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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-solvent
non-solvent
methyl ethyl ketone
polypropylene 160 (poly)tetrafluoroethylene
(Miller et al.1849)(Shibuichi et al.
1996)(Coulson et al.2000)
pH
SAM

Nakajima et al.2000
(TEOStetraethyl orthosilicate)Si(OC2H5)4

Si(OR)4 + H2O Si(OR)3(OH) + ROH


Si(OR)3(OH) + Si(OR)3(OH) (OR)3Si-O-Si(OR)3 + H2O

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 Films472
37-43
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

100~105

0.4

104.88

107.85

105.14

105.6

105.78

105.85

0.2

109.24

111.42

102.53

106.52

110.13

107.968

0.1

105.30

107.86

102.42

108.44

110.78

106.96

0.05

108.45

105.84

107.46

100.25

106.89

105.778

0.025

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 Peak

Area

177.7

184.6

191.9

199.4

0.1

0.1

0.3

207.2

0.2

0.3

0.7 Peak

215.4

0.6

0.7

1.5

223.8

1.5

1.6

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

261

12

10.8

12.8

271.3

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

5.5

328.8

4.3

5.4

3.3

341.7

2.2

3.2

1.8

355.1

1.8

0.9

369

0.4

0.9

0.4

383.5

0.1

0.4

0.2

398.6

0.2

0.1

414.2

0.1

Mean
100

Width
280.9

68.4

0.1 Peak Analysis by volume


Area
1

10.7 Peak

Mean
100

Area
1

Width
284.1

Mean
100

OTS 0~30

75.5

Width
274

72.3

% in class

Size distribution(s)

15

10

500
Diameter (nm)
OTS 0~30

Size(nm)

Intensity

Volume

Number

Peak Analysis by intensity

166.5

0 Peak

Area

173.6

181

188.7

196.8

0.1

0.1

0.3

205.2

0.2

0.3

0.8 Peak

214

0.7

0.8

1.7

223.2

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

263.9

12.1

10.7

12.8

275.2

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

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

0.4

401.2

0.1

0.5

0.2

418.4

0.3

0.1

436.3

0.2

Mean
100

Width
285.2

75.8

0.1 Peak Analysis by volume


Area
1

10.8 Peak

Mean
100

Area
1

Width
290.4

Mean
100

OTS 30~60

85.2

Width
277.6

80.6

% in class

Size distribution(s)

15

10

500
Diameter (nm)
OTS 30~60

Size(nm)

Intensity

Volume

Number

Peak Analysis by intensity

156

0 Peak

Area

164.9

174.3

184.2

0.1 Peak Analysis by volume

194.7

0.1

0.3

205.8

0.3

0.1

0.6 Peak

217.5

0.8

0.2

1.2

29

326.7

109.3

229.8

1.8

0.4

2.1

71

465.6

56

242.9

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

303.1

14.6

3.5

7.4

59.9

310.8

138.8

320.3

14.6

3.9

7.1

40.1

467.5

57

338.6

12.8

6.2

357.8

9.7

3.8

5.1

378.2

6.5

3.5

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

0.2

0.1

557.1

Mean
100

Area

Width
315.6

Mean

Area

Width

Mean

OTS 60~90

111.3

Width

% in class

Size distribution(s)

15

10

500
Diameter (nm)
OTS 60~90

Size(nm)

Intensity

Volume

Number

Peak Analysis by intensity

232.1

0 Peak

Area

236

240

244

0 Peak Analysis by volume

248.1

252.3

0.1

0.1

0.1 Peak

256.5

0.2

0.3

0.4

260.8

0.6

0.7

0.9

265.2

1.5

1.5

269.7

3.1

3.1

3.8

274.2

5.5

5.4

6.4 Peak

278.8

8.7

8.3

9.4

283.5

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

318.6

2.2

2.7

2.1

323.9

1.4

329.4

0.4

0.6

0.4

334.9

0.1

0.2

0.2

340.6

0.1

0.1

Mean
100

Area
1

Width
292.3

Mean
100

30.9

Width
293

32.4

2 Peak Analysis by number


Area
1

Mean
100

OTS 90~120

Width
291.2

32.4

% in class

Size distribution(s)

15

10

200 220 240 260 280


320 360
Diameter (nm)
OTS 90~120

Size(nm)

