KR20150016852A - Carbon nanotube dispersed solution and method for preparing the same - Google Patents

Carbon nanotube dispersed solution and method for preparing the same Download PDF

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KR20150016852A
KR20150016852A KR1020130092828A KR20130092828A KR20150016852A KR 20150016852 A KR20150016852 A KR 20150016852A KR 1020130092828 A KR1020130092828 A KR 1020130092828A KR 20130092828 A KR20130092828 A KR 20130092828A KR 20150016852 A KR20150016852 A KR 20150016852A
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carbon nanotube
nitrile rubber
weight
solvent
dispersion
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KR1020130092828A
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Korean (ko)
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김용태
김병열
안성희
김중인
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제일모직주식회사
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Priority to KR1020130092828A priority Critical patent/KR20150016852A/en
Priority to PCT/KR2013/011533 priority patent/WO2015020280A1/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82BNANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B1/00Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • B82B1/008Nanostructures not provided for in groups B82B1/001 - B82B1/007
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82BNANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • B82B3/0009Forming specific nanostructures
    • B82B3/0033Manufacture or treatment of substrate-free structures, i.e. not connected to any support
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82BNANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • B82B3/0095Manufacture or treatments or nanostructures not provided for in groups B82B3/0009 - B82B3/009
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/158Carbon nanotubes
    • C01B32/168After-treatment
    • C01B32/174Derivatisation; Solubilisation; Dispersion in solvents
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00Structure or properties of carbon nanotubes
    • C01B2202/04Nanotubes with a specific amount of walls
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00Structure or properties of carbon nanotubes
    • C01B2202/20Nanotubes characterized by their properties
    • C01B2202/28Solid content in solvents

Abstract

The carbon nanotube dispersion of the present invention is a carbon nanotube having a D99 value of particle size distribution of 50 m or less; Nitrile rubber; And a solvent. The carbon nanotube dispersion is obtained by uniformly dispersing carbon nanotubes in a solvent economically.

Description

TECHNICAL FIELD [0001] The present invention relates to a carbon nanotube dispersion and a method for manufacturing the carbon nanotube dispersion.

The present invention relates to a carbon nanotube dispersion and a method for producing the same. More particularly, the present invention relates to a carbon nanotube dispersion in which carbon nanotubes are uniformly dispersed in a solvent by applying carbon nanotubes and nitrile rubbers having specific sizes, and a method for producing the same.

Carbon nanotubes have a nano-sized cylindrical shape with a graphite sheet and an sp 2 bond structure. The characteristics of the conductor or semiconductor are shown according to the angle and structure of the graphite surface. In addition, depending on the number of bonds forming the wall, single-walled carbon nanotubes (SWCNTs), double walled carbon nanotubes (DWCNTs), multi-walled carbon nanotubes (MWCNTs) ), And rope carbon nanotubes. In particular, single-walled carbon nanotubes exhibit various electrical, chemical, physical and optical characteristics due to their metallic and semiconducting properties, and by using these properties, more detailed and integrated devices can be realized. Current applications of carbon nanotubes include transparent electrodes, electrostatic dispersion films, field emission devices, surface heating elements, optoelectronics devices, and various sensors and transistors.

However, despite the availability of such carbon nanotubes, the use of carbon nanotubes is limited due to their low solubility and low dispersibility. That is, carbon nanotubes can not stably disperse in an aqueous solution due to a strong van der Waals attractive force between them, and coagulation phenomenon occurs.

In order to solve such a problem, studies have been made on functionalization for modifying the surface of carbon nanotubes and imparting functionality, and one of them is noncovalent functionalization of carbon nanotubes. The non-covalent functionalization of carbon nanotubes refers to hydrogen bond, van der Waals bond, charge transfer, dipole-dipole interaction, π-electron interaction (π- π stacking interaction, etc., to bind the substance to be modified on the surface of the carbon nanotube to impart a desired function. The non-covalent functionalization is advantageous in that functional groups can be imparted while maintaining the intrinsic properties of the tube, since there is no need to induce defects in the carbon nanotube structure. Non-covalent functionalization is usually carried out using surfactants, aromatic hydrocarbons, biomaterials, etc., and most carbon nanotubes are dispersed stably in an aqueous solution.

