O O

lotus effect

/

~

(superhydrophobic surface)

()

OTS(Octadecyltrichlorosilane) TEOS (Tetraethylorthosilicate)

159

Abstract Superhydrophobic surfaces are generally made by lowering the surface energy and increasing the

surface roughness. In this experiment, we use different methods of spreading silicon dioxide nanoparticles properly on the surface in order to increase the surface roughness and also make superhydrophobic surfaces.

In the beginning, we find that the calcinations can cause its silicon dioxide nanoparticles to stick

together instead of increasing the contact angles. Then, add OTS (Octadecyltrichlorosilane) directly to manufacture process of sol-gel, and observe the situations of the average length and the spread of silicon dioxide nanoparticles with the time goes by. After a period of time, we will discover that many obvious big particles deposit and spin-coating on the glass surfaces flop easily. Hence, this phenomenon is nt proper for the following experiments or other uses. However, the contact angles have nothing to do with dropping the sol-gel catalyzed ammonia to TEOS(Tetraethylorthosilicate) by different flowing rates.

Finally, it is crucial for us to use the sandpapers to brush on the surfaces because it may cause the

silicon dioxide nanoparticles to spread well and obviously increase the contact angles. Combining the silicon dioxide surfaces with the change of spin-coating rate and the cover with hydrophobic SAM, we have made the superhydrophobic surfaces of 159.

()

TEOS ( )

OTS

Karl Fischer atomic force microscopeAFM (Scanning Electron MicroscopeSEM) ()

PDMS (polydimethylsiloxane) TEOS (Tetraethylorthosilicate) Si(OC2H5)4 OTS (Octadecyltrichlorosilane) C18H37Cl3Si FTS(tridecafluoro-1,1,2,2-tetrahydrooctyl)-1-trichlorosilane)

Onda et al. (1996) alkylketene dimmer (AKD)

170 Erbil et al. (2003) p-xylene good-solventnon-solventmethyl ethyl ketone polypropylene 160 (poly)tetrafluoroethylene (Miller et al.1849)(Shibuichi et al.1996)(Coulson et al.2000)

pHSAMNakajima et al.2000

(TEOStetraethyl orthosilicate)Si(OC2H

5)

4

Si(OR)4 + H

2O Si(OR)

3(OH) + ROH

Si(OR)3(OH) + Si(OR)

3(OH) (OR)

3Si-O-Si(OR)

3 + H

2O

Si(OR)3(OH) + Si(OR)

4 (OR)

3Si-O-Si(OR)

3 + ROH

TEOS ()

() NH3(aq) dip coating 13mL NH3(aq) 50mL 45 30 2 0.025mL0.05mL0.1mL0.2 mL0.4 mL 3

mLTEOS 3 90 4 NH3(aq) 30

() 1 2 3 424 5 6 ()

() NH3(aq) dip coating 136.8g 5.35g 10 2 2.30g TEOS 20 3 550mL 60 4 5 5 110 60

()

() 1 2 3 424 5 6

()

OTS

() NH3(aq) 136.8g 5.35g 10 2 2.30g TEOS 20 3 550mL 60 4 OTS ()

()

, 7:3() () () NH3(aq) 136.8g 5.35g 10 2 2.30g TEOS 20 3 550mL 60 4 5 60 60

() 1 2 3 424 5 6 ()

() NH3(aq) 136.8g 5.35g 10 2 2.30g TEOS 20 3 550mL 60 4 5 60 60

() 1 2 3 424 5 6

()

TEOS ()

TEOS () 1~2 OTS 105

OTS

OTS OTS OTS OTS 270~310nm OTS 60 () OTS OTS 30

4000rpm()

() 4000rpm

TEOS () OTS 30

4000rpm

159(

)

H.M. Shang, Y. Wang, S.J. Limmer,T.P. Chou, K. Takahashi,G.Z. Cao2005

Optically transparent superhydrophobic silica-based filmsThe Solid Films47237-43

Kota Sreenivasa Rao, Khalil El-Hami, Tsutomu Kodaki, Kazumi Matsushige, Keisuke Makino2005A novel method for synthesis of silica nanoparticlesJournal of Colloid and Interface Science289125-131

Michele Ferrari, Francesca Ravera, and Libero Liggieri2005Preparation of a superhydrophobic surface by mixed inorganic-organic coatingApplied Physics Letters88203125

