KR20120119487A - Manufacturing method of nano fluid containing metal treated carbon nano particle - Google Patents

Manufacturing method of nano fluid containing metal treated carbon nano particle Download PDF

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KR20120119487A
KR20120119487A KR1020110037444A KR20110037444A KR20120119487A KR 20120119487 A KR20120119487 A KR 20120119487A KR 1020110037444 A KR1020110037444 A KR 1020110037444A KR 20110037444 A KR20110037444 A KR 20110037444A KR 20120119487 A KR20120119487 A KR 20120119487A
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carbon nanoparticles
metal
carbon
acid
hydroxide
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KR1020110037444A
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Korean (ko)
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구자운
이시춘
홍대승
이태성
오원춘
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엔바로테크 주식회사
오원춘
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Priority to KR1020110037444A priority Critical patent/KR20120119487A/en
Priority to PCT/KR2011/003187 priority patent/WO2012144679A1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/10—Liquid materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30

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  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
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  • Nanotechnology (AREA)
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  • Inorganic Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • Combustion & Propulsion (AREA)
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  • Materials Engineering (AREA)
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  • Manufacturing & Machinery (AREA)
  • Health & Medical Sciences (AREA)
  • Carbon And Carbon Compounds (AREA)
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Abstract

PURPOSE: A manufacturing method of nano-fluid in which metal-processed carbon nano-particles is provided to waterborne the carbon nano-particles into a metal hydroxide aqueous solution. CONSTITUTION: A manufacturing method of nano-fluid in which metal-processed carbon nano-particles comprises the following steps: milling carbonaceous materials(s101); processing the milled the surface of carbon nano-particles with acid(s103); drying the acidified carbon nano-particles(s105); heat treating the dried carbon nano-particles(s107); and mixing the heat treated carbon nano-particles with the metal hydroxide aqueous solution, and irradiating the ultrasonic wave(s109). The carbonaceous material is one or more selected from activated charcoal, activated carbon fiber, carbon black and graphene. The first step is processed with tumbling ball mill and mono planar mill for 48 hours. [Reference numerals] (AA) Start; (BB) End; (S101) Milling step; (S103) Acid treating step; (S105) Drying step; (S107) Heat treating step; (S109) Irradiating ultrasonic wave step

Description

금속처리된 탄소 나노입자가 함유된 나노유체의 제조방법{MANUFACTURING METHOD OF NANO FLUID CONTAINING METAL TREATED CARBON NANO PARTICLE}MANUFACTURING METHOD OF NANO FLUID CONTAINING METAL TREATED CARBON NANO PARTICLE}

본 발명은 나노유체의 제조방법에 관한 것으로, 더욱 상세하게는 냉각기, 열교환기 및 윤활성이 요구되는 산업 전반에 사용 가능한 특성을 나타내는 금속처리된 탄소 나노입자가 함유된 나노유체의 제조방법에 관한 것이다.
The present invention relates to a method for producing a nanofluid, and more particularly, to a method for producing a nanofluid containing metal-treated carbon nanoparticles exhibiting properties that can be used throughout the industry requiring coolers, heat exchangers and lubricity. .

본 발명은 나노유체의 제조방법에 관한 것으로, 더욱 상세하게는 냉각기, 열교환기 및 윤활성이 요구되는 산업 전반에 사용 가능한 특성을 나타내는 금속처리된 탄소 나노입자가 함유된 나노유체의 제조방법에 관한 것이다.The present invention relates to a method for producing a nanofluid, and more particularly, to a method for producing a nanofluid containing metal-treated carbon nanoparticles exhibiting properties that can be used throughout the industry requiring coolers, heat exchangers and lubricity. .

현재, 국내 나노기술 수준은 선진국 대비 2001년 약 25%에서 2005년 66% 수준으로 향상된 것으로 평가되며, SCI 논문 및 특허 수는 세계 5위를 차지하고 있고 Lux Research (2005년도)는 우리나라를 나노기술분야에 있어 4대 강국으로 평가하고 있다.Currently, Korea's nanotechnology level is estimated to have improved from about 25% in 2001 to 66% in 2005, compared to developed countries, and the number of SCI papers and patents is ranked 5th in the world. It is rated as the 4th power in the world.

