KR20170023345A - Method for preparing dispersion sol of boron nitride nanosheet by microwave heating and dispersion sol of boron nitride nanosheet prepared by the method - Google Patents

Method for preparing dispersion sol of boron nitride nanosheet by microwave heating and dispersion sol of boron nitride nanosheet prepared by the method Download PDF

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KR20170023345A
KR20170023345A KR1020150118082A KR20150118082A KR20170023345A KR 20170023345 A KR20170023345 A KR 20170023345A KR 1020150118082 A KR1020150118082 A KR 1020150118082A KR 20150118082 A KR20150118082 A KR 20150118082A KR 20170023345 A KR20170023345 A KR 20170023345A
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boron nitride
dispersion sol
nitride nanosheet
microwave
nanosheet
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KR1020150118082A
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Korean (ko)
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KR101746529B1 (en
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김대성
이현진
김효태
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한국세라믹기술원
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/06Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/064Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
    • C01B21/0648After-treatment, e.g. grinding, purification
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122Incoherent waves
    • B01J19/126Microwaves
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641Nitrides
    • C23C14/0647Boron nitride

Abstract

The present invention relates to a process for producing a boron nitride nanosheets dispersion sol using microwave and a boron nitride nanosheet dispersion sol prepared therefrom, wherein a hexavalent boron nitride is dispersed in a solvent and produced by a microwave hydrothermal reaction method, And it is economically advantageous in terms of yield and processing cost in the manufacturing process. More particularly, the present invention relates to a process for producing a boron nitride nanosheet dispersion sol having excellent heat dissipation and heat resistance characteristics and applicable to an organic material and hybridization, and a boron nitride nanosheet dispersion sol produced therefrom.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a boron nitride nanosheet dispersed sol using a microwave and a boron nitride nanosheet dispersed sol prepared therefrom,

The present invention relates to a process for producing a boron nitride nanosheets dispersion sol by microwave and a boron nitride nanosheet dispersion sol produced therefrom, wherein the hexavalent boron nitride is dispersed in a solvent and produced by a microwave hydrothermal reaction method, The present invention relates to a process for producing a boron nitride nanosheet dispersed sol which is excellent in organic solvent and hybridization, and to a boron nitride nanosheet dispersion sol produced therefrom.

Boron nitride (BN) is a stable graphite-like material whose chemical and physical properties are similar to graphite, because boron atoms and nitrogen atoms form a planar two-dimensional hexagonal structure and have a hexagonal structure similar to graphite. to be. Hexagonal boron nitride has excellent thermal conductivity, corrosion resistance, heat resistance, electrical insulation, and is used as an additive in various substrates.

Recently, as demand and interest in nanotechnology grows, research is underway to obtain boron nitride in the form of nanosheets and nanotubes. Currently, hexagonal boron nitride nanosheets are manufactured by mechanical separation, boron nitride intercalation compound method, and chemical vapor deposition (CVD).

The mechanical method is a method in which single or multi-layer boron nitride is removed from hexagonal boron nitride by ultrasonic treatment in a solvent, but the boron nitride nanosheet can be simply produced, but it is difficult to mass-produce it.

As the boron nitride interlayer compound method, a single layer of boron nitride can be prepared by preparing a dispersion in which a functional group such as a hydroxy group is bonded to hexagonal boron nitride to relax the interlayer attraction and improve the affinity between the functional group and the solvent , There is a disadvantage that the yield of the single layer boron nitride produced is low.

The CVD method is a method in which a catalyst metal is deposited on a substrate to form a thin metal film, then a gas containing boron and nitrogen is flowed at a high temperature and then cooled to obtain a boron nitride nanosheet formed on the metal film. It has disadvantages in terms of area and price.

Korean Patent No. 10-1212717 Korean Patent Publication No. 10-2013-0115910

An object of the present invention is to provide a method for producing a crystalline boron nitride nanosheet dispersion sol having excellent dispersibility and stability using a microwave in a short time.

It is another object of the present invention to provide a coating film having excellent heat dissipation and heat resistance by applying a boron nitride nanosheet dispersion sol prepared by the method for producing a boron nitride nanosheet dispersion sol of the present invention to an organic hybrid coating material.

In order to achieve the above object, the present invention provides a method for producing a boron nitride nanosheet dispersed sol using microwave, comprising the steps of: dispersing hexagonal boron nitride in a solvent; A microwave hydrothermal reaction step in which the dispersed boron nitride is reacted in a microwave hydrothermal reactor; And an ultrasonic treatment step of ultrasonic-treating the reacted boron nitride.

The solvent in the dispersion step may include at least one selected from the group consisting of alcohols, glycols, and dimethylformamide, and the glycols may include at least one of ethylene glycol and polyethyleneglycol.

