# Investigation of the growth of nanoparticles with controlled size and controlled surface chemistry, which will be used as nanofillers in polymers

Sakina Mefath, Fahmi Bedoui, Isabelle Lisiecki, Djimédo Kondo, Anh-Tu Ngo

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Sakina Mefath, Fahmi Bedoui, Isabelle Lisiecki, Djimédo Kondo, Anh-Tu Ngo. Investigation of the growth of nanoparticles with controlled size and controlled surface chemistry, which will be used as nanofillers in polymers. International Symposium on Polymer Nanocomposites 2022: From Elaboration to Applications (ISPn), Sep 2022, Lorient, France. hal-04021776

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Submitted on 9 Mar 2023

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# Investigation of the growth of nanoparticles with controlled size and controlled surface chemistry, which will be used as nanofillers in polymers

MEFTAH Sakina¹,² – BEDOUI Fahmi¹ – KONDO Djimédo³ – NGO Anh-Tu² – LISIECKI Isabelle²

Laboratoire Roberval UTC Compiègne¹ - Laboratoire Monaris Sorbonne Université² - Institut d'Alembert Sorbonne Université³

sakina.meftah@utc.fr

## Context

To Investigate the effects of size, surface chemistry and morphology of iron oxide nanofillers on the mechanical and thermal properties of nanoreinforced polymers:

1. Ligand-coated maghemite ($\gamma$-Fe$_2$O$_3$) nanoparticles are synthesized by the thermal decomposition of an organometallic precursor.

<figure><img src="image_2.png" /></figure>

2. Growth mechanisms are revealed by studying the effect of each key parameter (mentioned in the next section) on the nanoparticle characteristics (size, surface chemistry, morphology).

3. Key parameter effects are exploited to control the characteristics of the nanoparticles to be incorporated. Envisaged characteristics: see the scheme

## Synthesis of ligand-coated $\gamma$-Fe$_2$O$_3$ nanoparticles

Thermal decomposition process (under reflux)

<figure><img src="image_3.png" /></figure>

J. Phys. Chem. C 2014, 118, 3795–3810

<figure><img src="image_4.png" /></figure>

## Key parameters for controlling nanoparticles growth

<figure><img src="image_5.png" /></figure>

### Water trace

Solvent : Dioctyl ether

Ligand : Oleic acid

Dehydration condition

<figure><img src="image_6.png" /></figure>

The wetter the precursor, the smaller the NPs

<figure><img src="image_7.png" /></figure>

### Reflux temperature

Ligand : Oleic acid

<figure><img src="image_8.png" /></figure>

The trend direction may depend on the nature of the solvent (polar, alkene...etc). Study in progress

Reflux temperature (defined by the solvent boiling point) varies the size of the nanoparticles

<figure><img src="image_9.png" /></figure>

### Reflux time

<figure><img src="image_10.png" /></figure>

Solvent : Hexadecene

Ligand : Oleic acid

<figure><img src="image_11.png" /></figure>

### Precursor impurities

Synthesis of the precursor

<figure><img src="image_12.png" /></figure>

Microanalysis of the precursor used (% atomic)

<table><tr><td>%Fe</td><td>25</td><td>43</td><td>100</td></tr><tr><td>%Na</td><td>48</td><td>54</td><td>0</td></tr><tr><td>%Cl</td><td>27</td><td>3</td><td>0</td></tr></table>

Resulting morphologies

<figure><img src="image_13.png" /></figure>

All scale bars are at 50nm

<figure><img src="image_14.png" /></figure>

Solvent : Dioctyl ether

Ligand : Oleic acid

Poisoning the surface with different agents varies the growth rates on low index planes such as {111}, {110} and {100}.

<figure><img src="image_15.png" /></figure>

## Conclusion

<figure><img src="image_16.png" /></figure>

* Series of experiments are conducted to understand the growth mechanism of iron oxide nanoparticles synthesised by thermal decomposition of an organometallic precursor.

<figure><img src="image_17.png" /></figure>

* The effects of trace of water, temperature & reflux time, impurities in the precursor were observed.

* The understanding of the growth mechanism of the nanoparticles will be extended by studying the other key parameters mentioned in the "synthesis" section, and will be supported by a theoretical study on the solubility of the synthesis reagents.

* The study of control parameters will be explored to produce nanoparticles with controlled size, surface chemistry and morphology with low size dispersion to serve as nanofillers for a polymer matrix.

* The incorporation of nanoparticles into a polymer will reveal the evolution of the mechanical and thermal properties of the nanocomposite according to the characteristics of the inserted nanoparticles.

<figure><img src="image_18.png" /></figure>

Institut de science des matériaux

ALLIANCE SORBONNE UNIVERSITÉ