나노유체에 관한 연구는 주로 CuO, Al2O3 입자를 분산시킨 나노유체에 대하여 수행되어 왔으며 CNT에 대한 연구도 보고되고 있으며, 기본 유체 및 입자분율에 따라 10 내지 150%의 열전도도 증가 효과를 나타내고 있다. 또한, Xuan, Ding 등 몇몇 연구자들은 이들 나노유체의 대류 열전달 상승효과에 대하여 실험적 결과를 발표하고 있으며, 대류 열전달에 나노유체의 적용시 열전달 상승효과보다 수배 내지 수십배가 증가한다고 보고되고 있다.Research on nanofluids has been carried out mainly on nanofluids in which CuO and Al2O3 particles are dispersed, and studies on CNTs have been reported, and the thermal conductivity of 10 to 150% is increased depending on the basic fluid and particle fraction. In addition, several researchers, such as Xuan and Ding, have published experimental results on the convective heat transfer synergistic effects of these nanofluids, and reported that the application of nanofluids to convective heat transfer increases several times to tens of times.

이는 입자에 의한 나노유체 열전달 상승에 의한 열전달 상승뿐만 아니라 유체내 입자 이동 및 열경계층 교란에 의한 추가적인 열전달 상승효과로 기인한다고 추측되고 있다.This is presumed to be due to the heat transfer increase due to the increase of nanofluid heat transfer by the particles, as well as the additional heat transfer increase effect due to the particle movement in the fluid and the thermal boundary layer disturbance.

우리나라의 경우 에너지의 해외 의존도가 97% 정도나 될 만큼 에너지원의 해외 의존도가 매우 높다. 따라서 에너지 이용 효율을 획기적으로 향상시킬 수 있는 고효율의 열교환 장치가 필요하다. 또한 온실가스 감축을 위한 기후변화협약 의정서가 채택, 공식 발효됨에 따라 화석연료 사용 저감을 통해 이산화탄소 등의 배출가스를 저감할 수 있는 국내 고유기술 확보가 매우 시급히 요구되고 있다. 따라서 에너지원을 자체 개발할 수 있는 단계에 이르기까지는 기존 설비의 에너지 소모량을 최대한 줄일 수 있도록 장치의 효율을 극대화시키는 작업이 필요하다. 이러한 관점에서 본 연구에서 개발된 나노유체를 각종 열교환 장치에 적용함으로써 에너지 사용량을 저감하여 에너지 비용을 획기적으로 줄일 수 있을 것으로 예상된다.In Korea, energy dependence abroad is very high, with 97% dependence on energy overseas. Therefore, there is a need for a high efficiency heat exchanger that can dramatically improve energy utilization efficiency. Also, with the adoption and official entry into force of the Climate Change Convention to reduce greenhouse gases, there is an urgent need to secure unique domestic technologies that can reduce emissions such as carbon dioxide by reducing the use of fossil fuels. Therefore, until the stage where the energy source can be developed by itself, it is necessary to maximize the efficiency of the device so as to reduce the energy consumption of the existing facilities as much as possible. In view of this, the nanofluid developed in this study can be applied to various heat exchangers to reduce energy consumption and significantly reduce energy costs.

이러한 에너지 사용의 저감은 단순히 금전적 측면의 이익뿐 아니라, 에너지원의 사용으로 인한 대기오염 및 온실가스 발생을 저감시킴으로써 환경문제의 해결에도 일부분 기여하게 된다.
This reduction in energy use not only provides financial benefits, but also contributes to solving environmental problems by reducing air pollution and greenhouse gas emissions caused by the use of energy sources.

본 발명의 목적은 냉각, 열교환 및 윤활성이 우수한 금속처리된 탄소 나노입자가 함유된 나노유체의 제조방법을 제공하는 것이다.
An object of the present invention is to provide a method for producing nanofluids containing metal-treated carbon nanoparticles having excellent cooling, heat exchange and lubricity.

본 발명의 목적은 탄소질 재료를 밀링하는 밀링단계, 상기 밀링단계를 거친 탄소 나노입자의 표면을 산으로 처리하는 산처리단계, 상기 산처리단계를 거친 탄소 나노입자를 건조하는 건조단계, 상기 건조단계를 거친 탄소 나노입자를 열처리하는 열처리단계 및 상기 열처리단계를 거친 탄소 나노입자를 금속 수산화물 수용액과 혼합하고 초음파를 조사하는 수분산단계로 이루어지는 것을 특징으로 하는 금속처리된 탄소 나노입자가 함유된 나노유체의 제조방법을 제공함에 의해 달성된다.An object of the present invention is a milling step of milling a carbonaceous material, an acid treatment step of treating the surface of the carbon nanoparticles subjected to the milling step with an acid, a drying step of drying the carbon nanoparticles subjected to the acid treatment step, the drying Nano-contained metal-treated carbon nanoparticles comprising a heat treatment step of heat-treating the carbon nanoparticles, and the water dispersion step of mixing the carbon nanoparticles undergoing the heat treatment step with an aqueous metal hydroxide solution and irradiating ultrasonic waves By providing a method of making the fluid.