The method using the aromatic hydrocarbon dispersant is one of the most studied methods among the non-covalent functionalization methods of the carbon nanotubes. The walls of the carbon nanotubes are made of hexagonal graphite structure, and can interact with molecules (dispersants) made of aromatic hydrocarbons such as conjugated polymers.

The conjugated polymer, which has an aromatic ring in the polymer chain, interacts with the wall of the nanotube and interacts with the nanotube. Such conjugated polymers include PmPV (poly (metaphenylene vinylene)), PPE (poly (arylenethynylene)), PPvPV (poly ((2,6-pyridinylenevinylene) -co - [(2,5-dioctyloxy- ), PMMA (Poly (methyl methacrylate)), PAmPV (Poly (5-alkoxym-phenylenevinylene)), PPV (polyphenylene vinylene), cisoidal PPA (polyphenylacetylene) and transoidal PPA.

However, since the conjugated polymer dispersant used in the carbon nanotube dispersion method (non-covalent functionalization method) is expensive, there is a demand for a method of dispersing carbon nanotubes using an inexpensive compound (stabilizer).

An object of the present invention is to provide a carbon nanotube dispersion liquid and a method for producing the same, which can uniformly disperse carbon nanotubes in a solvent.

It is another object of the present invention to provide a carbon nanotube dispersion which can economically disperse carbon nanotubes and a method of manufacturing the same.

It is still another object of the present invention to provide an electronic material produced using the carbon nanotube dispersion.

The above and other objects of the present invention can be achieved by the present invention described below.

One aspect of the present invention relates to a carbon nanotube dispersion. The carbon nanotube dispersion may be a carbon nanotube having a particle size distribution D99 value of 0.5 to 50 탆. Nitrile rubber; And a solvent.

In an embodiment, the content of the total solute including the carbon nanotube and the nitrile rubber is 1 to 15 wt%, the content of the solvent is 85 to 99 wt%, and the content of the carbon nanotubes Is 50 to 90% by weight, and the content of the nitrile rubber is 10 to 50% by weight.

In an embodiment, the carbon nanotubes may include at least one of a single-walled carbon nanotube, a double-walled carbon nanotube, a multi-walled carbon nanotube, and a multi-walled carbon nanotube.

In an embodiment, the nitrile rubber may include at least one of a nitrile rubber including a repeating unit represented by the following formula (1) and a hydrogenated nitrile rubber (HNBR) including a repeating unit represented by the following formula (2) :

[Chemical Formula 1]

Figure pat00001

(2)

Figure pat00002

In the above formulas (1) and (2), m and n are each independently 50 to 250.

In an embodiment, the nitrile rubber may have a weight average molecular weight of from 5,000 to 50,000 g / mol.

In an embodiment, the solvent may include at least one of an organic solvent containing nitrogen atoms (N) having a non-covalent electron pair, and an alcohol having 1 to 4 carbon atoms.

In an embodiment, the carbon nanotube dispersion may further comprise a stabilizer comprising at least one of polyvinylidene fluoride (PVDF), polyvinyl pyrrolidone (PVP), and diisopropyl amine (DIPA) .

Another aspect of the present invention relates to a method for producing a carbon nanotube dispersion. The carbon nanotube slurry is prepared by mixing and adjusting the carbon nanotubes and the solvent so that the D99 value of the particle size distribution of the carbon nanotubes is 0.5 to 50 mu m. Mixing the carbon nanotube slurry with nitrile rubber; .

In an embodiment, the content of the total solute including the carbon nanotube and the nitrile rubber is 1 to 15 wt%, the content of the solvent is 85 to 99 wt%, and the content of the carbon nanotubes Is 50 to 90% by weight, and the content of the nitrile rubber is 10 to 50% by weight.

