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1 J. Kor. Powd. Met. Inst., Vol. 20, No. 2, 2013 DOI: /KPMI SMPS l ( )ƒ ù d e w y Á w t w» t l The Effect of Water Droplets on the Nano Particle Size Distribution using the SMPS System Seon-Ae HwangboGand Min-Cheol Chu Center for New Functional Materials Metrology, KRISS, Daejeon , Korea (Received March 12, 2013; Accepted April 15, 2013) Abstract In this paper we have studied the effect of water droplet size on nano-particle size distribution using SMPS(Scanning Mobility Particle Sizer)system. It can be seen that the unknown peak at >100 nm was caused by water droplets which did not dry completely when DI water was used as a solvent in the SMPS system. Therefore, it is important to dry water droplets generated from atomizer in the SMPS system when measuring the particle size distribution using less than 100 nm nano-particles in diameter. From this study, It can be concluded that the napion was a useful material as dryer ones and using EAG(Electro Aerosol Generator) as a particle generator was the most effective in reducing the effect of water droplets. Keywords: SMPS, Nano-particles, Size distribution measurement, Water droplets, Atomizer 1.» ù» w š, w y w ù t 60%ƒ e,, y t,, k» y t ù w x ù ù œ, ù p ( ) yƒ y w š. ù 2007 z ù» w z t mw ù» 3 w» y y t wš. ù» w w» y, ù v y w ù y wš [1]. ù 100 nm w (Ultrafine Particle) w. w ù ù w j»ƒ p w w k. ù ù š w p ¾ w w, ù y e w w w. w ù y e w w ƒ š [2-8]. ù» wì ù w w ƒw, z(european Commission)ƒ 1~100 nm j» ƒ ƒ 50% sww ù š w. ù yw w» w j» j» sd w. *Corresponding Author : Min-Cheol Chu, TEL: , FAX: , chumin@kriss.re.kr 129

2 130 y Á w ù d e SMPS(Scanning Mobility Particle Sizer) DLS(Dynamic Laser light Scattering)ƒ. DLS k g ƒ k q y y mw j» w e. d 5~6 š v j» ƒ j yw» [9]. 1~100 nm j» ƒ d d w SMPS wš. SMPS» p w d w. l j»(atomizer), y»(neutralizer),»(dma, Differential Mobility Analyzer),»(CPC, Condensation Particle Counter), š mw l w l. Clean air œ» w» (Atomizer) š š DMA m w. DMA (Polydisperse Aerosol) Kr, Po g» y w j» wüš, CPC e p w d SMPS v mw s y w e. SMPS w ù d Base d š,» mw w d w w.»» Atomizer w, Atomizer d w ù ( ) k clean air œ» w (water droplet) j e. Atomizerƒ ƒ wš w, Ÿ w j» k». Atomizer Diffusion Dryer w w, d wš w DMA(Differential Mobility Analyzer) ü. ( )ü w ù (water droplet), d wš w ù yww» w ù j» s d j w., SMPS w 100 nm w ù d w (Water Droplet) w y ³ w v ƒ. SMPS w ù d e ( ) w Atomizer j»ƒ d e w w w š, w w w. 2. x d PSLt (STADEX SC-010-S, JSR). s³ Û0.66 nm. d d SMPS(Scanning Mobility Particle Sizer, TSI 3080). d 4ƒ, Tap( ), Filtered(1 ), DI(Deionized Water) DI Water w Distilled Water. Filtered Water, DI Water Distilled Water 1 ùkü. Tap Water w. Filtered Water( ) Microdepth Filter(5 µm), Activated Carbon Filter š Microdepth Filter(1 µm) 3ƒ vl w w š, Deionized Water(k ) 2 Deionization Filter Final 0.2 µm Filter mw wì w. (Distilled Water) DI Water 1, 2, 3 ¾ w x w. x Atomizer (Water Droplet) j»ƒ ƒ (A, B, C) w. Atomizer A j» ƒ ƒ j 10 µm~ 20 µm, B 350 nm, š C 150 nm. A B clean air w ƒ j»ƒ j r. C(EAG: Electro-spray Aerosol Generator) ƒ j» j Atomizer DMA e.» DMA ƒ ƒ» Diffusion Dryer Water Droplet k. Diffusion Dryer Silica gel Napion w sƒw. Silica gel SMPS l Diffusion Dryer w. œ š ü t jš œ» w Fig. 1. Schematic diagram of Tap water, Filtered water, DI water Distilled water creation equipment. Journal of Korean Powder Metallurgy Institute (J. Kor. Powd. Met. Inst.)

