KR101439323B1 - planetary ball mill method and solvothermal method - Google Patents

planetary ball mill method and solvothermal method Download PDF

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Publication number
KR101439323B1
KR101439323B1 KR1020130123108A KR20130123108A KR101439323B1 KR 101439323 B1 KR101439323 B1 KR 101439323B1 KR 1020130123108 A KR1020130123108 A KR 1020130123108A KR 20130123108 A KR20130123108 A KR 20130123108A KR 101439323 B1 KR101439323 B1 KR 101439323B1
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South Korea
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milling
rotating plate
base
vessel
ball mill
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KR1020130123108A
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Korean (ko)
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양현경
양승철
최지연
김동국
정남조
김찬수
김한기
좌은진
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한국에너지기술연구원
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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
    • B82B3/0095—Manufacture or treatments or nanostructures not provided for in groups B82B3/0009 - B82B3/009
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/04—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with unperforated container
    • B02C17/08—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with unperforated container with containers performing a planetary movement
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Abstract

The present invention relates to a method of manufacturing a nano crystal by using a ball milling and a solvothermal method at the same time and installing a heater in a planetary ball mill apparatus to increase a pressure inside a vessel, and the planetary ball mill apparatus including: a base; a heating bath installed onto the base and having a space therein, and provided therein with a heating mean; a rotating plate installed on the base inside the heating bath; and a milling vessel installed on the rotating plate to rotate according to a rotation of the rotating plate, having a space therein and being able to rotate with respect to the rotating plate, in which a raw sample, a milling ball, and a solvent are loaded in the milling vessel. Accordingly, the present invention may control pressure by controlling temperature and may manufacture a nano crystal without a post heat treatment.

Description

유성형볼밀방법과 열용매방법을 혼합한 나노결정 제조장치{planetary ball mill method and solvothermal method}[0001] The present invention relates to a planetary ball mill method and a solvothermal method,

본 발명은 유성형볼밀방법과 열용매방법을 혼합한 나노결정 제조장치에 관한 것으로, 더욱 상세하게는 유성형볼밀링(planetary ball mill) 장치에 히터를 장착하여 용기내부의 압력을 증가시켜 볼밀링과 동시에 열용매방법을 이용한 나노결정의 제조방법에 관한 것이다. 따라서, 본 발명은 온도의 제어를 통하여 압력의 제어가 가능하며, 후 열처리 과정 없이 나노결정을 제조할 수 있다.
The present invention relates to an apparatus for producing nanocrystals in which a planetary ball mill method and a heat solvent method are mixed, and more particularly, to a planetary ball mill apparatus in which a heater is installed to increase the pressure inside the vessel, And a method for producing nanocrystals using a thermal solvent method. Therefore, the present invention can control the pressure through temperature control, and can produce nanocrystals without post-heat treatment.

나노결정 제조에 대하여 일반적인 고상반응에 의해 나노결정을 얻어내기는 쉽지 않다. It is not easy to obtain nanocrystals by general solid reaction for nanocrystal production.

그리고, 열수용법, 열용매법등의 화학적인 합성방법을 이용한 나노입자의 합성법은 100 ㎚ 이하의 작고 균일한 입자의 합성은 가능하지만, 합성의 공정이 복잡하며, 후열처리 과정이 필요하고 한번의 공정으로 생산할 수 있는 시료의 양이 적은 문제점이 있다.
The synthesis method of nanoparticles using chemical synthesis methods such as hydrothermal method and thermal solvent method can synthesize small and uniform particles of 100 nm or less, but the synthesis process is complicated, post heat treatment process is required, There is a problem in that the amount of sample that can be produced is small.

한국특허공개 제10-2012-0056075호Korean Patent Laid-Open No. 10-2012-0056075

상기의 목적을 달성하기 위한 본 발명은, 나노크기의 미세하고 입경분포가 좁고, 고순도의 나노결정의 제조를 간단한 공정과 후 열처리를 통하지 않고 열수용법, 열용매법과 대비하여 대량생산이 가능하게 하는 유성형볼밀방법과 열용매방법을 혼합한 나노결정 제조장치를 제공하는 것을 목적으로 한다.
In order to accomplish the above object, the present invention provides a method of manufacturing a nanocrystal having a narrow nano-scale and narrow particle size distribution and having high purity and capable of mass production in comparison with a hot solvent method and a heat solvent method, It is an object of the present invention to provide a nanocrystal manufacturing apparatus in which a planetary ball mill method and a heat solvent method are mixed.