In the embodiment, the mixing and the particle size may be controlled by a dispersion method including at least one of ultrasonic treatment and milling in the production of the carbon nanotube slurry.

In embodiments, stabilizers comprising at least one of polyvinylidene fluoride (PVDF), polyvinyl pyrrolidone (PVP), and diisopropyl amine (DIPA) may be further mixed with the nitrile rubber.

Another aspect of the present invention relates to electronic materials. The electronic material is manufactured using the carbon nanotube dispersion.

In an embodiment, the electronic material may be a positive electrode or a negative electrode of a secondary battery.

The present invention provides a carbon nanotube dispersion in which carbon nanotubes are uniformly dispersed in a solvent and a method for producing the same, and has the effect of providing an electronic material produced using the carbon nanotube dispersion.

Brief Description of the Drawings Fig. 1 is a photograph of a carbon nanotube dispersion prepared according to Examples 1 to 6 of the present invention by diluting 2,000 times with an NMP solvent, centrifuging at 3,000 rpm for 30 minutes, separating the supernatant, to be.
FIG. 2 is a photograph of the CNT dispersion prepared according to Comparative Examples 1 to 3 of the present invention by diluting 2,000 times with NMP solvent, centrifuging at 3,000 rpm for 30 minutes, separating the supernatant and leaving it for 24 hours to be.

Hereinafter, the present invention will be described in detail.

The carbon nanotube dispersion according to the present invention comprises (A) a carbon nanotube having a D99 value of particle size distribution of 0.5 to 50 탆, (B) a nitrile rubber, and (C) a solvent.

(A) Carbon nanotubes

The carbon nanotubes (CNTs) used in the present invention include, for example, single-walled carbon nanotubes (SWCNTs), double-walled carbon nanotubes (DWCNTs) A multi-walled carbon nanotube (MWCNT), a rope carbon nanotube, or a combination thereof, and has a D99 value of the particle size distribution of 0.5 to 50 mu m, for example, 5 to 30 mu m . Here, D99 value means a value corresponding to 99% when the grain size is converted from a small size to a cumulative percentage. When the D99 value of the particle size distribution is less than 0.5 탆, the electrical conductivity and structural reinforcement effect of the carbon nanotube may be deteriorated or a large cost may be required to control the particle size. When the D99 value is more than 50 탆, It is not uniformly dispersed, and there is a fear that aggregation and precipitation may occur.

The content of the carbon nanotubes (A) may be 50 to 90% by weight, preferably 65 to 90% by weight, of the total solutes (carbon nanotube (A) and nitrile rubber (B)). The carbon nanotubes can be uniformly dispersed in the solvent in the above range.

(B) Nitrile rubber

The nitrile butadiene rubber (NBR) used in the present invention serves as a stabilizer for uniformly dispersing and maintaining the carbon nanotubes in a solvent. For example, the nitrile rubber may be a conventional nitrile rubber including a repeating unit represented by the following formula (1), a hydrogenated nitrile butadiene rubber (HNBR) containing a repeating unit represented by the following formula (2) Mixture, and the like.

[Chemical Formula 1]

Figure pat00003

(2)

Figure pat00004

M and n may be independently from 50 to 250, and m: n may be, for example, from 2: 8 to 8: 2, specifically from 4: 6 to 6: 4, It is not limited.

Specifically, the nitrile rubber may be a hydrogenated nitrile rubber (HNBR).

In an embodiment, the nitrile rubber may have a weight average molecular weight of 5,000 to 50,000 g / mol, preferably 10,000 to 30,000 g / mol. The carbon nanotubes can be uniformly dispersed in the solvent in the above range.

The content of the nitrile rubber (B) may be 10 to 50 wt%, preferably 10 to 35 wt% of the total solutes (carbon nanotube (A) and nitrile rubber (B)). The carbon nanotubes can be uniformly dispersed in the solvent in the above range.