(A:B:C:D:E: SampleF: G:H:I: J: CCD cameraK:L:)

(mL/)

(degree) Average

100~105 100~1050.4 104.88 107.85 105.14 105.6 105.78 105.85 0.2 109.24 111.42 102.53 106.52 110.13 107.9680.1 105.30 107.86 102.42 108.44 110.78 106.96 0.05 108.45 105.84 107.46 100.25 106.89 105.7780.025 110.20 108.52 101.17 110.66 106.18 107.346

TEOS ()

(degree) Average 100~105 100~105

130.17 130.23 131.28 130.56 129.52 124.47 121.66 125.2167

AFM

AFM

Size(nm) Intensity Volume Number Peak Analysis by intensity

171 0 0 0 Peak Area Mean Width 177.7 0 0 0 1 100 280.9 68.4184.6 0 0 0 191.9 0 0 0.1 Peak Analysis by volume 199.4 0.1 0.1 0.3 207.2 0.2 0.3 0.7 Peak Area Mean Width 215.4 0.6 0.7 1.5 1 100 284.1 75.5223.8 1.5 1.6 3 232.6 3.1 3.1 5.2 Peak Analysis by number 241.7 5.5 5.4 7.9 251.2 8.7 8.1 10.7 Peak Area Mean Width

261 12 10.8 12.8 1 100 274 72.3271.3 14.3 12.9 13.7 281.9 14.8 13.6 12.9

293 13.4 12.7 10.9 304.5 10.5 10.7 8.2 316.4 7.2 8 5.5 328.8 4.3 5.4 3.3 341.7 2.2 3.2 1.8 355.1 1 1.8 0.9

369 0.4 0.9 0.4 383.5 0.1 0.4 0.2 398.6 0 0.2 0.1 414.2 0 0.1 0

OTS 0~30

OTS 0~30

Size distribution(s)

500Diameter (nm)

5

10

15

% in

cla

ss

Size(nm) Intensity Volume Number Peak Analysis by intensity

166.5 0 0 0 Peak Area Mean Width 173.6 0 0 0 1 100 285.2 75.8

181 0 0 0 188.7 0 0 0.1 Peak Analysis by volume 196.8 0.1 0.1 0.3 205.2 0.2 0.3 0.8 Peak Area Mean Width

214 0.7 0.8 1.7 1 100 290.4 85.2223.2 1.6 1.7 3.2 232.7 3.2 3.2 5.4 Peak Analysis by number 242.7 5.7 5.3 8.1 253.1 8.9 8 10.8 Peak Area Mean Width 263.9 12.1 10.7 12.8 1 100 277.6 80.6275.2 14.4 12.6 13.5

287 14.8 13.3 12.6 299.2 13.2 12.5 10.6

312 10.3 10.6 7.9 325.4 7 8 5.3 339.3 4.1 5.5 3.2 353.8 2.1 3.4 1.8

369 0.9 1.9 0.9 384.7 0.4 1 0.4 401.2 0.1 0.5 0.2 418.4 0 0.3 0.1 436.3 0 0.2 0

OTS 30~60

OTS 30~60

Size distribution(s)

500Diameter (nm)

5

10

15

% in

cla

ss

Size(nm) Intensity Volume Number Peak Analysis by intensity

156 0 0 0 Peak Area Mean Width 164.9 0 0 0 1 100 315.6 111.3174.3 0 0 0 184.2 0 0 0.1 Peak Analysis by volume 194.7 0.1 0 0.3 205.8 0.3 0.1 0.6 Peak Area Mean Width 217.5 0.8 0.2 1.2 1 29 326.7 109.3229.8 1.8 0.4 2.1 2 71 465.6 56242.9 3.6 0.8 3.4 256.7 6.2 1.4 4.8 Peak Analysis by number 271.3 9.5 2.1 6.2 286.8 12.6 2.8 7.1 Peak Area Mean Width 303.1 14.6 3.5 7.4 1 59.9 310.8 138.8320.3 14.6 3.9 7.1 2 40.1 467.5 57338.6 12.8 4 6.2 357.8 9.7 3.8 5.1 378.2 6.5 3.5 4 399.7 3.7 3.3 3.2 422.5 1.9 3.7 2.9 446.5 0.8 18.6 11.1 471.9 0.3 31.9 18.3 498.7 0.1 15.6 8.9 527.1 0 0.2 0.1 557.1 0 0 0

