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Adhesion forces between TiO2 nanoparticles

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Force measurements <strong>between</strong> TiO 2<br />

<strong>nanoparticles</strong> forming agglomerates<br />

Samir Salameh<br />

Lucio Colombi Ciacchi<br />

Lutz Mädler<br />

Fachbereich Produktionstechnik, Universität Bremen<br />

Paolo Facci<br />

S3 national center of CNR-INFM, Modena<br />

Samir Salameh<br />

1


Outline<br />

Nanoparticle synthesize and AFM implementation<br />

Results of adhesion force <strong>between</strong> pure TiO 2 aggregates<br />

Results on modeling<br />

Conclusion<br />

Samir Salameh<br />

2


Particle synthesis with flame spray<br />

pyrolysis<br />

2 cm<br />

Mädler et al. (2002) Jou. of mat. Res.,<br />

17, 1356-1362<br />

Samir Salameh<br />

3


Filmstructure off TiO 2 aggregates on<br />

Mica<br />

20 µm 500 nm<br />

Samir Salameh<br />

4


Idealized force measurements on<br />

<strong>nanoparticles</strong><br />

Butt et al. (2005) Surface Science Reports 59 1-152<br />

Samir Salameh<br />

5


<strong>Adhesion</strong> force <strong>between</strong> TiO 2<br />

nanoparticle aggregates<br />

3<br />

2<br />

1<br />

Force in nN<br />

0<br />

-1<br />

-2<br />

-3<br />

-4<br />

-5<br />

retraction<br />

approach<br />

0,0 0,5 1,0 1,5 2,0 2,5 3,0 3,5<br />

seperation in µm<br />

Samir Salameh<br />

6


<strong>Adhesion</strong> force <strong>between</strong> TiO 2<br />

nanoparticle aggregates<br />

3<br />

2<br />

1<br />

Force in nN<br />

0<br />

-1<br />

-2<br />

-3<br />

-4<br />

-5<br />

retraction<br />

approach<br />

0,0 0,5 1,0 1,5 2,0 2,5 3,0 3,5<br />

seperation in µm<br />

Samir Salameh<br />

7


<strong>Adhesion</strong> force <strong>between</strong> TiO 2<br />

nanoparticle aggregates<br />

3<br />

2<br />

1<br />

Force in nN<br />

0<br />

-1<br />

-2<br />

-3<br />

-4<br />

-5<br />

retraction<br />

approach<br />

0,0 0,5 1,0 1,5 2,0 2,5 3,0 3,5<br />

seperation in µm<br />

Samir Salameh<br />

8


<strong>Adhesion</strong> force <strong>between</strong> TiO 2<br />

nanoparticle aggregates<br />

3<br />

2<br />

1<br />

Force in nN<br />

0<br />

-1<br />

-2<br />

-3<br />

-4<br />

-5<br />

retraction<br />

approach<br />

0,0 0,5 1,0 1,5 2,0 2,5 3,0 3,5<br />

seperation in µm<br />

Samir Salameh<br />

9


Distribution of the adhesion force with R<br />

x̄ = 3,6<br />

Standard dev.= 1,97<br />

n = 1025<br />

Samir Salameh<br />

10


Mean and standard deviation increase<br />

for the last set of measurements<br />

6<br />

mean value of force measurements<br />

5<br />

4<br />

Force in nN<br />

3<br />

2<br />

1<br />

0<br />

0-200 200-400 400-600 600-800 800-1000<br />

set of 200 measurements<br />

Samir Salameh<br />

11


Particle number increase with<br />

increasing number of measurements<br />

n < 10 n > 50<br />

1 µm<br />

2 µm<br />

Samir Salameh<br />

12


Minimum force for breaking chains<br />

Rong, Mädler et al. (2004) Nanoletters,<br />

4, 2287-2292<br />

Samir Salameh<br />

13


MD modelling of TiO 2 particle seperation<br />

Force in nN<br />

Distance in nm<br />

Samir Salameh<br />

14


Iron in TiO 2 lattice changes<br />

surface properties<br />

40<br />

30<br />

TiO 2<br />

TiO 2<br />

10% Fe<br />

20<br />

10<br />

Zeta-Potential<br />

0<br />

-10<br />

-20<br />

-30<br />

-40<br />

Teoh et al. (2007) Catalysis today,<br />

120, 203-213<br />

3 4 5 6 7 8 9 10 11<br />

PH-Wert<br />

Samir Salameh<br />

15


Iron atoms prefer the outer levels<br />

Samir Salameh<br />

16


conclusion<br />

Method for analyzing adhesion force <strong>between</strong><br />

<strong>nanoparticles</strong><br />

Particles migrate from layer to the AFM tip<br />

Experimental data and Modelling fits well<br />

Samir Salameh<br />

17


outlook<br />

Statistical analysis of TiO 2 10% Fe force measurements<br />

Validation of resultes with a rutile single crystal in<br />

mikrometer size<br />

Perform fishing experiments on TiO 2 monolayers with<br />

different particle sizes<br />

Samir Salameh<br />

18


Force measurements <strong>between</strong> TiO 2<br />

<strong>nanoparticles</strong> forming agglomerates<br />

Samir Salameh<br />

Lucio Colombi Ciacchi<br />

Lutz Mädler<br />

Fachbereich Produktionstechnik, Universität Bremen<br />

Paolo Facci<br />

S3 national center of CNR-INFM, Modena<br />

Samir Salameh<br />

19


Back up<br />

http://www.nyah.ch/fun/archiv/backup.jpg<br />

Samir Salameh<br />

20


SEM picture from Si 3 N 4 tip<br />

Samir Salameh<br />

Samir Salameh<br />

21<br />

21


AFM force curve <strong>between</strong> TiO 2<br />

<strong>nanoparticles</strong><br />

3<br />

2<br />

1<br />

0<br />

Force in nN<br />

-1<br />

-2<br />

-3<br />

-4<br />

-5<br />

-6<br />

-7<br />

-8<br />

-9<br />

retraction<br />

approach<br />

-10<br />

0,0 0,5 1,0 1,5 2,0 2,5 3,0 3,5<br />

seperation in µm<br />

Samir Salameh<br />

22


Minima to maxima analysis of<br />

force curves<br />

Samir Salameh<br />

23


EFTEM analysis of TiO 2 10% Fe<br />

Iron TiO 2<br />

Samir Salameh<br />

24


EDX analysis of TiO 2 10%Fe<br />

Samir Salameh<br />

Samir Salameh<br />

25<br />

25


Primary particles size of TiO 2 and Fe/TiO 2<br />

26<br />

26<br />

24<br />

TiO 2<br />

10% Fe<br />

TiO 2<br />

Partikelgröße d BET<br />

in nm<br />

22<br />

20<br />

18<br />

16<br />

14<br />

12<br />

10<br />

8<br />

1.0 1.5 2.0 2.5<br />

Verhältnis Durchflussrate Präkursor/Sauerstoffstrom<br />

Samir Salameh<br />

Samir Salameh<br />

26

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