to form a three dimensional network. In addition, it was confirmed that the carbon nanotube / graphene hybrid carbon-based material has a reduced surface resistance and significantly improved electrical characteristics.
The method of producing a high-concentration carbon nanotube / graphene mixed dispersion according to the present invention comprises homogenizing a feed solution containing graphite and carbon nanotubes to form a carbon nanotube / graphene mixture A dispersion 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 system are markedly improved by the three-dimensional network formed between the graphene and the carbon nanotube.
1 shows the result of observing a mixed dispersion of carbon nanotubes / graphene prepared in the example of the present invention with an SEM image (Fig. 1 (a): Example 1, Fig. 1 (b) ).
Fig. 2 shows the result of visual observation of the carbon nanotube / graphene mixed dispersion prepared in the example of the present invention.
3 shows the results of surface resistance measurement of the PET film coated with the carbon nanotube / graphene mixed dispersion of the example of the present invention.
Fig. 4 shows the result of measuring the surface resistance of the PET film coated with the graphene dispersion of the comparative example of the present invention.
Best Mode for Carrying Out the Invention Hereinafter, preferred embodiments are shown to facilitate understanding of the present invention. However, the following examples are intended to illustrate the present invention without limiting it thereto.
Example One
A solution containing 35 g of graphite (BNB90), 7 g of PVP (Mw = 58,000) and 500 mL of NMP (N-Methyl-2-pyrrolidone) was prepared. Separately, a solution containing 3.5 g of carbon nanotubes (multiwall CNT (1 탆) from ACN Co.) and 200 mL of NMP was prepared. The two solutions were stirred at 6,000 rpm for 30 minutes in a high-speed homogenizer (Silverson model L5M mixer), and then the two solutions were mixed and stirred at 6,000 rpm for 10 minutes 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 an inlet portion of the raw material, an outlet portion of the peeled product, and a microchannel connecting the inlet portion and the outlet portion and having a micrometer scale diameter. A high pressure of 1,600 bar was applied through the inlet to feed the feed solution and a high shear force was applied while passing a fine flow path having a diameter of 75 μm. The dispersion liquid recovered from the outlet portion was reintroduced into the inlet portion of the high pressure homogenizer to repeat the high pressure homogenization process and the carbon nanotube / graphene mixed dispersion was repeated until the high pressure homogenization process was repeated five times in total .
Example 2
A solution containing 35 g of graphite (3 mu m in diameter), 7 g of PVP (Mw = 58,000) and 500 mL of NMP (N-Methyl-2-pyrrolidone) was prepared. Separately, a solution containing 14 g of carbon nanotubes (multiwall CNT (1 탆) from ACN), 2.8 g of PVP and 200 mL of NMP was prepared. The two solutions were stirred at 6,000 rpm for 30 minutes in a high-speed homogenizer (Silverson model L5M mixer), and then the two solutions were mixed and stirred at 6,000 rpm for 10 minutes 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 an inlet portion of the raw material, an outlet portion of the peeled product, and a microchannel connecting the inlet portion and the outlet portion and having a micrometer scale diameter. A high pressure of 1,600 bar was applied through the inlet to feed the feed solution and a high shear force was applied while passing a fine flow path having a diameter of 75 μm. The dispersion liquid recovered from the outlet was reintroduced into the inlet of the high pressure homogenizer and the high pressure homogenization process was repeated. The carbon nanotube / graphene dispersion was repeated 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 / Grapina Observation of mixed dispersion
The surface of the graphene in the carbon nanotube / graphene mixed dispersion prepared in the above example was confirmed by SEM image, and the result is shown in FIG. As shown in FIG. 1, it was confirmed that carbon nanotubes with well-separated graphene flakes and disentanglement were formed, and carbon nanotubes were formed on the surface of graphenes to form a three-dimensional network there was.
In the case of Example 2, the degree of dispersion was visually observed and the results are shown in Fig. As shown in FIG. 2, it was confirmed that graphene and carbon nanotubes were well dispersed without re-aggregation.