The microwave hydrothermal reaction may be performed at a reaction temperature of 50 to 200 ° C and a reaction time of 10 minutes to 5 hours. In addition, the microwave hydrothermal reaction step may be performed in a closed or open microwave hydrothermal reactor.

The present invention can provide a boron nitride nanosheet dispersion sol produced by the above-described production method. The boron nitride nanosheet may have an average particle diameter of 0.1 to 10 mu m and a thickness of 1 to 100 nm.

In addition, the present invention can provide a coating agent comprising the boron nitride nanosheet dispersion sol prepared by the above-described method.

The boron nitride nanosheet dispersion sol using microwave according to the present invention is advantageous in that the peeling process is effectively performed within a short period of time, so that it is easy to manufacture and economical in terms of yield and processing cost in the manufacturing process.

1 is a flowchart showing a method for producing a boron nitride nanosheet dispersion sol according to the present invention.
FIG. 2 is a photograph showing a result of analysis of a boron nitride nanosheet prepared according to Example 2 by a Field Emission Scanning Electron Microscope (FE-SEM).
3 is a photograph showing the result of analysis of a boron nitride nanosheet prepared according to Example 2 by a transmission electron microscope (TEM).
4 is a photograph showing a result of analysis of a boron nitride nanosheet prepared according to Example 2 by an atomic force microscope (AFM).

Advantages and features of the present invention and methods of achieving them will become apparent with reference to the embodiments described in detail below. The present invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. To fully disclose the scope of the invention to those skilled in the art, and the invention is only defined by the scope of the claims.

Unless defined otherwise, all terms (including technical and scientific terms) used herein may be used in a sense commonly understood by one of ordinary skill in the art to which this invention belongs. In addition, commonly used predefined terms are not ideally or excessively interpreted unless explicitly defined otherwise.

The present invention relates to a process for producing a boron nitride nanosheets dispersion sol by microwave and a boron nitride nanosheet dispersion sol produced therefrom, wherein the hexavalent boron nitride is dispersed in a solvent and produced by a microwave hydrothermal reaction method, A method of preparing a boron nitride nanosheet dispersed sol which is excellent in organic materials and hybridization, and a boron nitride nanosheet dispersion sol prepared therefrom.

First, a method for producing a boron nitride nanosheet dispersion sol using a microwave according to the present invention includes: a dispersion step of dispersing hexagonal boron nitride in a solvent; A microwave hydrothermal reaction step in which the dispersed boron nitride is reacted in a microwave hydrothermal reactor; And an ultrasonic treatment step of ultrasonic-treating the reacted boron nitride.

The dispersing step is a step of dispersing hexagonal boron nitride in a solvent. The solvent is not particularly limited, but may include at least one selected from the group consisting of alcohols, glycols, and dimethylformamide, May include at least one of ethylene glycol and polyethylene glycol.

The microwave hydrothermal reaction step is a step of reacting the dispersed boron nitride in a microwave hydrothermal reactor to weaken or activate the binding force of van der Waals force between layers of a single sheet of boron nitride by microwave irradiation.

In the microwave hydrothermal reaction step, the reaction temperature may be 50 to 200 ° C, and the reaction time may be 10 minutes to 5 hours, preferably 30 minutes to 3 hours.

If the reaction temperature is less than 50 ° C, there is a problem that the pretreatment effect on the heat treatment is not exhibited. If the reaction temperature exceeds 200 ° C, there is a problem in loss of the energy source supplied and commercialization due to the need for the reactor designed for high temperature and high pressure. If the reaction time is less than 10 minutes, the reaction time tends to be shorter and the pretreatment effect does not appear. On the other hand, if the reaction time exceeds 5 hours, there is a disadvantage of energy loss not.

In addition, the microwave hydrothermal reaction step may be performed in a closed or open microwave hydrothermal reactor.

The ultrasonic wave treatment step may include ultrasonic treatment in which ultrasonic waves are applied to boron nitride which has weakened or activated the interlayer coupling force of the single sheet through the microwave hydrothermal reaction step to be peeled off into a boron nitride nanosheet to form a boron nitride nanosheet dispersion sol . The boron nitride nanosheet may have an average particle diameter of 0.1 to 10 mu m, preferably 0.5 to 7 mu m, and a thickness of 1 to 100 nm, preferably 1 to 50 nm.

Next, the boron nitride nanosheet dispersion sol of the present invention is a boron nitride nanosheet having an average particle diameter of 0.1 to 10 mu m, a thickness of 1 to 100 nm and formed by removing hexagonal boron nitride; And a dispersion solvent.

The dispersion solvent may include at least one selected from the group consisting of alcohols, glycols, and dimethylformamide, and the glycols may include at least one of ethylene glycol and polyethyleneglycol.

In addition, the present invention can provide a coating film having excellent heat dissipation and heat resistance by applying the prepared boron nitride nanosheet dispersion sol to an organic-inorganic hybrid coating material.