OTS 60~90

OTS 60~90

Size distribution(s)

500Diameter (nm)

5

10

15

% in

cla

ss

Size(nm) Intensity Volume Number Peak Analysis by intensity

232.1 0 0 0 Peak Area Mean Width 236 0 0 0 1 100 292.3 30.9240 0 0 0 244 0 0 0 Peak Analysis by volume

248.1 0 0 0 252.3 0.1 0.1 0.1 Peak Area Mean Width 256.5 0.2 0.3 0.4 1 100 293 32.4260.8 0.6 0.7 0.9 265.2 1.5 1.5 2 Peak Analysis by number 269.7 3.1 3.1 3.8 274.2 5.5 5.4 6.4 Peak Area Mean Width 278.8 8.7 8.3 9.4 1 100 291.2 32.4283.5 12 11.3 12.2 288.3 14.3 13.5 14 293.1 14.8 14.2 14

298 13.4 13.2 12.4 303.1 10.5 10.8 9.7 308.1 7.2 7.7 6.6 313.3 4.3 4.9 4 318.6 2.2 2.7 2.1 323.9 1 1.4 1 329.4 0.4 0.6 0.4 334.9 0.1 0.2 0.2 340.6 0 0.1 0.1

OTS 90~120

OTS 90~120

Size distribution(s)

200 220 240 260 280 320 360Diameter (nm)

5

10

15

% in

cla

ss

Size(nm) Intensity Volume Number Peak Analysis by intensity

24.4 0 0 0 Peak Area Mean Width 30.7 0 0 0 1 56.6 253 62.938.6 0 0 0 2 43.4 555.6 246.748.7 0 0 0 61.3 0 0 0 Peak Analysis by volume 77.1 0 0 0 97.1 0 0 0 Peak Area Mean Width

122.3 0 0 0 1 2.6 252 46.3154 0 0 0 2 97.4 495.6 232.2

193.9 0 0.6 4 244.1 48.7 1.3 8.4 Peak Analysis by number 307.3 8 0.8 4.7

387 0 23.7 20.7 Peak Area Mean Width 487.2 19.9 47.9 41 1 16.3 249.9 48.1613.4 23.5 25 20.9 2 83.7 484.9 231772.4 0 0.7 0.3 972.5 0 0 0

1224.4 0 0 0 1541.6 0 0 0

1941 0 0 0 2443.9 0 0 0

3077 0 0 0 3874.2 0 0 0

4878 0 0 0

OTS 0~30

OTS 0~30

Size distribution(s)

5 10 50 100 500 Diameter (nm) (x10^1)

20

40% in

cla

ss

Size(nm) Intensity Volume Number Peak Analysis by intensity

242 0 0.9 1.8 Peak Area Mean Width 304.7 8.8 25.9 26.8 1 100 376.7 93.4383.6 91.2 49.1 48.2

483 0 24.1 23.2 Peak Analysis by volume 608.2 0 0 0 765.7 0 0 0 Peak Area Mean Width 964.1 0 0 0 1 100 385.8 180

1213.9 0 0 0 1528.4 0 0 0 Peak Analysis by number 1924.4 0 0 0 2422.9 0 0 0 Peak Area Mean Width 3050.6 0 0 0 1 100 383 181.5

3841 0 0 0 4836.1 0 0 0

6089 0 0 0 7666.6 0 0 0 9652.8 0 0 0

12153.7 0 0 0 15302.4 0 0 0 19266.9 0 0 0 24258.5 0 0 0 30543.4 0 0 0 38456.5 0 0 0 48419.7 0 0 0

OTS 30~60

OTS 30~60

Size distribution(s)

5 10 50 100 500Diameter (nm) (x10^2)

50

100

% in

cla

ss

Size(nm) Intensity Volume Number Peak Analysis by intensity

56 0 0.2 18.5 Peak Area Mean Width 68.4 0.7 0.5 40.5 1 1 74 24.183.6 0.4 0.3 25.3 2 82.2 563.2 479.8

102.1 0 0.1 3.4 3 16.7 1614.8 984.6124.8 0 0 0 152.4 0 0 0 Peak Analysis by volume 186.2 0 0 0 227.5 0.5 0.1 0.1 Peak Area Mean Width

