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Photonic crystals in biology

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Poster Session, Tuesday, June 15<br />

Theme A1 - B702<br />

Submicron Sized Boric Acid Particles Production By Wet Mill<strong>in</strong>g<br />

Mehmet Ikbal Isik 1* Em<strong>in</strong>e Bakan 1 Ozgenur Kahvecioglu 1 Servet Timur 1<br />

1 Metallurgical & Materials Eng<strong>in</strong>eer<strong>in</strong>g Department, Istanbul Technical University, 34469 Istanbul, Turkey<br />

Abstract— Submicron sized boric acid particles are be<strong>in</strong>g used <strong>in</strong> traditional lubrication oils due to provid<strong>in</strong>g low friction<br />

coefficient while it is friendly to environment. In the present study, size and morphology changes of wet milled boric acid<br />

particles were <strong>in</strong>vestigated and characterized by SEM, XRD, BET, TG-DTA and MasterSizer. It is seen that <strong>in</strong>creas<strong>in</strong>g<br />

time of mill<strong>in</strong>g results <strong>in</strong> a smaller particle formation and more homogen size distribution.<br />

Submicron sized particles have received <strong>in</strong>creas<strong>in</strong>g <strong>in</strong>terest<br />

<strong>in</strong> miscellaneous fields of science dur<strong>in</strong>g the last years [1-3].<br />

Size reduction by us<strong>in</strong>g mechanical mill<strong>in</strong>g is simple and<br />

widely used process <strong>in</strong> <strong>in</strong>dustrial or laboratory scale [4,5].<br />

High energy ball mill<strong>in</strong>g is based on collisions between<br />

particles and balls that causes smaller particles formation.<br />

Boric acid (H 3 BO 3 ) also known as boracic acid, orthoboric<br />

acid, boron trihydroxide, borofax, bortrac, dia flea-mate, flea<br />

prufe, trihydroxyborane, trihydroxyborone, three elephant,<br />

hydrogen orthoborate, sassolite, acidum boricum, a well<br />

known antiseptic and pesticide is a colorless, odorless white<br />

crystall<strong>in</strong>e solid [6]. Major process parameters that are<br />

alter<strong>in</strong>g particle size and morphology can be summarized as<br />

miller type, mill<strong>in</strong>g atmosphere, mill<strong>in</strong>g media, ball to<br />

powder ratio, mill<strong>in</strong>g time and mill<strong>in</strong>g temperature. In this<br />

study, all these parameters were kept constant except mill<strong>in</strong>g<br />

time.<br />

For further understand<strong>in</strong>g of production of boric acid<br />

particles some of other techniques were studied [7]. Dry<br />

mill<strong>in</strong>g and flame spray synthesis of boric acid particles<br />

were <strong>in</strong>vestigated with<strong>in</strong> our research group. Fig. 1-a shows<br />

120 m<strong>in</strong> dry milled and Fig. 1-b shows flame spray<br />

synthesized boric acid particles SEM images.<br />

a<br />

b<br />

Figure 1. SEM image of boric acid particles produced by<br />

different techniques; (a) 120 m<strong>in</strong> dry milled and (b) flame spray<br />

synthesized.<br />

Precursor material used for high energy ball mill<strong>in</strong>g was<br />

high purity boric acid powder. Ball to powder ratio (BPR)<br />

was kept constant <strong>in</strong> all set of experiments as 10:1. Mill<strong>in</strong>g<br />

process was done with sta<strong>in</strong>less steel balls and conta<strong>in</strong>ers<br />

us<strong>in</strong>g 15 ml of hexane as dispersant media. Experimental<br />

mill<strong>in</strong>g durations were chosen as 30-90-150-210 m<strong>in</strong>ute. In<br />

order to remove moisture boric acid precursor powder was<br />

heated to 85 o C and kept at this temperature for 24 hours.<br />

TG-DTA analysis (Fig. 2) showed that boric acid<br />

decomposition does not occur at 85 o C. After moisture<br />

removal, powder is prepared for further process stages.<br />

As it is well known, X-ray diffraction patterns of<br />

materials show an alteration when size reduction achieved.<br />

XRD patterns of wet milled particles showed broaden<strong>in</strong>g<br />

that proves size reduction. MasterSizer was used to get<br />

Weight (mg)<br />

Temperature ( o C)<br />

Figure 2. Thermo gravimetric-differential thermal analysis of<br />

high purity boric acid.<br />

size and size distribution of particles and BET analyses for<br />

specific surface area determ<strong>in</strong>ation. Size distribution of<br />

particles becomes more homogen and f<strong>in</strong>er particles were<br />

formed with <strong>in</strong>creas<strong>in</strong>g mill<strong>in</strong>g time. However, there is no<br />

doubt that agglomeration will create a great challenge <strong>in</strong><br />

longer mill<strong>in</strong>g time while energy consumption <strong>in</strong>creases and<br />

energy efficiency goes down.<br />

In conclusion, it is showed that;<br />

•Wet mill<strong>in</strong>g is capable of produc<strong>in</strong>g submicron sized<br />

boric acid particles.<br />

•Sta<strong>in</strong>less steel balls and conta<strong>in</strong>er are found to be proper<br />

for mill<strong>in</strong>g boric acid powders.<br />

•Increas<strong>in</strong>g mill<strong>in</strong>g time provides f<strong>in</strong>er particle size and<br />

better size distribution.<br />

•Temperature <strong>in</strong>creases caused by collisions is found to be<br />

negligible.<br />

Special thanks to Prof.Dr. M. Lütfi Öveçoğlu, Asst.Prof.Dr. Nuri<br />

SOLAK, Hüsey<strong>in</strong> Sezer, Ph.D. Hasan Gökçe, M.Sc. Şeyma Duman<br />

*Correspond<strong>in</strong>g author: isikme@itu.edu.tr<br />

[1] A. G. Gnedovets, A. V. Gusarov, I. Smurov, Applied Surface<br />

Science, 154-155 (2000) 508-513<br />

[2] L.C. Santa Maria, M.A.S. Costa, J.G.M. Soares, S.H. Wang,<br />

M.R. Silva, Polymer, 46 (2005) 11288-11293<br />

[3] S.S. Dukh<strong>in</strong>, Y. Shen, R. Dave, R. Pfeffer, Advances <strong>in</strong><br />

Colloid and Interface Science, 134-135 (2007) 72-88M.L.<br />

Steigerwald, L.E. Brus, Annu. Rev. Mater. Sci. 19 (1986) 471.<br />

[4] A. Calka, D. Wexler, A.Y. Mosbah, Journal of Alloys and<br />

Compounds, 434-435 (2007) 463-466<br />

[5] T. Isobe, Y. Hotta, K. Watari, Materials Science and<br />

Eng<strong>in</strong>eer<strong>in</strong>g: B, 148 (2008) 192-195<br />

[6] Material Safety data for boric acid,<br />

http://msds.chem.ox.ac.uk/BO/boric_acid.html (2005).<br />

[7] M.I. Isik, M.Sc. thesis, Flame Sythhesis of Nano-boric Acid,<br />

Istanbul Technical University (2007).<br />

Microvolt (μV)<br />

6th Nanoscience and Nanotechnology Conference, zmir, 2010 326

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