3 SMPS l ( )ƒ ù d e w 131». y³ ƒ 60% w, y t ƒ ƒ š w. t w n w wš, silica gel ƒ w ƒ w ƒ w, w š. Napion Tetrafluoroethylene(Teflon) wù, ù. 3. š 3.1. ù d š 2 PSL(Polystylene Latex) t SEM. PSL t 100 nm w ƒ x. 3 SMPS w PSL t (100 nm ) d ùk ü. (a) (b) ƒƒ /ml /ml w d w. û d w ( (a)), x ù, d Unknown Particles 100 nm w w j» yw w w. wr, (a) Fig. 2. SEM image of PSL reference material. w d w ( (b)), ƒ d, Unknown Particles w ù w. ù j» w j» d w, d e t ƒ w., vw» w û 100 nm w j» ƒ xw yw d w». ù yw d. sƒ j ù w ƒ ƒw w. 3 d ùkù PSL t j» 100 nm w d Unknown Particles w w ƒ ƒ w. PSL t PSL t ƒ w., 100 nm j» ƒ PSL ƒ w ù DI water ƒ w ƒ w. x 300 ml t 1 ml ƒw» t w w w š w. w ƒ w š w. ƒ w,» Atomizer û d ƒ w. w ƒ w vl w w 100 nm w x Unknown Particles w ƒ w w d w w 4 SMPS w Tap Water, Filtered Water, DI Water d ùkü. Tap Water vl Fig. 3. Particle size distribution result of PSL CRM (Nominal size: 100 nm) for two kind of samples with different concentration. (a) Concentration: /ml, (b) Concentration: /ml. Vol. 20, No. 2, 2013

4 132 황보선애 추민철 입자가 존재한다고 할 수 없으며, 증류수에서 측정되어지 는 입자들은 물 자체의 입자(액적)가 측정 된 것이라고 짐 작 할 수 있다. 따라서 Unknown Particle이 발현되는 첫번 째 가정이었던 PSL 표준 입자 이외의 또 다른 입자의 존 재에 대한 가정은 맞지 않은 것으로 판단된다. 그래서 두 번째 가정인 Unknown Particle이 Atomizer에서 발생되는 액적이 완전히 건조되지 않아 남아있는 잔여 액적이 측정 되어진 결과라는 가정에 대한 실험을 하였다. 액적 의 크기의 영향 분사되어지는 액적의 크기(Water Droplet Size)가 서로 다른 3종류(A, B, C)의 Atomizer를 사용해 DI Water의 입 도를 측정하였다. 여기서 A에서 발생되는 액적의 크기는 10~20 µm, B는 350 nm, 그리고 C는 150 nm이다. 그림 6 은 입도측정결과를 나타낸다. 발생되는 액적의 크기가 작 은 Atomizer를 사용 할수록 100 nm 이하에서 나타나는 Unknown Particle의 영향을 줄이는데 상당히 효과적임을 알 수 있다. 특히 가장 작은 크기의 droplet을 발생시키는 C 의 Atomizer(EAG: Electro-spray Aerosol Generator)로 측정할 경우, 100 nm 이하에서 나타나는 Unknown Particle입자의 발현을 줄이는데 탁월한 효과가 있음을 확인할 수 있었다. 그러나 C Atomizer(EAG)는 측정 가능한 입자크기가 100 nm 이하로 제한된다. 그 이유는 EAG는 입자가 통과 하는 관이 가는 금속노즐로 연결되어있으며. 노즐 직경은 40 µm로 아주 가늘어 측정대상입자에 의해 노즐이 자주 막 히는 현상이 발생해 노즐관을 교체해야하거나 측정이 되지 않는 경우가 빈번히 발생하기 때문이다. 따라서 비교적 큰 입자를 측정할 경우 EAG를 사용하여 측정하는데 어려움이 따른다. 그러므로 측정이 가능한 범위내의 작은 입자의 경우 에는 가장 작은 크기의 액적을 발생시키는 C Atomizer(EAG) 를 사용하면 정확한 측정에 유용하나, 측정대상입자가 큰 경 우에는 사용에 불편이 따르는 단점이 있다. 이상의 결과로부터, 100 nm 이하에서 발생되는 Unknown 3.3. Fig. 4. Particle size distribution results of Tap water, Filtered water and DI water. Fig. 5. Particle size distribution result of Distilled water. 통해 입자를 제거하고, 다시 이온을 제거한 후의 입도측정 결과를 보면 상당수의 미세입자의 개수농도가 줄어들었으 나, 6개의 필터를 거쳐 물속의 미세입자와 이온을 제거했음 에도 불구하고 DI Water의 측정결과를 보면 20~30 nm 정도 의 입자가 다수 존재함을 확인할 수 있다. 이온까지 제거한 DI Water에도 잔존하는 입자가 존재할 수도 있으므로 잔존 하는 입자를 완전히 제거하기 위해서 DI Water를 증류하여 얻어진 증류수를 다시 입도측정 실험을 하였다. 그림 5은 SMPS를 이용한 증류수의 입도측정결과를 나 타낸다. 증류수 장비를 통해 DI Water를 1차, 2차, 3차까 지 반복하여 증류하였고 DI Water와 1차, 2차, 3차 증류수 를 비교측정 하였다. 비교측정 결과 40~80 nm 정도의 비 교적 큰 입자들은 줄어드는 경향을 보였지만, DI Water를 3차까지 증류했음에도 불구하고 20~40 nm 정도의 입자가 다수 측정 되어 지는 것을 확인할 수 있었다. 만약 어떠한 또 다른 입자가 잔존한다는 가정이 옳다면 6개의 필터로 입자를 모두 제거하고, 이온을 제거한 DI Water를 다시 증류한 증류수로 입도측정을 할 경우 입자 들이 모두 걸러져 입자가 측정되지 않아야 한다. 하지만 DI Water에서나 DI Water를 증류한 증류수에서나 발현되 는 입자의 개수변화가 미미한 것을 미루어 볼 때, 어떠한 (Water Droplet) Fig. 6. Particle size distribution results of DI water using atomizer equipments with different droplet size. Journal of Korean Powder Metallurgy Institute (J. Kor. Powd. Met. Inst.)