278 3.8 0.4 0.4 1 1 73 33339.6 9.6 2.4 1.2 2 45.4 533.3 303.7414.9 15.4 11 3.2 3 53.6 1218.9 596.8506.8 18.6 16.8 4 619.2 16.8 11.2 1.9 Peak Analysis by number 756.4 11.3 6.2 0.4 924.1 5.6 12.3 0.4 Peak Area Mean Width 1129 2.8 18.9 0.4 1 87.4 71.5 30.9

1379.3 4 10.9 0.2 2 11.6 493.5 247.61685 6.2 3.6 0

2058.5 4.2 3.6 0 2514.9 0 1.4 0 3072.4 0 0 0 3753.5 0 0 0 4585.5 0 0 0

5602 0 0 0

OTS 60~90

OTS 60~90

Size distribution(s)

5 10 50 100 500Diameter (nm) (x10^1)

10

20

% in

cla

ss

Size(nm) Intensity Volume Number Peak Analysis by intensity

64 0 0 7.3 Peak Area Mean Width80.5 0.6 0 17.8 1 100 568.4 621.9101.4 0.9 0.1 14.8 127.7 1.3 0 6.1 Peak Analysis by volume 160.7 1.8 0 2.5 202.4 2.8 0 1.2 Peak Area Mean Width254.8 4.9 0.1 0.9 1 99.8 800.4 382.6320.8 8.3 0.2 1.2 403.9 13.1 1.4 3 Peak Analysis by number 508.5 18.2 2.3 4 640.3 20.9 24.8 11.7 Peak Area Mean Width806.1 18.3 47.2 19.7 1 50.1 99.8 52.7 1015 8.9 23.7 9.8 2 49.9 739.9 405.8

1277.9 0 0.1 0 1608.9 0 0 0 2025.7 0 0 0 2550.5 0 0 0 3211.2 0 0 0 4043.1 0 0 0 5090.5 0 0 0 6409.2 0 0 0 8069.6 0 0 0 10160.1 0 0 0 12792.1 0 0 0

OTS 90~120

OTS 90~120

Size distribution(s)

10 50 100 5001000Diameter (nm) (x10^1)

10

20%

in c

lass

whetted times

(degree) Average

Space 100105 100~105Five 144.80 142.47 147.20 150.34 150.09 137.59 139.23 139.21 146.14 150.65 147.772Ten 146.25 151.49 149.60 148.53 143.32 147.28 150.90 149.11 146.88 148.30 148.166

Many 147.71 152.26 140.83 149.27 148.22 148.55 138.55 141.11 147.46 142.65 145.661

(a)(b)(c)

(d)frame

d (mm)

frame pixels

frame frame

(a) (b)

(c) (d)

(a)(b)(c)

(d)frame

d (mm)

frame pixels

frame frame

(a) (b)

(c) (d)

(a)(b)(c)

(d)frame

d (mm)

frame pixels

d (mm)

frame frame

(a) (b)

(c) (d)

frame frame

(a) (b)

(c) (d)

Speed(rpm) A(degree) Average

space 100~105 100~1051012 147.75 146.25 140.89 145.15 138.60 143.728 2944 151.15 144.56 146.97 152.39 145.39 148.092 4528 129.65 133.06 135.21 125.09 133.08 131.218 6068 131.90 125.35 132.34 130.69 131.59 130.374

Speed(rpm) B(degree) Average

space 120 120 1012 147.81 153.48 154.15 149.70 150.80 151.188 2944 145.04 153.25 153.42 151.20 ------ 150.72754528 147.75 148.33 149.05 145.70 149.03 147.972 6068 125.62 125.71 124.46 119.93 116.39 122.422

A (Octadecyltrichlorosilane (OTS)

B (tridecafluoro-1,1,2,2-tetrahydrooctyl)-1-trichlorosilane (FTS)

AFM --- 1012rpm

AFM --- 2944rpm

AFM --- 4528rpm

AFM --- 6068rpm

SEM

157.61159.79

0 0.5 1 1.5 2156.5

157

157.5

158

158.5

159

0 0.5 1 1.5 2158.5

159

159.5

160

160.5

161

0 0.5 1 1.5 2-0.5

0

0.5

1

1.5

2

0 200 400 600 800-100

0

100

200

300

400

157.61159.79(a)(b)

(c)(d)frame

lotus effect Abstract