본 발명의 바람직한 특징에 따르면, 상기 탄소질 재료는 활성탄, 활성탄섬유, 카본블랙 및 그래핀으로 이루어진 그룹으로부터 선택된 하나 이상으로 이루어지는 것으로 한다.According to a preferred feature of the invention, the carbonaceous material is made of one or more selected from the group consisting of activated carbon, activated carbon fiber, carbon black and graphene.

본 발명의 더 바람직한 특징에 따르면, 상기 밀링단계는 탄소질 재료를 텀블링볼밀과 모노 플레너밀로 48시간 동안 밀링하여 이루어지는 것으로 한다.According to a further preferred feature of the invention, the milling step is to be made by milling the carbonaceous material with a tumbling ball mill and a mono planner mill for 48 hours.

본 발명의 더욱 바람직한 특징에 따르면, 상기 산은 m-클로로퍼벤조익엑시드, 염산 및 황산으로 이루어진 그룹으로부터 선택된 하나로 이루어지는 것으로 한다.According to a more preferred feature of the invention, the acid is to be made of one selected from the group consisting of m-chloroperbenzoic acid, hydrochloric acid and sulfuric acid.

본 발명의 더욱 더 바람직한 특징에 따르면, 상기 열처리 단계는 상기 건조단계를 거친 탄소 나노입자를 400 내지 500℃의 온도로 가열하여 이루어지는 것으로 한다.According to a further preferred feature of the invention, the heat treatment step is to be made by heating the carbon nanoparticles undergoing the drying step to a temperature of 400 to 500 ℃.

본 발명의 더욱 더 바람직한 특징에 따르면, 상기 수분산단계는 상기 열처리단계를 거친 탄소 나노입자 4 내지 7 중량부를 금속 수산화물 93 내지 97 중량부와 혼합하고 초음파를 1시간 동안 조사하여 이루어지는 것으로 한다.According to a further preferred feature of the invention, the water dispersion step is to be made by mixing 4 to 7 parts by weight of the carbon nanoparticles subjected to the heat treatment step with 93 to 97 parts by weight of the metal hydroxide and irradiated with ultrasonic waves for 1 hour.

본 발명의 더욱 더 바람직한 특징에 따르면, 상기 금속수산화물 수용액은 수산화리튬, 수산화알루미늄, 탄산수소나트륨, 수산화철, 수산화납 및 수산화몰리브덴으로 이루어진 그룹으로부터 선택된 하나 이상으로 이루어진 금속 수산화물 0.05 내지 0.2mol을 200ml의 정제수와 혼합하여 이루어지는 것으로 한다.According to an even more preferred feature of the present invention, the aqueous metal hydroxide solution 200 ml of the metal hydroxide 0.05 to 0.2 mol of at least one selected from the group consisting of lithium hydroxide, aluminum hydroxide, sodium hydrogen carbonate, iron hydroxide, lead hydroxide and molybdenum hydroxide It shall be mixed with purified water.

본 발명의 더욱 더 바람직한 특징에 따르면, 상기 초음파는 진동수가 20kHz이며, 진폭이 48.8 마이크로미터인 것으로 한다.
According to a still further preferred feature of the invention, the ultrasonic wave is said to have a frequency of 20 kHz and an amplitude of 48.8 micrometers.

본 발명에 따른 금속처리된 탄소 나노입자가 함유된 나노유체의 제조방법은 냉각, 열교환 및 윤활성이 우수한 금속처리된 탄소 나노입자가 함유된 나노유체를 제공하는 탁월한 효과를 나타낸다.
The method for preparing nanofluids containing metal-treated carbon nanoparticles according to the present invention exhibits an excellent effect of providing nanofluids containing metal-treated carbon nanoparticles having excellent cooling, heat exchange and lubricity.

도 1은 본 발명에 따른 탄소 나노입자가 함유된 나노유체의 제조방법을 나타낸 순서도이다.1 is a flow chart showing a method for producing a nanofluid containing carbon nanoparticles according to the present invention.

이하에는, 본 발명의 바람직한 실시예와 각 성분의 물성을 상세하게 설명하되, 이는 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자가 발명을 용이하게 실시할 수 있을 정도로 상세하게 설명하기 위한 것이지, 이로 인해 본 발명의 기술적인 사상 및 범주가 한정되는 것을 의미하지는 않는다.
Hereinafter, preferred embodiments of the present invention and physical properties of the respective components will be described in detail with reference to the accompanying drawings. However, the present invention is not limited thereto, And this does not mean that the technical idea and scope of the present invention are limited.

