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The effect of high power ultrasound on an aqueous suspension of graphite

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HAL Id: in2p3-00433527

http://hal.in2p3.fr/in2p3-00433527

Submitted on 19 Nov 2009

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The effect of high power ultrasound on an aqueous

suspension of graphite

Fabrice Guittonneau, Abdesselam Abdelouas, Bernd Grambow, Sandrine

Huclier

To cite this version:

Fabrice Guittonneau, Abdesselam Abdelouas, Bernd Grambow, Sandrine Huclier. The effect of high power ultrasound on an aqueous suspension of graphite. Ultrasonics Sonochemistry, Elsevier, 2010, 17, pp.391-398. �10.1016/j.ultsonch.2009.08.011�. �in2p3-00433527�

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Figure 1: Decrease of the particle size by ultrasonic treatment on graphite powder

0 1 2 3 4 5 6 7 0 10 20 30 40 50 60 70 80 90 100 Particle diameter (µm) % V o l 10W/cm² 25min 10W/cm² 50min 10W/cm² 100min 20W/cm² 25min 20W/cm² 50min 20W/cm² 100min 30W/cm² 25min 30W/cm² 50min 30W/cm² 100min Reference

(3)

Figure 2: Particle size vs. energy density

0 10 20 30 40 50 60 70 80 0 1 2 3 4 5 6 7 8 9 Energy density (105 J.g-1) Par ticule size x 16 , x 50 et x84 (µm) 10 W/cm² 20 W/cm² 30 W/cm² x16 x50 x84

(4)

Figure 3: HRTEM photographs showing the graphite crystallites before and after

ultrasound treatment (with probe A)

Sample not

treated

Sample

treated at

20 W/cm²

Sample

treated at

30 W/cm²

A

B

C

D

E

F

Turn-arounds

Sheets

Loops

Faggot

s

(5)

Figure 4: pH and H

2

O

2

curves during graphite sonolysis (powder A, probe A, m = 1 g,

V = 1 L, T = 20 °C, Argon satured, I = 20 W/cm²)

3.5 4.0 4.5 5.0 5.5 6.0 0 50 100 150 200 250 300 Time (min) pH 0 20 40 60 80 100 120 140 160 nH2 O 2 (µ mo l) pH with graphite pH without graphite H2O2 with graphite H2O2 without graphite

0,85 µmol/min 1,58 µmol/min

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Figure 5: Mass spectrum in the range [68-102] in APCI+ Fourier Transform mode

eau sonifiee HR #10 RT:0.09 AV:1 NL:3.41E6

T:FTMS + p APCI corona Full ms [50.00-214.00]

70 75 80 85 90 95 100 m/z 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 Relat iv e A b und a nc e 95.04935 C6H7O 77.03879 C6H5 75.02630 C6H3 81.07011 C6H9 96.05269 C H8O3N2 73.04704 C H5N4 78.04214 C H6O2N2 93.03688 C6H5O 91.05448 C7H7 99.08067 C6H11O 69.07009 C5H9 83.08575 C6H11 87.04430 C4H7O2 72.08102 C4H10N C3H9Si 79.05447 C6H7

eau sonifiee HR #10 RT:0.09 AV:1 NL:3.41E6

T:FTMS + p APCI corona Full ms [50.00-214.00]

70 75 80 85 90 95 100 m/z 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 Relat iv e A b und a nc e 95.04935 C6H7O 77.03879 C6H5 75.02630 C6H3 81.07011 C6H9 96.05269 C H8O3N2 73.04704 C H5N4 78.04214 C H6O2N2 93.03688 C6H5O 91.05448 C7H7 99.08067 C6H11O 69.07009 C5H9 83.08575 C6H11 87.04430 C4H7O2 72.08102 C4H10N C3H9Si 79.05447 C6H7

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Figure 6: Scheme of the graphite degradation by ultrasound treatment in water

12.5 mm 48 m m )

)

)

Compact Grains 10 µm -1 mm )

)

)

10 nm - 1 µm Cristallites )

)

)

Fragments 1 Å - 100 nm Grafted damaged sheets )

)

)

H· HO· )

)

)

H· HO· Aromatic compounds )

)

)

H· HO· Acids, CO2 a few nm a few Å

Figure

Figure 1: Decrease of the particle size by ultrasonic treatment on graphite powder  01234567 0 10 20 30 40 50 60 70 80 90 100 Particle diameter (µm)% Vol 10W/cm² 25min10W/cm² 50min 10W/cm² 100min20W/cm² 25min20W/cm² 50min20W/cm² 100min30W/cm² 25min30W/cm²
Figure 2: Particle size vs. energy density  0 1020304050607080 0 1 2 3 4 5 6 7 8 9 Energy density (10 5  J.g -1 )Particule size x16, x50 et x84 (µm) 10 W/cm²20 W/cm²30 W/cm²x16x50x84
Figure 3: HRTEM photographs showing the graphite crystallites before and after  ultrasound treatment (with probe A)
Figure 4: pH and H 2 O 2  curves during graphite sonolysis (powder A, probe A, m = 1 g,  V = 1 L, T = 20 °C, Argon satured, I = 20 W/cm²)  3.54.04.55.05.56.0 0 50 100 150 200 250 300 Time (min)pH 0 20406080 100120140160 n H2O2 (µmol)pH with graphitepH with
+3

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