Experimental Example 2: Evaluation of surface resistance
Step 1) Preparation of positive electrode paste
The anode paste was prepared from the carbon nanotube / graphene mixed dispersion prepared in the above example and the characteristics thereof were evaluated.
Specifically, 8.47 g of KF 1100 binder (11.8 wt% in NMP), 0.75 g of super-C65, 2.5 g of the carbon nanotube / graphene dispersion prepared in Example 2 and 2 g of NMP were placed in a paste mixer- rpm for 5 minutes. 23.11 g of NMC-based cathode active material and 5 g of NMP were added thereto, followed by mixing at 1,500 rpm for 5 minutes to prepare a slurry.
A predetermined amount of the slurry was sprayed onto a PET film (thickness: 18.6 μm), coated with a Mayer bar (wire size: # 9), and then dried in a convection oven at 100 ° C. for 2 hours. The thickness of the coating on the PET film was measured and the sheet resistance was measured at 25-point at 5.5 × 4.5 size using a four-point-probe. The results are shown in Table 1 below.
Step 2) Preparation of positive electrode paste (comparative example)
For comparison, a positive electrode paste was prepared in the same manner as in
The film was coated on a PET film in the same manner as in the
(average: 25-point)
(25-point)
As shown in Table 1, the surface resistance and the deviation of the carbon nanotubes of the examples according to the present invention were significantly lower than those of the comparative examples. This is due to the fact that the carbon nanotubes formed a three-dimensional network together with the separated graphenes.
Step 3) Evaluation of sheet resistance according to warpage
The silver paste was applied to the diagonal ends of the coated PET film prepared in
As shown in FIG. 3, in the embodiment according to the present invention, the average value in the flat state was 3.10 k? /? And the average value in the bending state was 3.23? / ?. When the bending radius was measured at 15 mm, tensile strain was increased by about 0.9% and surface resistance was increased by about 4%.
On the other hand, as shown in FIG. 4, in the comparative example, the average value in the flat state was 16.60 k? /? And the average value in the bending state was 17.28? / ?. When the bending radius was measured at 15 mm, tensile strain was increased by about 0.9% and surface resistance was increased by about 4%.
As described above, the sheet resistance of the example according to the present invention was significantly smaller than that of the comparative example, and it was confirmed that the sheet resistance was small and the deviation was remarkably small even in the vending state.
Claims (16)
2) passing the feed solution through an inlet, an outlet, and a high pressure homogenizer comprising a microchannel connecting between the inlet and outlet and having a micrometer scale diameter,
Wherein the carbon nanotube / graphene mixed dispersion is prepared.
Wherein the weight ratio of the graphite and the carbon nanotube is 20: 1 to 1:
Gt;
Characterized in that the concentration of graphite in the feed solution is from 0.5 to 5%
Gt;
Wherein the concentration of the carbon nanotubes in the feed solution is 0.1 to 5 wt%
Gt;
Characterized in that the feed solution further comprises a dispersing agent.
Gt;
The dispersant may be a pyrene-based low molecular weight material; Cellulosic polymers; Cationic surfactants; Anionic surfactants; Gum arabic; n-Dodecyl bD-maltoside; Amphoteric surfactants; Polyvinylpyrrolidone type polymers; Polyethylene oxide type polymers; Ethylene oxide-propylene oxide copolymer; Tannic acid; Or a mixture of plural kinds of polyaromatic hydrocarbon oxides, wherein the mixture contains a polyaromatic hydrocarbon oxide having a molecular weight of 300 to 1000 in an amount of not less than 60% by weight,
Gt;
Wherein the dispersing agent is polyvinyl pyrrolidone.
Gt;
Wherein the total weight of the graphite and the carbon nanotube and the weight ratio of the dispersing agent is 2.5 to 20,
Gt;
Wherein the step 1 is a step of mixing the graphite and the carbon nanotube and then homogenizing at a high speed to prepare a feed solution.
Gt;
Characterized in that the high-speed homogenization is carried out by stirring the dispersion solution at 3000 to 8000 rpm.