Hereinafter, the present invention will be described in detail with reference to the following examples, which should not be construed as limiting the scope of protection defined by the appended claims.

Example  One

0.2 g of boron nitride powder (average particle diameter: 12 탆) was dispersed in 100 ml of ethylene glycol (EG) solvent, and the resultant was placed in a microwave apparatus in a closed microwave hydrothermal reactor. And reacted for 30 minutes. The solution in which the reaction was completed was sonicated for 3 hours.

The dispersion exhibited a liquid crystal phase, diluted to make it transparent, and exhibited a tinning phenomenon when the laser was shined.

Example  2

The same procedure as in Example 1 was followed except that the heat treatment time was 1 hour.

Example  3

The same procedure as in Example 1 was followed except that the heat treatment time was 2 hours.

Example  4

The same procedure as in Example 1 was followed except that the heat treatment time was 3 hours.

Example  5

0.2 g of boron nitride powder (average particle diameter 12 占 퐉) was dispersed in 100 ml of ethylene glycol (EG) solvent. Then, in an open microwave hydrothermal reactor in a microwave apparatus, a quartz- The reaction solution was placed in a bottom flask, and the temperature of the reaction solution was raised to 150 캜 and allowed to react for 1 hour. The solution in which the reaction was completed was sonicated for 3 hours.

The dispersion exhibited a liquid crystal phase, diluted to make it transparent, and exhibited a tinning phenomenon when the laser was shined.

Example  6

The procedure was carried out in the same manner as in Example 5 except that the microwave heat treatment time was changed to 3 hours.

Comparative Example  One

0.2 g of boron nitride powder (average particle size of 12 탆) was dispersed in 100 ml of ethylene glycol (EG) solvent, and the autoclave was heated to 150 캜 for reaction for 24 hours. The solution in which the reaction was completed was sonicated for 3 hours.

Comparative Example  2

0.2 g of boron nitride powder (average particle size of 12 탆) was dispersed in 100 ml of isopropyl alcohol (IPA) solvent, and the autoclave was heated to 150 캜 for reaction for 24 hours. The solution in which the reaction was completed was sonicated for 3 hours.

Comparative Example  3

0.2 g of boron nitride powder (average particle size of 12 탆) was dispersed in 100 ml of ethylene glycol (EG) solvent, and ultrasonic treatment was performed for 3 hours.

Property evaluation

≪ Measurement of peeled particles &

The peeled-off particles were measured using a JEM-2000 Transmission Electron Microscope (JEOL) TEM apparatus and a JEOL JSM-7610F Field Emission Scanning Electron Microscope (FE-SEM) apparatus. The peeled sample was dropped on a TEM grid (carbon-coated 200 mesh copper grid) and dried in a 60 ° C oven for at least 6 hours to remove any residual solvent and measure the peeled particles.

As shown in Fig. 2, the shape of the particles of the boron nitride nanosheet prepared in Example 2 was analyzed by a field emission scanning electron microscope, and it was confirmed that the particle size had a particle size of 1-3 mu m.

As shown in Fig. 3, the boron nitride nanosheet prepared in Example 2 was analyzed by a transmission electron microscope. As a result, a nanosheet having a grain size of about 1 탆 and a thickness of about 1 nm was observed .

≪ Measurement of peel particle thickness &

The particle thickness was measured with an Atomic Force Microscope (AFM) instrument. The surface of the Si wafer was coated with the peeled platelets, the probe was suspended at the end of the cantilever, and a small needle And the tunnel current was measured to measure the atomic phase of the surface.

As shown in Fig. 4, the boron nitride nanosheet prepared in Example 2 was analyzed by AFM, and as a result, a nanosheet having a particle diameter of 0.5-1 탆 and a thickness of about 4-24 nm was observed.

<Measurement of peel particle size>

The particle size was measured using ELS-Z equipment manufactured by Otsuka Co., Ltd. The nanosheet dispersion was diluted and the particle size was measured after ultrasonic treatment for 3 minutes to remove bubbles.

The boron nitride nanosheets dispersion sol prepared in Examples and Comparative Examples of the present invention were measured according to the physical property evaluation method, and the measurement results are shown in Table 1 below.

Particle size (탆) Thickness (nm) Nanosheet yield (%)

Example
One 1.48 5-50 67
2 1.45 5-30 73 3 1.45 2-15 84 4 1.3 1-10 92 5 2.9 10-25 86 6 2.1 4-20 89
Comparative Example
One 0.29 15-20 78
2 0.31 14-65 68 3 8.2 20-56 63

In Examples 1 to 4, boron nitride nanosheets obtained by ultrasonic treatment of boron nitride particles produced according to heat treatment time using a closed microwave hydrothermal reactor were observed. In the case of Example 4, 1, it was confirmed that the nanosheet particles became smaller and the thickness became thinner after the ultrasonic treatment. It was also found that the yield of the nanosheet was increased as the thickness became thinner.

