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1 Journal of the Combustion Society of Japan Vol.55 No.171 (2013) ORIGINAL PAPER 酸化微粒子塗布バーナによる表面改質 Surface Modification by Oxide Particles Spray Burner 1 2 * GOTO, Masaya 1, TAKAHASHI, Shuhei 2 *, HAMAGUCHI Keita 1, IHARA, Tadayoshi 2, and WAKAI, Kazunori Gifu University, 1-1 Yanagido, Gifu, Gifu , Japan Gifu University, 1-1 Yanagido, Gifu, Gifu , Japan ; Received 21 August, 2012; Accepted 1 November, 2012 Abstract : The effect of the sintering characteristics of silica and titania particles on surface modification was investigated experimentally. The turbulent premixed burner, in which hexamethyl disiloxane (HMDS) or titanium tetraisopropoxide (TTIP) diluted with isopropyl alcohol (IPA) was sprayed, were used to feed silica or titania particles on the base material. According to the observation by SEM, the silica particles were agglomerates of small primary particles, whereas the titania particles had spherical shape under the same burner condition. Additionally, the coverage ratio of silica was larger than that of titania. The difference in the shape of those particles was due to the difference in the characteristic sintering time between silica and titania; the characteristic sintering time of titania was smaller than that of silica by 2-4 orders of magnitude. The result of the adhesive strength test showed that the adhesive strength was enhanced by 3-4 times at the maximum with HMDS. However, the excess surface particles after surface was saturated reduced the strength, therefore, there was an optimal condition for the spray time and the spray mass concentration. With TTIP, the adhesive strength was not so enhanced compared with HMDS, which was due to the spherical shape of titania particles that resulted in poor absorption on the base. Key Words : Oxide particles, Burner, Surface, Adhesive strength, Silica, Titania 1. 緒言 (VOC) * Corresponding author. shuhei@gifu-u.ac.jp ( ) VOC (O[Si(CH3)3]2 (73)

74 55 171 2013 HMDS) (Ti[OCH(CH3)2]4 TTIP) 2 (SEM) 2 SEM 2. 実験装置および方法 Fig.

0 ml/min (JIS K5600-5-7) ( ) ( ) 20 mm Fig.2 24 24 1 MPa/s 90 s 3. 表面観察における結果および考察 Fig.1 Schematic of oxide particles spray burner. Fig.2 Concept of pull-off adhesion test.

2 HMDS) (Ti[OCH(CH3)2]4 TTIP) 2 (SEM) 2 SEM 2. 実験装置および方法 Fig.1 (KOFLOC MODEL 8500 MODEL 8550) (KD Scientific KDS100 IC300 ) (ATOMAX AM6S-OSV) 2.0 L/min ( 0.20 MP 4.0 L/min 17 L/min (IPA: C3H8O) 1.0 ml/min (JIS K ) ( ) ( ) 20 mm Fig MPa/s 90 s 3. 表面観察における結果および考察 Fig.1 Schematic of oxide particles spray burner. Fig.2 Concept of pull-off adhesion test SEM による基材表面観察結果 IPA 2 wt% 5 wt% 10 wt% 10 mm 100 mm 10 mm 10 s SEM ( S-3000N S-4300) 20 mm 20 mm Fig.3( 30 mm 1000 SEM HMDS 2 wt% 5 wt% 10 wt% 10 s 2 wt% 5 wt% 10 wt% Fig.3( (74)

10 wt% 30 mm 10 s 3000 SEM Fig.4 HMDS TTIP SEM 0.1 μm 3 μm Fig.

The distance between the burner and the base is 30mm, and the spray time is 10s.

3 75 Fig.3 SEM images of particles using HMDS and TTIP on the aluminum base with varying the mass concentration of spray. The distance between the burner and the base is 30mm, and the spray time is 10sec. 10 wt% 30 mm 10 s 3000 SEM Fig.4 HMDS TTIP SEM 0.1 μm 3 μm Fig.4 Details of sintered particles on the aluminum base of HMDS and TTIP. The distance between the burner and the base is 30mm, and the spray time is 10s. The mass concentration is 10wt%. TTIP SEM Fig.3( 2 wt% 5 wt% 10 wt% 10 s 2 wt% HMDS 5 wt% 10 wt% 3.2. XPS による基材表面分析結果 SEM X ( Quantera-SXM XPS) 10 wt% 30 mm 10 s 350 μm 350 μm Fig.5 Fig.5( HMDS Si C1s ev ev ev (SiO2) Fig.5( TTIP Ti (75)