Gt;
Characterized in that the high-speed homogenization is carried out for 0.5 to 3 hours.
Gt;
The solvent of the feed solution can be selected from the group consisting of water, N-methyl-2-pyrrolidone, acetone, N, N-dimethylformamide, DMSO, CHP, N-dodecyl-pyrrolidone ), Benzyl benzoate, N-octyl-pyrrolidone, dimethyl-imidazolidinone, cyclohexanone, dimethylacetamide, NMF (N-Methyl Formamide), bromobenzene, chloroform, chlorobenzene, benzonitrile , Quinoline, benzyl ether, ethanol, isopropyl alcohol, methanol, butanol, 2-ethoxyethanol, 2-butoxyethanol, 2-methoxypropanol, tetrahydrofuran (THF), ethylene glycol, , Methyl ethyl ketone (butanone), alpha-terpineol, formic acid, ethyl acetate and acrylonitrile.
Gt;
Wherein the graphite in the feed solution is peeled while passing through the fine flow path under application of a shear force to produce graphene.
Gt;
Characterized in that the fine flow path has a diameter of 50 to 300 mu m.
Gt;
Wherein the feed solution flows into the inlet portion of the high-pressure homogenizer under a pressure of 500 to 3000 bar and passes through the microchannel.
Gt;
Characterized in that the step 2 is further carried out 2 to 10 times.
Gt;
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| KR20190140275A (en) * | 2018-06-11 | 2019-12-19 | 주식회사 엘지화학 | Carbon nanotube dispersed solution and method for preparing the same |
| KR20230002198A (en) * | 2018-06-11 | 2023-01-05 | 주식회사 엘지화학 | Carbon nanotube dispersed solution and method for preparing the same |
| WO2019240439A1 (en) * | 2018-06-11 | 2019-12-19 | 주식회사 엘지화학 | Carbon nanotube dispersion and preparation method therefor |
| JP2021520040A (en) * | 2018-06-11 | 2021-08-12 | エルジー・ケム・リミテッド | Carbon nanotube dispersion liquid and its manufacturing method |
| US11845655B2 (en) | 2018-06-11 | 2023-12-19 | Lg Chem, Ltd. | Carbon nanotube dispersion and method for preparing the same |
| US11542164B2 (en) | 2018-06-11 | 2023-01-03 | Lg Chem, Ltd. | Carbon nanotube dispersion and method for preparing the same |
| KR20220030766A (en) * | 2020-09-03 | 2022-03-11 | (주)투디엠 | Filler for polymer composites and the process for producing the same |
| CN115346804A (en) * | 2021-05-13 | 2022-11-15 | 中国科学院大连化学物理研究所 | Self-powered sensor circuit platform with embedded super capacitor and preparation method thereof |
| CN115386317A (en) * | 2022-08-16 | 2022-11-25 | 浙江工业大学 | Preparation method of high-thermal-conductivity and high-electrical-conductivity composite adhesive taking graphene and carbon nano tubes as fillers |
| KR102518417B1 (en) * | 2022-09-05 | 2023-04-06 | 주식회사 베터리얼 | Carbon nanotube despersion, manufacturing method for same, slurry composition for electrode comprising same, eletrode comprising same and lithum secondary battery comprising same |
| WO2024053889A1 (en) * | 2022-09-05 | 2024-03-14 | 주식회사 베터리얼 | Carbon nanotube dispersion solution, preparation method therefor, electrode slurry composition comprising same, electrode comprising same, and secondary battery comprising same |
| CN115717064A (en) * | 2022-11-03 | 2023-02-28 | 清华大学 | Graphene oxide-carbon nanotube composite oil displacement agent and application thereof |
| CN115717064B (en) * | 2022-11-03 | 2023-09-12 | 清华大学 | Graphene oxide-carbon nano tube composite oil displacement agent and application thereof |
| CN116004087A (en) * | 2023-01-10 | 2023-04-25 | 广东耐迪化工有限公司 | Antistatic graphene coating and preparation method thereof |
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