상기의 목적을 달성하기 위한 본 발명은, 베이스; 상기 베이스의 상부에서 설치되고 내부에 공간을 가지며, 가열수단이 내장되는 가열조; 상기 베이스 상부에 상기 가열조 내부로 설치되는 회전판; 상기 회전판 상에 설치되어 상기 회전판의 회전에 따라 회전하고, 내부에 공간을 가지며, 상기 회전판에 대하여 자전이 가능한 밀링용기를 포함하며, 상기 밀링용기 내부에는 원료시료, 밀링볼, 및 용매가 장입되는 나노결정 제조장치이다.According to an aspect of the present invention, A heating tank installed at an upper portion of the base and having a space therein and having a heating means built therein; A rotating plate installed in the heating chamber above the base; And a milling container installed on the rotating plate, rotating according to rotation of the rotating plate, having a space therein, and capable of rotating with respect to the rotating plate, wherein a raw material sample, a milling ball, and a solvent are charged into the milling container Is a nanocrystal manufacturing apparatus.

상기 용매는 에탄올, 메탄올, 이소프로파놀, 아세톤, 및 증류수 중에서 선택되는 어느 하나인 것을 특징으로 한다.The solvent is any one selected from the group consisting of ethanol, methanol, isopropanol, acetone, and distilled water.

또, 상기 밀링용기는 테플론(Teflon), 알루미나(Al2O3) 세라믹, 지르코니아(ZrO) 세라믹, 및 스테인레스 스틸(SUS) 중 어느 하나로 이루어지는 것을 특징으로 한다.The milling vessel is characterized in that the milling vessel is made of any one of Teflon, Al 2 O 3 ceramic, ZrO 2 ceramic, and stainless steel (SUS).

또, 상기 밀링볼은 지르코니아(ZrO2), 아루미나(Al2O3), 실리카(SiO2), 타이타니아(TiO2) 세라믹 중 어느 하나로 이루어지는 것을 특징으로 한다.
The milling balls may be made of zirconia (ZrO 2 ), alumina (Al 2 O 3 ), silica (SiO 2 ), titania (TiO 2 ) Ceramic, and the like.

본 발명을 통하여, 나노결정 제조에 대하여 합성공정이 간단하며 열수용법, 열용매법과 대비하여 대량생산이 가능하여 경쟁력 있는 제조방법을 제공할 수 있다.
Through the present invention, it is possible to provide a competitive manufacturing method because the synthesis process is simple for nanocrystal production, and mass production is possible in comparison with the hot water application method and the heat solvent method.

도 1은 본 발명의 실시예에 따른 나노결정 제조장치의 사시도이다.1 is a perspective view of an apparatus for producing nanocrystals according to an embodiment of the present invention.

이하, 본 발명의 바람직한 실시예를 첨부한 도면을 참조하여 설명하기로 한다. 하기의 각 도면의 구성 요소들에 참조 부호를 부가함에 있어서, 동일한 구성 요소들에 한해서는 비록 다른 도면상에 표시되더라도 가능한 한 동일한 부호를 가지도록 하며, 본 발명의 요지를 불필요하게 흐릴 수 있다고 판단되는 공지 기능 및 구성에 대한 상세한 설명은 생략한다.Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings. In the drawings, the same reference numerals are used to designate the same or similar components, and the same reference numerals will be used to designate the same or similar components. Detailed descriptions of known functions and configurations are omitted.

도 1에서 도면부호 100은 본 발명의 실시예에 따른 나노결정 제조장치를 지시한다.1, reference numeral 100 designates an apparatus for producing nanocrystals according to an embodiment of the present invention.

상기 나노결정 제조장치(100) 크게, 베이스(102)와, 상기 베이스(102) 상에 설치되는 가열조(108)와, 상기 가열조(108) 내부에 배치되는 밀리용기(120)을 포함한다. The apparatus for manufacturing nanocrystals 100 comprises a base 102, a heating tank 108 provided on the base 102, and a milli-vessel 120 disposed inside the heating tank 108 .

상기 베이스(102)에는 조작부(104)와 표시부(106)가 설치되어, 작업자가 원하는 온도와 회전속도, 작동시간을 설정하고, 이를 시각적으로 확인할 수 있다.The base 102 is provided with an operation unit 104 and a display unit 106, and can set a desired temperature, a rotation speed, and an operation time by the operator, and visually check the temperature, the rotation speed, and the operation time.

상기 가열조(108)는 상기 베이스(102) 상에 고정되며, 내부에 공간(110)을 가진다. 상기 가열조(108)는 상기 공간(100)을 개방하도록 가열조커버(114)가 설치된다. 또는, 상기 가열조(108)가 하부가 개방이고 상기 베이스(102)에 착탈가능하도록 설치되는 것도 가능하다.The heating tank 108 is fixed on the base 102 and has a space 110 therein. The heating tank 108 is provided with a heating tank cover 114 to open the space 100. Alternatively, the heating tank 108 may be installed to be detachable from the base 102 with its bottom opened.