(C) Solvent

Examples of the solvent used in the present invention include organic solvents used in the dispersion of carbon nanotubes, including, but not limited to, N-methylpyrrolidone (NMP), pyridine, morpholine, dimethylaminobenzene, diethylamino An organic solvent containing nitrogen atoms (N) having a pair of non-covalent electrons such as benzene and n-butylamine, an alcohol having 1 to 4 carbon atoms such as methanol, ethanol, propanol and butanol, It does not. N-methylpyrrolidone (NMP) can be preferably used.

In an embodiment, the content of the total solute (carbon nanotube (A) and nitrile rubber (B)) is 1 to 15 wt%, preferably 3 to 7 wt%, and the content of solvent (C) By weight, preferably 93 to 97% by weight. It is possible to obtain a carbon nanotube dispersion homogeneously dispersed in the above range.

The carbon nanotube dispersion according to the present invention may further contain a stabilizer including polyvinylidene fluoride (PVDF), polyvinyl pyrrolidone (PVP), and diisopropyl amine (DIPA) . When the stabilizer is used, 0.1 to 5 parts by weight, for example, 0.2 to 1.5 parts by weight, based on 100 parts by weight of the carbon nanotube dispersion (A + B + C) may be included. The dispersion stability in the above range can be more excellent.

The method for producing a carbon nanotube dispersion according to the present invention is characterized in that the carbon nanotube (A) and the solvent (C) have a D99 value of the particle size distribution of the carbon nanotube (A) of 0.5 to 50 μm And mixing the nitrile rubber (B) with the slurry of carbon nanotubes to prepare a carbon nanotube slurry.

In preparing the carbon nanotube slurry, the mixing and particle size control (dispersion) may be performed by a conventional dispersion method, and may be performed by a dispersion method such as ultrasonic treatment or milling. Specifically, it can be carried out by using a general milling equipment such as a ball mill, a bead mill, and a basket mill, for example, a milling apparatus using a bead mill .

The mixing and particle size control time is not particularly limited as long as the carbon nanotubes can be controlled and dispersed to have a D99 value of the particle size distribution of 50 탆 or less, but may be, for example, 10 minutes to 3 hours.

When the carbon nanotube slurry is used, it is possible to shorten the process time (particularly, the particle size control time) by a method of mixing carbon nanotubes, dispersants, and the like and milling them to control the particle size.

In an embodiment, the nitrile rubber (B) is added in the form of a nitrile rubber solution in which the nitrile rubber (B) is mixed with the solvent (C) so as to include 1 to 15 wt%, for example, 5 to 8 wt% But is not limited thereto. The total solute (A + B) content of the carbon nanotube (A) and the nitrile rubber (B) among the whole carbon nanotube dispersion solution obtained by mixing the carbon nanotube slurry and the nitrile rubber solution is 1 And the solvent (C) is 85 to 99% by weight, the content of the carbon nanotube (A) in the total solute (A + B) is 50 to 90% The content of the rubber (B) should be 10 to 50% by weight.

The carbon nanotube slurry and the nitrile rubber (B) may be mixed without any limitations, such as the above dispersion method, ordinary mixing method such as stirring, and the like. For example, when the nitrile rubber (B) is mixed in the form of a nitrile rubber solution, ease of handling due to dissolution and viscosity of the nitrile rubber can be secured.

The carbon nanotube (A), the nitrile rubber (B) and the solvent (C) are mixed and dispersed such that the D99 value of the particle size distribution of the carbon nanotube (A) is 0.5 to 50 탆, and And adjusting the particle size.

The mixing and particle size control (dispersion) may be performed by a conventional dispersion method, and may be performed by a dispersion method such as ultrasonic treatment or milling. Specifically, it can be carried out by using a general milling equipment such as a ball mill, a bead mill, and a basket mill, for example, a milling apparatus using a bead mill .