Examples 5 and 6 were obtained by observing boron nitride nanosheets prepared by ultrasonic treatment after heat treatment using an open microwave hydrothermal reactor. As compared with Example 5, the particle size and thickness of Example 6 were smaller than those of Example 5, .

On the other hand, Comparative Examples 1 and 2 are boron nitride nanosheets produced by ultrasonic treatment after heat treatment by a hydrothermal reaction, and the particle size is smaller than those of the examples. However, since the particle size is decreased as the time is longer than that of the embodiment, do. If the particle size is too small, the interface for heat transfer increases in terms of heat dissipation characteristics, which may adversely affect the heat dissipation control. Further, if the process time is long, energy is lost.

Comparative Example 3 is a boron nitride nanosheet prepared by ultrasonic wave alone treatment without hydrothermal treatment, and has a smaller particle size and lower yield than the Examples and Comparative Examples. Particularly, there is a problem that the uniform dispersion due to the organic / inorganic hybridization is difficult due to the large particle size and the precipitation occurs.

On the other hand, in the case of the boron nitride nanosheet processed by microwave in a short time, it can be seen that the size of 1 mu m or more is maintained even though the thickness is thin. Therefore, the embodiments of the present invention in which the peeling process is effective in a short time are superior to the comparative examples.

Claims (7)

A dispersing step of dispersing hexagonal boron nitride in a solvent;
A microwave hydrothermal reaction step in which the dispersed boron nitride is reacted in a microwave hydrothermal reactor; And
And an ultrasonic treatment step of ultrasonic-treating the reacted boron nitride.
The method according to claim 1,
Wherein the solvent of the dispersing step comprises at least one selected from the group consisting of alcohols, glycols, and dimethylformamide.
3. The method of claim 2,
Wherein the glycols include at least one of ethylene glycol and polyethyleneglycol.
The method according to claim 1,
Wherein the microwave hydrothermal reaction step is a microwave-assisted nanosheet dispersion sol having a reaction temperature of 50 to 200 DEG C and a reaction time of 10 minutes to 5 hours.
The method according to claim 1,
Wherein the microwave hydrothermal reaction step is performed in a closed or open microwave hydrothermal reactor.
A boron nitride nanosheet dispersion sol produced by the production method according to any one of claims 1 to 5,
Wherein the nanosheet has an average particle diameter of 0.1 to 10 mu m and a thickness of 1 to 100 nm.
A coating agent comprising the boron nitride nanosheets dispersion sol according to claim 6.


KR1020150118082A 2015-08-21 2015-08-21 Method for preparing dispersion sol of boron nitride nanosheet by microwave heating and dispersion sol of boron nitride nanosheet prepared by the method KR101746529B1 (en)

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN110683573A (en) * 2019-11-18 2020-01-14 河北工业大学 Method for preparing indium oxide nanotube by using porous BN nano fiber as template
KR102122019B1 (en) * 2019-04-26 2020-06-11 서울대학교산학협력단 Polyolefin nanocomposites with functionalized boron nitride and manufacturing method thereof
CN111807335A (en) * 2020-07-08 2020-10-23 陕西科技大学 Microwave-assisted method for preparing boron nitride nanosheets

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KR102155067B1 (en) * 2018-11-30 2020-09-11 한국생산기술연구원 manufacturing method for two-dimensional calcium carbonate nano sheet and two-dimensional calcium carbonate nano sheet manufactured thereby
KR20230037904A (en) * 2021-09-10 2023-03-17 (주)알킨스 Manufacturing mehtod of Large h-BNNS dispersion solution by solvothermal method

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KR20130115910A (en) 2012-04-13 2013-10-22 삼성전자주식회사 Hexagonal boron nitride and substrate assembly including the same

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KR101212717B1 (en) 2011-02-23 2012-12-14 한국과학기술원 Method of forming high-quality hexagonal boron nitride nanosheet using multi component eutectic point system
KR20130115910A (en) 2012-04-13 2013-10-22 삼성전자주식회사 Hexagonal boron nitride and substrate assembly including the same

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KR102122019B1 (en) * 2019-04-26 2020-06-11 서울대학교산학협력단 Polyolefin nanocomposites with functionalized boron nitride and manufacturing method thereof
CN110683573A (en) * 2019-11-18 2020-01-14 河北工业大学 Method for preparing indium oxide nanotube by using porous BN nano fiber as template
CN111807335A (en) * 2020-07-08 2020-10-23 陕西科技大学 Microwave-assisted method for preparing boron nitride nanosheets
CN111807335B (en) * 2020-07-08 2023-01-31 陕西科技大学 Microwave-assisted method for preparing boron nitride nanosheets

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