본 발명에 따른 금속처리된 탄소 나노입자가 함유된 나노유체의 제조방법은 탄소질 재료를 밀링하는 밀링단계(S101), 상기 밀링단계(S101)를 거친 탄소 나노입자의 표면을 산으로 처리하는 산처리단계(S103), 상기 산처리단계(S103)를 거친 탄소 나노입자를 건조하는 건조단계(S105), 상기 건조단계(S105)를 거친 탄소 나노입자를 열처리하는 열처리단계(S107) 및 상기 열처리단계(S107)를 거친 탄소 나노입자를 금속 수산화물 수용액과 혼합하고 초음파를 조사하는 수분산단계(S109)로 이루어진다.
Method for producing a nanofluid containing the metal-treated carbon nanoparticles according to the present invention is a milling step (S101) of milling the carbonaceous material, the acid treatment of the surface of the carbon nanoparticles after the milling step (S101) with acid Treatment step (S103), drying step of drying the carbon nanoparticles subjected to the acid treatment step (S103) (S105), heat treatment step (S107) and the heat treatment step of heat treating the carbon nanoparticles subjected to the drying step (S105) (S107) is made of a water dispersion step (S109) of mixing the carbon nanoparticles with the aqueous metal hydroxide solution and irradiating ultrasonic waves.

전술한 밀링단계(S101)는 탄소질 재료를 밀링하는 단계로 활성탄, 활성탄섬유, 카본블랙 및 그래핀으로 이루어진 그룹으로부터 선택된 하나 이상으로 이루어지는 탄소질 재료를 텀블링볼밀과 모노 플레너밀로 48시간 동안 밀링하여 이루어지는데, 이러한 밀링단계(S101)를 거치면, 탄소질 재료의 입자가 나노 크기로 미분쇄된다.
The above-described milling step (S101) is a step of milling a carbonaceous material by milling a carbonaceous material consisting of at least one selected from the group consisting of activated carbon, activated carbon fiber, carbon black and graphene with a tumbling ball mill and a mono planner mill for 48 hours. In this milling step (S101), the particles of carbonaceous material are pulverized to nano size.

전술한 산처리단계(S103)는 전술한 밀링단계(S101)를 거쳐 제조된 탄소 나노 입자의 표면을 산으로 처리하는 단계로, 전술한 밀링단계(S101)를 거쳐 제조된 탄소 나노 입자를 m-클로로퍼벤조익엑시드, 염산 및 황산으로 이루어진 그룹으로부터 선택된 하나로 이루어진 산용액에 함침하여 탄소 나노 분말의 표면에 작용기(FUNCTIONAL GROUP)를 형성시키는데, 표면에 작용기가 형성된 탄소 나노 입자는 전술한 수분산단계(S109)에서 금속성 재료와 결합하여 표면이 금속으로 처리된 탄소 나노 입자를 제공할 수 있도록 하는 단계다.The above-described acid treatment step (S103) is a step of treating the surface of the carbon nanoparticles prepared through the aforementioned milling step (S101) with an acid, and m- the carbon nanoparticles prepared through the aforementioned milling step (S101). Impregnated in an acid solution selected from the group consisting of chloroperbenzoic acid, hydrochloric acid and sulfuric acid to form a functional group (FUNCTIONAL GROUP) on the surface of the carbon nanopowder, the carbon nanoparticles having a functional group on the surface is the above-described water dispersion step In operation S109, the surface is combined with the metallic material to provide the carbon nanoparticles having the surface treated with the metal.

전술한 산처리단계(S103)는 전술한 산 이외에 기타 산화제가 사용될 수도 있다.
In the above-described acid treatment step (S103), other oxidants may be used in addition to the above-described acid.

전술한 건조단계(S105)는 전술한 산처리단계(S103)를 거친 탄소 나노입자를 건조하는 단계로, 전술한 산처리단계(S103)를 통해 탄소 나노입자의 표면에 도포된 산 성분을 건조하는 단계다.The above-mentioned drying step (S105) is a step of drying the carbon nanoparticles subjected to the above-described acid treatment step (S103), and drying the acid component applied to the surface of the carbon nanoparticles through the above-described acid treatment step (S103). Step.

이때, 건조단계(S105)는 산처리단계(S103)를 거친 탄소 나노입자를 50 내지 90℃의 온도로 가열하여 이루어지는데, 전술한 가열온도는 특별히 한정되는 것이 아니며, 탄소 나노입자의 표면에 잔존하는 산성분을 제거할 수 있는 온도범위라면 어떠한 온도범위든 가능하다.
At this time, the drying step (S105) is made by heating the carbon nanoparticles subjected to the acid treatment step (S103) to a temperature of 50 to 90 ℃, the above-mentioned heating temperature is not particularly limited, remaining on the surface of the carbon nanoparticles Any temperature range is possible so long as it can remove the acid component.