4 Fig.6 Sintering of primary particles and neck formation. Fig.5 XPS analysis of particles with HMDS and TTIP. ev ev ev (TiO2) Fig.7 Characteristic sintering time of silica and titania with varying the temperature and the primary particle diameter 種類の試薬における焼結性状 Fig.4 HMDS TTIP 2 (Fig.6) [1,2] 1 1 τ Fig (d pi /2) 0.83 (1) [3,4] l f E A T R SiO2 TiO2 [4] τsilica τtitania Xiong [5] Kobata [3,6] (2) (3) SiO2 TiO2 1 Seto [7] 5 nm 15 nm (2)(3) Fig nm 10 nm 15 nm 1700 K SiO2 (76)

5 77 Fig.9 Particle size distribution on the aluminum base with varying the mass concentration of TTIP. The distance between the burner and the base is 30mm, and the spray time is 10s. Fig.8 Coverage ratio on the aluminum base with varying the distance between the burner and the aluminum base, and the mass concentration of HMDS and TTIP. The spray time is 10s s TiO s SiO2 2 4 Eggersdorfer [8] τ t = 10 1 (Fig.6 ) t > 10 4 (Fig.6 ) SiO2 Fig.4 1 TiO 基材表面での粒子の吸着特性 2 wt% 5 wt% 10 wt% 10 mm 100 mm 10 s (Media Cybernetics Image-Pro Plus ver.4.0) Fig.8 HMDS TTIP SEM Fig.8( 10 s HMDS 2 wt% SEM 5 wt% 10 mm 5 wt% 10 wt% 50 % SEM 50 % 50 % HMDS 10 s 5 wt% SiO2 Fig.4 SiO2 SiO2 SiO2 TTIP (Fig.8() 10 wt% HMDS 50 % 2 wt% 5 wt% 20 mm 30 mm TiO2 250 nm SiO2 10 wt% Fig.9 30 mm 10 s TTIP 10 wt% 2 1 μm (77)

6 Fig.10 Coverage ratio on the glass base with varying the spray time and the distance between the burner and the base. HMDS and TTIP. The mass concentration is 10wt%. Fig.11 Adhesion force with varying the spray time and the distance between the burner and the base. HMDS and TTIP. The base is glass, and the mass concentration is 10wt%. HMDS 4. 付着性試験の結果および考察 4.1. バーナ火炎の照射時間の影響 10 wt% 10 mm 30 mm 100 mm 3 1 s 10 s 1 s 10 ( 30 mm 30 mm) SEM ( No.541) Fig.10 HMDS 10 mm 50 % 1 s SiO2 TTIP HMDS Fig.11 HMDS Fig.11( (78)

7 79 TTIP HMDS SiO2 TiO2 Fig.11( HMDS TTIP 4.2. 試薬濃度の影響 HMDS Fig.10( 10 wt% 1 s 50 % 1 s 10 wt% 30 mm ( 3M Scotch ) HMDS Fig.12( 3 wt% 10 wt% 1 wt% 5 wt% wt% 5 wt% 6 wt% 50 % 1 s 6 wt% TTIP Fig.12( TTIP Fig.10( 10 s 10 wt% 8 % HMDS 10 wt% 60 wt% wt% HMDS 10 HMDS Fig.12 Adhesion force and coverage ratio with varying mass concentration of HMDS and TTIP. The base is glass, the distance between the burner and the base is 30mm, and the spray time is 1s. TTIP TiO2 HMDS 5. 結言 HMDS TTIP 2 SEM 1. HMDS TTIP HMDS TTIP TiO2 SiO (79)

8 HMDS 5 wt% 10 wt% 10 s TTIP 2 wt% 5 wt% 20 mm 30 mm 10 wt% 3. HMDS HMDS 1 s 5 wt% 3 4 TTIP 謝辞 SEM XPS References 1. Nakaso, K., Shimada, M. and Okuyama, K., Earozoru Kenkyu (in Japanese), 15(3): (2000). 2. Nakaso, K., Okuyama, K., Shimada, M. and Pratsinis, S. E., Chemical Engineering Science, 58: (2003). 3. Kobata, A., Kusakabe, K.. and Morooka, A., AIChE Journal, 37: (1991). 4. Okuyama, K., Powder Technology, Taylor & Francis Group, LLC: (2007). 5. Xiong, Y., and Pratsinis, S. E., Journal of Aerosol Science, 24: (1993). 6. Seto, T., Shimada, M. and Okuyama, K., Aerosol Science and Technology, 23: (1995). 7. Seto, T., Hirota, A., Fujimoto, T., Shimada, M. and Okuyama, K., Aerosol Science and Technology, 27: (1997). 8. Eggersdorfer, M. L., Kadau, D., Herrmann, H. J. and Pratsinis, S. E., Journal of Aerosol Science, 46: 7-19 (2012). (80)

特-4.indd

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