상기 가열조(108)의 벽체에는 가열수단(108)이 설치되어 상기 가열조(108) 내부의 온도를 50~250℃로 가열한다. 상기 가열수단(108)으로는 SiC 히터, 칸탈 히터(Kanthal heater), 세라믹 히터(ceramic heater) 할로겐 히터(Halogen heater), 니크로털 발열체(Nikrothal heater) 등의 공지의 히터를 사용할 수 있다. 그리고, 온도를 측정하기 위해 상기 가열조(108) 내에 써모미터와 같은 온도센서(124)가 추가설치될 수 있다.The wall of the heating tank 108 is provided with a heating means 108 to heat the inside of the heating tank 108 to 50 to 250 ° C. As the heating means 108, known heaters such as a SiC heater, a Kanthal heater, a ceramic heater, a halogen heater, and a Nikrothal heater may be used. Then, a temperature sensor 124 such as a thermometer may be additionally provided in the heating tank 108 for measuring the temperature.

회전판(116)이 상기 베이스(102) 상부에 상기 가열조(108) 내부로 설치된다. 상기 회전판(116)은 회전이 가능하며, 10~70rpm으로 회전할 수 있다. 상기 회전판(116)에는 상기 밀링용기(120) 복수개가 방사상으로 설치된다. 상기 밀링용기(120)는 착탈이 용이하도록 상기 회전판(116)에 배치되는 소켓(118)에 장착될 수 있다.A rotating plate 116 is installed inside the heating tank 108 above the base 102. The rotating plate 116 is rotatable and can rotate at 10 to 70 rpm. A plurality of the milling containers 120 are radially installed on the rotary plate 116. The milling container 120 may be mounted on a socket 118 disposed on the rotating plate 116 to facilitate detachment.

상기 밀링용기(120)는 상기 회전판(116)의 회전과 별개로 50~350rpm으로 자전이 가능하다. 상기 밀링용기(120)의 공전 및 자전운동은, 상기 회전판(116)과 상기 밀링용기(120)에 연결되는 유성기어에 의해 이루어진다. 따라서, 상기 회전판(116)과 상기 밀링용기(120)는 일정한 기어비를 통해 일정한 회전속도비를 가질 수 있다. 물론, 별도의 기계구조를 가지는 것도 가능하나, 장비가 복잡해지는 단점이 있다.The milling vessel 120 can rotate at 50 to 350 rpm independently of the rotation of the rotary plate 116. The revolving or rotating motion of the milling container 120 is performed by a planetary gear connected to the rotary plate 116 and the milling container 120. Accordingly, the rotating plate 116 and the milling container 120 may have a constant rotational speed ratio through a constant gear ratio. Of course, it is also possible to have a separate mechanical structure, but there is a disadvantage that the equipment becomes complicated.

상기 밀링용기(120)도 내부를 개방할 수 있도록 밀링용기커버(122)를 가진다. 그리고, 높은 회전수에 따른 밀링볼의 충격에 견딜 수 있도록 상기 밀링용기(120)는 테플론(Teflon), 알루미나(Al2O3) 세라믹, 지르코니아(ZrO) 세라믹, 및 스테인레스 스틸(SUS) 중 어느 하나로 이루어질 수 있다.The milling vessel 120 also has a milling vessel cover 122 for opening the inside thereof. In order to withstand the impact of the milling balls according to the high rotation speed, the milling container 120 is formed of a material selected from the group consisting of Teflon, alumina (Al 2 O 3 ) ceramic, zirconia (ZrO) ceramic, and stainless steel It can be done in one.

상기 밀링용기(120) 내부에는 원료시료, 밀링볼, 및 용매가 장입된다. 상기 원료시료로는 탄소나노소재로는 탄소나노튜브, 탄소나노섬유, 플러렌, 탄소나노혼, 나노카본블랙, 탄소섬유 중에서 선택되는 어느 하나 이상일 수 있다.A raw material sample, a milling ball, and a solvent are charged into the milling vessel 120. The raw material sample may be at least one selected from carbon nanotubes, carbon nanofibers, fullerenes, carbon nanofines, nano carbon black, and carbon fibers.

그리고, 상기 밀링볼은 지르코니아(ZrO2), 아루미나(Al2O3), 실리카(SiO2), 타이타니아(TiO2) 세라믹 중 어느 하나로 이루어질 수 있다. 또, 상기 용매는 에탄올(ethanol), 메탄올(methanol), 이소프로파놀(isopropanol), 아세톤(acetone), 및 증류수(distilled water) 중에서 선택되어 사용될 수 있다.The milling balls may be made of zirconia (ZrO 2 ), alumina (Al 2 O 3 ), silica (SiO 2 ), titania (TiO 2 ) Ceramics or the like. The solvent may be selected from ethanol, methanol, isopropanol, acetone, and distilled water.