전술한 열처리단계(S107)는 전술한 건조단계(S105)를 거친 탄소 나노입자를 열처리하는 단계로, 전술한 건조단계(S105)를 거쳐 제조된 탄소 나노입자를 400 내지 500℃의 온도로 가열하여 이루어지는데, 전술한 열처리단계(S107)를 거치면 탄소 나노입자에 함유된 휘발성 불순물 등이 제거되어, 순도가 높은 탄소 나노입자가 제공된다.
The above-described heat treatment step (S107) is a step of heat-treating the carbon nanoparticles passed through the drying step (S105) described above, by heating the carbon nanoparticles prepared through the drying step (S105) described above to a temperature of 400 to 500 ℃ Although the heat treatment step (S107) described above is made, volatile impurities and the like contained in the carbon nanoparticles are removed to provide high-purity carbon nanoparticles.

전술한 수분산단계(S109)는 전술한 열처리단계(S107)를 거친 탄소 나노입자를 금속 수산화물 수용액과 혼합하고 초음파를 조사하는 단계로, 탄소 나노입자 4 내지 7 중량부를 금속 수산화물 수용액 93 내지 97 중량부와 혼합하고 진동수가 20kHz이며, 진폭이 48.8 마이크로미터인 초음파를 1시간 동안 조사하여 이루어지는데, 전술한 초음파의 조사를 통해 수분산성이 향상된 금속처리된 탄소 나노입자가 함유된 나노유체가 제조된다.The above-described water dispersion step (S109) is a step of mixing the carbon nanoparticles undergoing the above-described heat treatment step (S107) with a metal hydroxide aqueous solution and irradiating ultrasonic waves, 4 to 7 parts by weight of the carbon nanoparticles 93 to 97 weight of the aqueous metal hydroxide solution It is made by mixing ultrasonic waves with a frequency of 20 kHz and an amplitude of 48.8 micrometers for one hour. .

이때, 전술한 금속 수산화물 수용액은 수산화리튬, 수산화알루미늄, 탄산수소나트륨, 수산화철, 수산화납 및 수산화몰리브덴으로 이루어진 그룹으로부터 선택된 하나 이상으로 이루어진 금속 수산화물 0.05 내지 2mol을 200ml의 정제수와 혼합하여 이루어진다.
At this time, the above-described metal hydroxide aqueous solution is made by mixing 0.05 to 2 mol of metal hydroxide consisting of at least one selected from the group consisting of lithium hydroxide, aluminum hydroxide, sodium hydrogen carbonate, iron hydroxide, lead hydroxide and molybdenum hydroxide with 200 ml of purified water.

이하에서는, 본 발명에 따른 금속처리된 탄소 나노입자가 함유된 나노유체의 제조방법 및 물성을 실시예를 들어 설명한다.
Hereinafter, the production method and physical properties of the nanofluid containing the metal-treated carbon nanoparticles according to the present invention will be described with reference to Examples.

<실시예 1>&Lt; Example 1 >

활성탄을 텀블링볼밀과 모노 플레너밀로 48시간 동안 밀링하여 나노사이즈로 분쇄하고, M-클로로퍼벤조익엑시드에 분쇄된 탄소 나노입자를 침지하여 표면처리하고, 침지된 탄소 나노입자를 분리하여 60℃의 온도로 건조하고, 건조된 탄소 나노입자를 500℃의 온도로 가열하여 열처리하고, 열처리 된 탄소 나노입자를 5 중량부를 탄산수소나트륨 0.05mol을 정제수 200ml에 혼합한 수용액 95 중량부와 혼합하고, 진동수가 20kHz이며, 진폭이 48.8 마이크로미터인 초음파를 1시간 동안 조사하여 금속처리된 탄소 나노입자가 함유된 나노유체를 제조하였다.
Activated carbon was milled for 48 hours using a tumbling ball mill and a mono planner mill to pulverize the nano-sized, surface-treated by immersing the pulverized carbon nanoparticles in M-chloroperbenzoic acid, and the immersed carbon nanoparticles were separated, The dried carbon nanoparticles were heated to a temperature of 500 ° C. and heat-treated, and 5 parts by weight of the heat-treated carbon nanoparticles were mixed with 95 parts by weight of an aqueous solution in which 0.05 mol of sodium hydrogen carbonate was mixed with 200 ml of purified water. Was 20 kHz, and an ultrasonic wave having an amplitude of 48.8 micrometers was irradiated for 1 hour to prepare a nanofluid containing carbonized carbon nanoparticles.

<실시예 2><Example 2>

실시예 1과 동일하게 진행하되, 탄산수소나트륨 대신 수산화알루미늄을 사용하여 금속처리된 탄소 나노입자가 함유된 나노유체를 제조하였다.
Proceed in the same manner as in Example 1, using a nano hydroxide instead of sodium hydrogen carbonate to prepare a nano-fluid containing the metal-treated carbon nanoparticles.