The mixing and particle size control time is not particularly limited as long as the DTA value of the carbon nanotubes is controlled to 50 탆 or less and can be dispersed, but may be, for example, 1 to 20 hours.

In an embodiment, the nitrile rubber (B) is added in the form of a nitrile rubber solution in which the nitrile rubber (B) is mixed with the solvent (C) so as to include 1 to 15 wt%, for example, 5 to 8 wt% But is not limited thereto. Wherein the content of the total solute (A + B) including the carbon nanotube (A) and the nitrile rubber (B) in the whole carbon nanotube dispersion is 1 to 15 wt%, and the content of the solvent (C) Wherein the content of the carbon nanotube (A) in the total solute (A + B) is 50 to 90 wt%, the content of the nitrile rubber (B) is 10 to 50 wt% shall.

The method for producing a carbon nanotube dispersion of the present invention may further include the step of adding the stabilizer to further improve dispersion stability. For example, it can be added together with the nitrile rubber.

Another aspect of the present invention relates to an electronic material such as an electrode. The electronic material is produced using the carbon nanotube dispersion.

In an embodiment, the electronic material may be a positive electrode or a negative electrode of a secondary battery. Specifically, the carbon nanotube dispersion may be used as a conductive additive for a cathode active material of a secondary battery or as a substitute for a carbon black of an anode. The manufacture of such a secondary battery anode or cathode can be easily carried out by those skilled in the art.

Hereinafter, the configuration and operation of the present invention will be described in more detail with reference to preferred embodiments of the present invention. It is to be understood, however, that the same is by way of illustration and example only and is not to be construed in a limiting sense.

The contents not described here are sufficiently technically inferior to those skilled in the art, and a description thereof will be omitted.

Example

Example  One

(Nynocyl, product name: NC7000) was added to 77.75% by weight of N-methylpyrrolidone (NMP) solvent and the mixture was milled using a milling equipment (manufacturer: Buhler, Mill) to adjust the D99 value of the particle size distribution to be 24.3 탆. A hydrogenated nitrile rubber (weight average molecular weight: 16,200 g / mol) containing recurring units represented by the following formula (2) was added to a carbon nanotube slurry (CNT slurry) , n: methylpyrrolidone (NMP) solution containing m: n = 4: 6) was added and stirred and stabilized for 5 hours to prepare a carbon nanotube dispersion.

(2)

Figure pat00005

Example  2

(Nynocyl, product name: NC7000) was added to 77.25% by weight of N-methylpyrrolidone (NMP) solvent and the mixture was milled using a milling equipment (manufacturer: Buhler, To adjust the D99 value of the particle size distribution to 18.8 탆. 18.75 wt% of the nitrile rubber solution of Example 1 and 0.5 wt% of polyvinylpyrrolidone (PVP, manufacturer: Sigma Aldrich, product name: PVP10) were added to a carbon nanotube slurry having controlled particle sizes, And the mixture was stirred and stabilized for 5 hours to prepare a carbon nanotube dispersion.

Example  3

(Nynocyl, product name: NC7000) was added to 77.25% by weight of N-methylpyrrolidone (NMP) solvent and the mixture was milled using a milling equipment (manufacturer: Buhler, To adjust the D99 value of the particle size distribution to be 20.4 占 퐉. 18.75 weight% of the nitrile rubber solution of Example 1 and 0.5 weight% of polyvinylidene fluoride (PVDF, manufactured by Solvay, product name: SOLEF 6020) was added, and the mixture was stirred and stabilized for 5 hours to prepare a carbon nanotube dispersion.

Example  4

3.5 wt% of carbon nanotubes (manufactured by Nynocyl, product name: NC7000) was added to 83 wt% of N-methylpyrrolidone (NMP) solvent and milling equipment (manufacturer: Buhler, To adjust the D99 value of the particle size distribution to be 15.4 占 퐉. 12.5% by weight of the nitrile rubber solution of Example 1 and 1% by weight of diisopropylamine (DIPA, manufactured by Nippon Kayaku Co., Ltd., product name: diisopropylamine, product name: CNT slurry) EP grade) was added, and the mixture was stirred and stabilized for 5 hours to prepare a carbon nanotube dispersion.