5 SMPS l ( )ƒ ù d e w 133 Fig. 7. Particle size distribution results of DI water using various drying method. Paricle x ( ) w w Atomizer(») ( ) ƒ d. SMPS w ù v d d w Atomizer(») ( ) g yw d š w w 7 Diffusion Drying w DI Water d ùkü. x w 4ƒ. 1., 2. Silica gel w, 3. Napion w, 4. Silica gel Napion w. w ƒ 100 nm w xw. w x š, Silica gel Napion droplet w w. p, Silica gel Napion w 100 w xw Unknown Paticle w z. 4. SMPS w ù d e ( ) w Atomizer j»ƒ d e w w w. Tap Water, Filtered Water, DI Water, Distilled Water d DI Water w ù xk ù d w, 100 nm w Unknown Particle xw x DI Water w SMPS» Atomizer ùkù x. ( )j»ƒ 3ƒ Atomizer x mw 100 nm w ù d w EAG w d w w z x mw y w. 100 nm ƒ d w, w Napion w Diffusion dryer w yw d z x mw y w. This work is supported by NRF (contract number: ). š x [1] M. S. Kim, K. H. Choi, Y. H. Kim and J. H. Yi: Clean Technology, 38 (2007) 159 (Korean). [2] B.-K. Choi, K.-H. Kim, D.-S. So and I.-J. Yu: Prospectives of Industrial Chemistry, 10 (2007) 48. [3] Y. Kim and J. Yi: News & Information for Chemical Engineers, 23 (2005) 338. [4] A. D. Maynard: Ann. Occup. Hyg., 51 (2007) 1. [5] A. D. Maynard: A research strategy for addressing risk, PEN 03. Project on Emerging Nanotechnologies (2006). [6] Maynard, A. D., Aitken, R. J., Butz, T., Colvin, V., Donaldson, K., Oberdrster, G., Philbert, M. A., Ryan, J., Seaton, A., Stone, V., Tinkle, S. S., Tran, L., Walker, N. J., and Warheit, D. B.: Nature, 444 (2006) 267. [7] Maynard, A. D. and Kuempel, E. D.: J. Nanopart. Res., 7 (2005) 587. [8] Kwangsik Park: J. Environ Toxicol, 20 (2005) 259 (Korean). [9] Keum-Shil Cho, Jin-Sup Shin, and Jung-Hyun Kim: Polumer Science and technology, 15 (2004) 198 (Korean). Vol. 20, No. 2, 2013

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