<실시예 3><Example 3>

실시예 1과 동일하게 진행하되, 탄산수소나트륨 대신 수산화리튬을 사용하여 금속처리된 탄소 나노입자가 함유된 나노유체를 제조하였다.
Proceed in the same manner as in Example 1, using lithium hydroxide instead of sodium hydrogen carbonate to prepare a nanofluid containing metal-treated carbon nanoparticles.

<실시예 4><Example 4>

실시예 1과 동일하게 진행하되, 활성탄 대신 활성탄섬유를 사용하여 금속처리된 탄소 나노입자가 함유된 나노유체를 제조하였다.
Proceed in the same manner as in Example 1, using activated carbon fibers instead of activated carbon to prepare a nanofluid containing metal treated carbon nanoparticles.

<실시예 5><Example 5>

실시예 2과 동일하게 진행하되, 활성탄 대신 활성탄섬유를 사용하여 금속처리된 탄소 나노입자가 함유된 나노유체를 제조하였다.
Proceed in the same manner as in Example 2, using activated carbon fibers instead of activated carbon to prepare a nanofluid containing metal-treated carbon nanoparticles.

<실시예 6><Example 6>

실시예 3과 동일하게 진행하되, 활성탄 대신 활성탄섬유를 사용하여 금속처리된 탄소 나노입자가 함유된 나노유체를 제조하였다.
Proceed in the same manner as in Example 3, using activated carbon fibers instead of activated carbon to prepare a nanofluid containing metal-treated carbon nanoparticles.

<실시예 7>&Lt; Example 7 >

실시예 1과 동일하게 진행하되, 활성탄 대신 카본블랙를 사용하여 금속처리된 탄소 나노입자가 함유된 나노유체를 제조하였다.
Proceed in the same manner as in Example 1, using carbon black instead of activated carbon to prepare a nanofluid containing metal-treated carbon nanoparticles.

<실시예 8>&Lt; Example 8 >

실시예 2와 동일하게 진행하되, 활성탄 대신 카본블랙를 사용하여 금속처리된 탄소 나노입자가 함유된 나노유체를 제조하였다.
Proceed in the same manner as in Example 2, using carbon black instead of activated carbon to prepare a nanofluid containing metal-treated carbon nanoparticles.

<실시예 9>&Lt; Example 9 >

실시예 3과 동일하게 진행하되, 활성탄 대신 카본블랙를 사용하여 금속처리된 탄소 나노입자가 함유된 나노유체를 제조하였다.
Proceed in the same manner as in Example 3, using carbon black instead of activated carbon to prepare a nanofluid containing metal treated carbon nanoparticles.

<실시예 10>&Lt; Example 10 >

실시예 1과 동일하게 진행하되, 활성탄 대신 그래핀을 사용하고, 탄산수소나트륨 대신 수산화납을 사용하여 금속처리된 탄소 나노입자가 함유된 나노유체를 제조하였다.
Proceed in the same manner as in Example 1, using graphene instead of activated carbon, using lead hydroxide instead of sodium hydrogen carbonate to prepare a nanofluid containing metal-treated carbon nanoparticles.

<실시예 11><Example 11>

실시예 1과 동일하게 진행하되, 활성탄 대신 그래핀을 사용하고, 탄산수소나트륨 대신 수산화철을 사용하여 금속처리된 탄소 나노입자가 함유된 나노유체를 제조하였다.
Proceed in the same manner as in Example 1, but using graphene instead of activated carbon, using iron hydroxide instead of sodium hydrogen carbonate to prepare a nanofluid containing metal-treated carbon nanoparticles.

<실시예 12>&Lt; Example 12 >

실시예 1과 동일하게 진행하되, 활성탄 대신 그래핀을 사용하고, 탄산수소나트륨 대신 수산화몰리브덴을 사용하여 금속처리된 탄소 나노입자가 함유된 나노유체를 제조하였다.
Proceed in the same manner as in Example 1, but using graphene instead of activated carbon, using molybdenum hydroxide instead of sodium hydrogen carbonate to prepare a nanofluid containing carbon-treated carbon nanoparticles.

<비교예 1>&Lt; Comparative Example 1 &

활성탄을 텀블링볼밀과 모노 플레너밀로 48시간 동안 밀링하여 나노사이즈로 분쇄하고, 나노사이즈로 분쇄된 탄소 나노입자 5 중량부를 정제수 95 중량부와 혼합하여 탄소 나노입자가 함유된 나노유체를 제조하였다.
The activated carbon was milled for 48 hours using a tumbling ball mill and a mono planner mill to be pulverized to nanosize, and 5 parts by weight of the nanoscale pulverized carbon nanoparticles were mixed with 95 parts by weight of purified water to prepare a nanofluid containing carbon nanoparticles.