Example  5

7.5 weight% of carbon nanotube (manufacturer: Nynocyl, product name: NC7000) and 43.75 weight% of the nitrile rubber solution of Example 1 were added to 48.75% by weight of N-methylpyrrolidone (NMP) ) Apparatus (manufacturer: Buhler, device name: K8) to adjust the D99 value of the particle size distribution to be 22.2 쨉 m to prepare a carbon nanotube dispersion.

Example  6

(Manufactured by Nynocyl, product name: NC7000) and 31.25% by weight of the nitrile rubber solution of Example 1 were added to 59.25% by weight of N-methylpyrrolidone (NMP) ) Equipment (manufacturer: Buhler, device name: K8) to adjust the D99 value of the particle size distribution to 34.6 탆. Next, diisopropylamine (DIPA, manufacturer: purified gold, product name: diisopropylamine, EP grade) was added and stirred and stabilized for 5 hours to prepare a carbon nanotube dispersion.

Comparative Example  One

3.5 wt% of carbon nanotubes (manufactured by Nynocyl, product name: NC7000) was added to 95 wt% of N-methylpyrrolidone (NMP) solvent, and a milling equipment (manufacturer: Buhler, To adjust the D99 value of the particle size distribution to 38.8 탆. 1.5% by weight of polyvinylpyrrolidone (PVP, manufacturer: Sigma Aldrich, product name: PVP10) was added to a carbon nanotube slurry having a controlled particle size, stirred and stabilized for 5 hours, A tube dispersion was prepared.

Comparative Example  2

3.5 wt% of carbon nanotubes (manufactured by Nynocyl, product name: NC7000) was added to 95 wt% of N-methylpyrrolidone (NMP) solvent, and a milling equipment (manufacturer: Buhler, To adjust the D99 value of the particle size distribution to be 40.3 mu m. 1.5% by weight of polyvinylidene fluoride (PVDF, manufacturer: Solvay, product name: SOLEF 6020) was added to a carbon nanotube slurry having a controlled particle size distribution, stirred and stabilized for 5 hours To prepare a carbon nanotube dispersion.

Comparative Example  3

(Manufactured by Nynocyl, product name: NC7000) and 18.75% by weight of the nitrile rubber solution of Example 1 were added to 77.75% by weight of N-methylpyrrolidone (NMP) And the mixture was stirred and stabilized to prepare a carbon nanotube dispersion (D99 value of carbon nanotube particle size distribution: 380 mu m).

Property evaluation method

1. Evaluation of Dispersibility: The prepared carbon nanotube dispersion was diluted 2,000 times with NMP solvent, centrifuged at 3,000 rpm for 30 minutes, and the supernatant was collected. After the supernatant was left at room temperature for 24 hours, the bottom and the wall were observed with naked eyes. Figures 1 and 2 show photographs, respectively. Good when no precipitate was formed, and poor when fine precipitate was generated.

2. Transmittance (%): The prepared carbon nanotube dispersion was diluted 2,000 times with NMP solvent and centrifuged at 3,000 rpm for 30 minutes. The supernatant was collected and UV-visible spectra were taken at a wavelength of 550 nm to determine the transmittance Respectively. The higher the degree of dispersion of carbon nanotubes, the lower the transmittance.

3. Particle size analysis: The prepared carbon nanotube dispersion was diluted 2,000 times with NMP solvent, and the D99 value of the carbon nanotube particle size distribution was measured using a Mastersizer 3000 instrument from Malvern.

Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Comparative Example 1 Comparative Example 2 Comparative Example 3 menstruum 95 94.5 94.5 94.5 89 88 95 95 95 CNT 3.5 3.5 3.5 3.5 7.5 7.5 3.5 3.5 3.5 Nitrile
Rubber
1.5 1.5 1.5 One 3.5 2.5 0 0 1.5
PVP 0 0.5 0 0 0 0 1.5 0 0 PVDF 0 0 0.5 0 0 0 0 1.5 0 DIPA 0 0 0 One 0 2 0 0 0 Dispersibility × × × Permeability (%) 62 51 53 55 59 64 76 81 92

From the above results, it can be seen that the carbon nanotube dispersions (Examples 1 to 6) of the present invention have a stable dispersibility even after being left for 24 hours, and the dispersion degree is high due to low UV-visible permeability even at 3,000 rpm by centrifugation .

On the other hand, when nitrile rubber is not used (Comparative Examples 1 and 2) and the D99 value of the particle size distribution of carbon nanotubes exceeds 50 m (Comparative Example 3), carbon nanotube precipitation occurs and UV-visible The dispersibility is remarkably lowered compared with the dispersion of the present invention since the permeability is high.

It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (13)

Carbon nanotubes having a particle size distribution D99 value of 0.5 to 50 탆;
Nitrile rubber; And
Wherein the carbon nanotube dispersion comprises a solvent.
The method according to claim 1, wherein the content of the total solute including the carbon nanotube and the nitrile rubber is 1 to 15% by weight, the content of the solvent is 85 to 99% by weight, Is from 50 to 90% by weight, and the content of the nitrile rubber is from 10 to 50% by weight.
The carbon nanotube dispersion according to claim 1, wherein the carbon nanotubes include at least one of a single-walled carbon nanotube, a double-walled carbon nanotube, a multi-walled carbon nanotube, and a multi-walled carbon nanotube.
The nitrile rubber according to claim 1, wherein the nitrile rubber comprises at least one of a nitrile rubber including a repeating unit represented by the following formula (1) and a hydrogenated nitrile rubber (HNBR) comprising a repeating unit represented by the following formula Carbon nanotube dispersion liquid characterized by:
[Chemical Formula 1]
Figure pat00006

(2)
Figure pat00007

In the above formulas (1) and (2), m and n are each independently 50 to 250.
The carbon nanotube dispersion according to claim 1, wherein the nitrile rubber has a weight average molecular weight of 5,000 to 50,000 g / mol.
The carbon nanotube dispersion according to claim 1, wherein the solvent comprises at least one of an organic solvent containing nitrogen atoms (N) having a pair of non-covalent electrons, and an alcohol having 1 to 4 carbon atoms.
The method of claim 1, wherein the carbon nanotube dispersion further comprises a stabilizer comprising at least one of polyvinylidene fluoride (PVDF), polyvinyl pyrrolidone (PVP), and diisopropyl amine (DIPA) Carbon nanotube dispersion.
Mixing and adjusting the carbon nanotubes and the solvent so that the D99 value of the particle size distribution of the carbon nanotubes is 0.5 to 50 占 퐉 to prepare a carbon nanotube slurry; And
Mixing the carbon nanotube slurry with nitrile rubber;
≪ / RTI > carbon nanotube dispersion.
9. The method according to claim 8, wherein the total solute including the carbon nanotube and the nitrile rubber is 1 to 15% by weight, the solvent content is 85 to 99% by weight, Wherein the content of the nitrile rubber is 50 to 90% by weight, and the content of the nitrile rubber is 10 to 50% by weight.
[9] The method of claim 8, wherein the carbon nanotube slurry is prepared by a dispersion method including at least one of ultrasonic treatment and milling.
The method according to claim 8, further comprising mixing a stabilizer comprising at least one of polyvinylidene fluoride (PVDF), polyvinyl pyrrolidone (PVP), and diisopropyl amine (DIPA) together with the nitrile rubber Wherein the carbon nanotube dispersion is prepared by a method comprising the steps of:
An electronic material produced by using the carbon nanotube dispersion according to any one of claims 1 to 7.
The electronic material according to claim 12, wherein the electronic material is a positive electrode or a negative electrode of a secondary battery.
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