Intensity

Volume

Number

Peak Analysis by intensity

24.4

0 Peak

Area

Mean

30.7

56.6

253

62.9

38.6

43.4

555.6

246.7

48.7

61.3

0 Peak Analysis by volume

77.1

97.1

0 Peak

122.3

2.6

252

46.3

154

97.4

495.6

232.2

193.9

0.6

244.1

48.7

1.3

8.4 Peak Analysis by number

307.3

0.8

4.7

387

23.7

487.2

19.9

47.9

41

16.3

249.9

48.1

613.4

23.5

25

20.9

83.7

484.9

231

772.4

0.7

0.3

972.5

1224.4

1541.6

1941

2443.9

3077

3874.2

4878

Area

20.7 Peak

Mean

Area

OTS 0~30

Width

Width

Mean

Width

% in class

Size distribution(s)

40

20

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

OTS 0~30

500

Size(nm)

Intensity

Volume

Number

Peak Analysis by intensity

242

0.9

1.8 Peak

Area

304.7

8.8

25.9

26.8

383.6

91.2

49.1

48.2

483

24.1

23.2 Peak Analysis by volume

608.2

765.7

0 Peak

964.1

1213.9

1528.4

0 Peak Analysis by number

1924.4

2422.9

0 Peak

3050.6

3841

4836.1

6089

7666.6

9652.8

12153.7

15302.4

19266.9

24258.5

30543.4

38456.5

48419.7

Mean
100

Area
1

376.7

Mean
100

Area
1

OTS 30~60

Width

Width
385.8

Mean
100

93.4

180

Width
383

181.5

Size distribution(s)

% in class

100

50

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

OTS 30~60

500

Size(nm)

Intensity

Volume

Number

Peak Analysis by intensity

56

0.2

18.5 Peak

Area

Mean

68.4

0.7

0.5

40.5

74

24.1

83.6

0.4

0.3

25.3

82.2

563.2

479.8

102.1

0.1

3.4

16.7

1614.8

984.6

124.8

152.4

0 Peak Analysis by volume

186.2

227.5

0.5

0.1

0.1 Peak

278

3.8

0.4

0.4

73

33

339.6

9.6

2.4

1.2

45.4

533.3

303.7

414.9

15.4

11

3.2

53.6

1218.9

596.8

506.8

18.6

16.8

619.2

16.8

11.2

756.4

11.3

6.2

924.1

5.6

12.3

0.4 Peak

1129

2.8

18.9

0.4

87.4

71.5

30.9

1379.3

10.9

0.2

11.6

493.5

247.6

1685

6.2

3.6

2058.5

4.2

3.6

2514.9

1.4

3072.4

3753.5

4585.5

5602

Area

Width

Mean

Width

1.9 Peak Analysis by number


0.4
Area

Mean

OTS 60~90

Width

Size distribution(s)

% in class

20

10

10

50 100
Diameter (nm) (x10^1)

500

OTS 60~90

Size(nm)

Intensity

Volume

Number

Peak Analysis by intensity

64

7.3

Peak

Area

Mean

Width

80.5

0.6

17.8

100

568.4

621.9

101.4

0.9

0.1

14.8

127.7

1.3

6.1

160.7

1.8

2.5

202.4

2.8

1.2

Peak

Area

Mean

Width

254.8

4.9

0.1

0.9

99.8

800.4

382.6

320.8

8.3

0.2

1.2

403.9

13.1

1.4

508.5

18.2

2.3

640.3

20.9

24.8

11.7

Peak

Area

Mean

Width

806.1

18.3

47.2

19.7

50.1

99.8

52.7

1015

8.9

23.7

9.8

49.9

739.9

405.8

1277.9

0.1

1608.9

2025.7

2550.5

3211.2

4043.1

5090.5

6409.2

8069.6

10160.1

12792.1

Peak Analysis by volume

Peak Analysis by number

OTS 90~120

% in class

Size distribution(s)

20

10

10

50 100
500 1000
Diameter (nm) (x10^1)

OTS 90~120

whetted
times

(degree)

Average

Space

100105

100~105

Five

144.80 142.47 147.20 150.34 150.09 137.59 139.23 139.21 146.14 150.65

147.772

Ten

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)

frame

(c)

frame
(d)

(mm)

frame

pixels

(a)(b)(c)
(d)frame

(a)

(b)

frame

(c)

frame
(d)

(mm)

frame

pixels

(a)(b)(c)
(d)frame

(a)

(b)

(a)

(b)

frame

(c)

frame
(d)

(mm)

frame

(c)

frame
(d)

(mm)

frame

pixels

(a)(b)(c)
(d)frame

Speed(rpm)

A(degree)

Average

space

100~105

100~105

1012

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

------

150.7275

4528

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

159

161

158.5

160.5

158

160

157.5

159.5

157

159

156.5

158.5
0

0.5

1.5

400

1.5

300

200

0.5

100

-0.5

0.5

1.5

-100

0.5

1.5

200

400

600

800

157.61159.79(a)(b)
(c)(d)frame

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