<비교예 2>Comparative Example 2

활성탄을 텀블링볼밀과 모노 플레너밀로 48시간 동안 밀링하여 나노사이즈로 분쇄하고, M-클로로퍼벤조익엑시드에 침지한 후에 건조한 탄소 나노입자 5 중량부를 정제수 95 중량부와 혼합하여 탄소 나노입자가 함유된 나노유체를 제조하였다.
Activated carbon was milled for 48 hours with a tumbling ball mill and a mono planner mill, pulverized to nano size, immersed in M-chloroperbenzoic acid, and 5 parts by weight of dry carbon nanoparticles were mixed with 95 parts by weight of purified water to contain carbon nanoparticles. Nanofluids were prepared.

<비교예 3>&Lt; Comparative Example 3 &

비교예 1과 동일하게 진행하되, 활성탄 대신 활성탄섬유를 사용하여 탄소 나노입자가 함유된 나노유체를 제조하였다.
Proceed in the same manner as in Comparative Example 1, using carbon nanoparticles instead of activated carbon to prepare a nanofluid containing the carbon nanoparticles.

<비교예 4>&Lt; Comparative Example 4 &

비교예 2와 동일하게 진행하되, 활성탄 대신 활성탄섬유를 사용하여 탄소 나노입자가 함유된 나노유체를 제조하였다.
Proceed in the same manner as in Comparative Example 2, using carbon nanoparticles instead of activated carbon to prepare a nanofluid containing the carbon nanoparticles.

<비교예 5>&Lt; Comparative Example 5 &

비교예 1과 동일하게 진행하되, 활성탄 대신 카본블랙를 사용하여 탄소 나노입자가 함유된 나노유체를 제조하였다.
Proceed in the same manner as in Comparative Example 1, using carbon black instead of activated carbon to prepare a nanofluid containing carbon nanoparticles.

<비교예 6>&Lt; Comparative Example 6 >

비교예 2과 동일하게 진행하되, 활성탄 대신 카본블랙를 사용하여 탄소 나노입자가 함유된 나노유체를 제조하였다.
Proceed in the same manner as in Comparative Example 2, using carbon black instead of activated carbon to prepare a nanofluid containing the carbon nanoparticles.

전술한 실시예 1 내지 12 및 비교예 1 내지 6을 통해 제조된 금속처리된 탄소 나노입자가 함유된 나노유체 및 탄소 나노입자가 함유된 나노유체의 열확산성 및 전기전도성을 측정하여 아래 표 1에 나타내었다.The thermal diffusion and electrical conductivity of the nanofluids containing the metal-treated carbon nanoparticles and the nanofluids containing the carbon nanoparticles prepared through the above Examples 1 to 12 and Comparative Examples 1 to 6 were measured. Indicated.

(단, 열확산계수는 α = k/(ρ×c) 의 열확산계수 측정법을 이용한 열확산계수 측정장치로 측정하였고, 전기전도성은 Trans Instruments사의 WalkLAB Digital Conductivity Pro meter로 측정하였다.)
(However, the thermal diffusion coefficient was measured by a thermal diffusion coefficient measuring device using a thermal diffusion coefficient measuring method of α = k / (ρ × c), and the electrical conductivity was measured by the WalkLAB Digital Conductivity Pro meter of Trans Instruments.

<표 1>TABLE 1

Figure pat00001
Figure pat00001

위에 표 1에 나타낸 것처럼 본 발명의 실시예 1 내지 12를 통해 제조된 금속처리된 탄소 나노입자가 함유된 나노유체는 비교예 1 내지 6을 통해 제조된 탄소 나노입자가 함유된 나노유체에 비해 열확산성과 전기전도성이 월등하게 향상되는 것을 알 수 있다.
As shown in Table 1 above, the nanofluid containing the metal-treated carbon nanoparticles prepared through Examples 1 to 12 of the present invention is thermally diffused compared to the nanofluid containing the carbon nanoparticles prepared through Comparative Examples 1 to 6. It can be seen that the performance and electrical conductivity are greatly improved.

S101 ; 밀링단계
S103 ; 산처리단계
S105 ; 건조단계
S107 ; 열처리단계
S109 ; 수분산단계S101; Milling stage
S103; Acid treatment step
S105; Drying step
S107; Heat treatment step
S109; Dispersion stage

Claims (8)