상기 밀링용기(120)가 자전 및 공전을 개시하면, 이때, 상기 밀링용기(120) 내부에서는 밀링볼과 원료시료가 자전에 의한 원심력과 공정에 의한 원심력으로 인해 밀링용기(120)에 부딪히고, 서로 충돌 및 타격하면서 나노결정을 제조할 수 있다.
When the milling vessel 120 starts to rotate and revolves, the milling balls and the raw material sample collide with the milling vessel 120 due to the centrifugal force due to the rotation and the centrifugal force due to the process, The nanocrystals can be produced while colliding with and hitting each other.

상기와 같이, 본 발명의 바람직한 실시예를 참조하여 설명하였지만 해당 기술 분야의 숙련된 당업자라면 하기의 특허청구범위에 기재된 본 발명의 사상 및 영역으로부터 벗어나지 않는 범위 내에서 본 발명을 다양하게 수정 및 변경시킬 수 있음을 이해할 수 있을 것이다.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it will be understood by those of ordinary skill 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. It can be understood that

100: 나노결정 제조장치 102: 베이스
104: 조작부 106: 표시부
108: 가열조 110: 공간
112: 가열수단 114: 가열조커버
116: 회전판 118: 소켓
120: 밀링용기 122: 밀링용기커버
124: 온도센서100: nanocrystal manufacturing apparatus 102: base
104: Operation section 106: Display section
108: Heating tank 110: Space
112: heating means 114: heating cover
116: spindle 118: socket
120: Milling container 122: Milling container cover
124: Temperature sensor

Claims (4)

베이스;
상기 베이스의 상부에서 설치되고 내부에 공간을 가지며, 가열수단이 내장되는 가열조;
상기 베이스 상부에 상기 가열조 내부로 설치되는 회전판;
상기 회전판 상에 설치되어 상기 회전판의 회전에 따라 회전하고, 내부에 공간을 가지며, 상기 회전판에 대하여 자전이 가능한 밀링용기를 포함하며,
상기 용기 내부에는 원료시료, 밀링볼, 및 용매가 장입되는 나노결정 제조장치.
Base;
A heating tank installed at an upper portion of the base and having a space therein and having a heating means built therein;
A rotating plate installed in the heating chamber above the base;
And a milling container mounted on the rotating plate, rotating in accordance with rotation of the rotating plate, having a space therein, and capable of rotating with respect to the rotating plate,
Wherein a raw material sample, a milling ball, and a solvent are charged into the vessel.
제1항에 있어서, 상기 용매는 에탄올, 메탄올, 이소프로파놀, 아세톤, 및 증류수 중에서 선택되는 어느 하나인 것을 특징으로 하는 나노결정 제조장치.
The apparatus for producing nanocrystals according to claim 1, wherein the solvent is any one selected from the group consisting of ethanol, methanol, isopropanol, acetone, and distilled water.
제1항에 있어서, 상기 밀링용기는 테플론(Teflon), 알루미나(Al2O3) 세라믹, 지르코니아(ZrO) 세라믹, 및 스테인레스 스틸(SUS) 중 어느 하나로 이루어지는 것을 특징으로 하는 나노결정 제조장치.
The apparatus for manufacturing nanocrystals according to claim 1, wherein the milling vessel is made of any one of Teflon, Al 2 O 3 ceramic, ZrO 2 ceramic, and stainless steel (SUS).
제1항에 있어서, 상기 밀링볼은 지르코니아(ZrO2), 아루미나(Al2O3), 실리카(SiO2), 타이타니아(TiO2) 세라믹 중 어느 하나로 이루어지는 것을 특징으로 하는 나노결정 제조장치.The method of claim 1, wherein the milling balls are selected from the group consisting of zirconia (ZrO 2 ), alumina (Al 2 O 3 ), silica (SiO 2 ), titania (TiO 2 ) Ceramic, and the like.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6126097A (en) 1999-08-21 2000-10-03 Nanotek Instruments, Inc. High-energy planetary ball milling apparatus and method for the preparation of nanometer-sized powders
KR20100051927A (en) * 2008-11-10 2010-05-19 주식회사 제이오 Combined pulverization and dispersion system enabling cnt dispersion

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6126097A (en) 1999-08-21 2000-10-03 Nanotek Instruments, Inc. High-energy planetary ball milling apparatus and method for the preparation of nanometer-sized powders
KR20100051927A (en) * 2008-11-10 2010-05-19 주식회사 제이오 Combined pulverization and dispersion system enabling cnt dispersion

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Characterization of mechanochemically synthesized ZnSe in a laboratory and an industrial mill, Solid State Ionics, 2011, Vol.192(1), pp.632-637. *
Materials, 2012, Vol. 5, pp.1404-1412. *

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