탄소질 재료를 밀링하는 밀링단계;
상기 밀링단계를 거친 탄소 나노입자의 표면을 산으로 처리하는 산처리단계;
상기 산처리단계를 거친 탄소 나노입자를 건조하는 건조단계;
상기 건조단계를 거친 탄소 나노입자를 열처리하는 열처리단계; 및
상기 열처리단계를 거친 탄소 나노입자를 금속 수산화물 수용액과 혼합하고 초음파를 조사하는 수분산단계;로 이루어지는 것을 특징으로 하는 금속처리된 탄소 나노입자가 함유된 나노유체의 제조방법.
Milling the carbonaceous material;
An acid treatment step of treating the surface of the carbon nanoparticles subjected to the milling step with an acid;
A drying step of drying the carbon nanoparticles subjected to the acid treatment step;
A heat treatment step of heat-treating the carbon nanoparticles subjected to the drying step; And
And a water dispersion step of mixing the carbon nanoparticles subjected to the heat treatment step with an aqueous solution of metal hydroxide and irradiating ultrasonic waves.
청구항 1에 있어서,
상기 탄소질 재료는 활성탄, 활성탄섬유, 카본블랙 및 그래핀으로 이루어진 그룹으로부터 선택된 하나 이상으로 이루어지는 것을 특징으로 하는 금속처리된 탄소 나노입자가 함유된 나노유체의 제조방법.
The method according to claim 1,
The carbonaceous material is a method for producing a nanofluid containing metal-treated carbon nanoparticles, characterized in that at least one selected from the group consisting of activated carbon, activated carbon fiber, carbon black and graphene.
청구항 1에 있어서,
상기 밀링단계는 탄소질 재료를 텀블링볼밀과 모노 플레너밀로 48시간 동안 밀링하여 이루어지는 것을 특징으로 하는 금속처리된 탄소 나노입자가 함유된 조성물의 제조방법.
The method according to claim 1,
The milling step is a method for producing a composition containing metal-treated carbon nanoparticles, characterized in that the carbonaceous material is milled for 48 hours with a tumbling ball mill and a mono planner mill.
청구항 1에 있어서,
상기 산은 m-클로로퍼벤조익엑시드, 염산 및 황산으로 이루어진 그룹으로부터 선택된 하나로 이루어지는 것을 특징으로 하는 금속처리된 탄소 나노입자가 함유된 나노유체의 제조방법.
The method according to claim 1,
Wherein said acid is one selected from the group consisting of m-chloroperbenzoic acid, hydrochloric acid and sulfuric acid.
청구항 1에 있어서,
상기 열처리 단계는 상기 건조단계를 거친 탄소 나노입자를 400 내지 500℃의 온도로 가열하여 이루어지는 것을 특징으로 하는 금속처리된 탄소 나노입자가 함유된 나노유체의 제조방법.
The method according to claim 1,
The heat treatment step is a method of producing a nanofluid containing metal-treated carbon nanoparticles, characterized in that the drying is performed by heating the carbon nanoparticles to a temperature of 400 to 500 ℃.
청구항 1에 있어서,
상기 수분산단계는 상기 열처리단계를 거친 탄소 나노입자 4 내지 7 중량부를 금속 수산화물 수용액 93 내지 97 중량부와 혼합하고 초음파를 1시간 동안 조사하여 이루어지는 것을 특징으로 하는 금속처리된 탄소 나노입자가 함유된 나노유체의 제조방법.The method according to claim 1,
The water dispersion step comprises 4 to 7 parts by weight of the carbon nanoparticles subjected to the heat treatment step and 93 to 97 parts by weight of a metal hydroxide aqueous solution, and the metal-treated carbon nanoparticles, characterized in that the irradiation for 1 hour Method of preparing nanofluids. 청구항 1 또는 청구항 6에 있어서,
상기 금속수산화물 수용액은 수산화리튬, 수산화알루미늄, 탄산수소나트륨, 수산화철, 수산화납 및 수산화몰리브덴으로 이루어진 그룹으로부터 선택된 하나 이상으로 이루어진 금속 수산화물 0.05 내지 2mol을 200ml의 정제수와 혼합하여 이루어지는 것을 특징으로 하는 금속처리된 탄소 나노입자가 함유된 나노유체의 제조방법.
The method according to claim 1 or 6,
The metal hydroxide aqueous solution is a metal treatment, characterized in that the mixture is mixed with 0.05 to 2 mol of metal hydroxide consisting of at least one selected from the group consisting of lithium hydroxide, aluminum hydroxide, sodium hydrogen carbonate, iron hydroxide, lead hydroxide and molybdenum hydroxide with 200 ml of purified water. Of a nanofluid containing the carbon nanoparticles.
청구항 1 또는 청구항 6에 있어서,
상기 초음파는 진동수가 20kHz이며, 진폭이 48.8 마이크로미터인 것을 특징으로 하는 금속처리된 탄소 나노입자가 함유된 나노유체의 제조방법. The method according to claim 1 or 6,
The ultrasonic wave has a frequency of 20 kHz, the amplitude of 48.8 micrometers, characterized in that the manufacturing method of the nanofluid containing carbon-treated carbon nanoparticles.
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