Bohic, Marianne (2007) Surface characterization of pigments treated by acrylic polyesters. PhD thesis Sciences et Génie des Matériaux, ENSMP - CEMEF Centre de Mise en Forme des Matériaux, ENSMP p.181.

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Abstract

This work is devoted to the surface treatment by acrylic polyesters of aluminum, iron and titanium oxides pigments and of the resulting properties. The wetting angle measurements show out hydrophobic character of pigments after their treatment. Which is the polymer fraction applied on then surface, the homogeneity of covering and the character of bonds formed by the polymer with the surface? An almost complete polymer deposit is observed by thermogravimetry and by infrared spectroscopy which can be partly removed by a solvent as a function of surface oxide. A small part of the polymer remains on alumina, a larger part on titanium oxide and is fixed on the various iron oxide pigments. Chemical bonds are observed by infrared spectroscopy thanks to quantum mechanics attributions. The surface treatment is inhomogeneous on the surface, as shown by AFM and XPS, with the aspect of small islands of polymer. AFM direct observation on alumina is decisive for the discussion. Each island results from a statistic coil conformation of the polymer chains. The inhomogeneous covering is inherent on entropic contribution on energy of polymer chains which inhibit a planar covering of molecules on the oxide surfaces. The use of shorter molecules or in-situ polymerization should be favored.

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Table of content

Sommaire

Introduction

Chapitre I Bibliographie

I.1 – Introduction.

I.2 – Méthodes expérimentales

I.3 – Pigments d’oxydes métalliques et traitements organiques

I.3.1 – Pigments d’oxydes métalliques.

I.3.2 – Physicochimie de surface

I.4 – Traitements de surface

I.4.1 – Nature et modes de traitement

I.4.2 – Isothermes d’adsorption.

I.4.3 – Adsorption ou réactivité chimique

I.4.4 – Conformation moléculaire en surface des pigments.

Chapitre II Les pigments et leur caractérisation.

II.1 – Choix des pigments et données fournisseurs

II.2 – Caractérisation des pigments

II.2.1 – Caractérisation des pigments par diffraction des rayons X.

II.2.2 – Observation des pigments par microscopies électroniques à balayage et en transmission

II.2.3 – Composition volumique des pigments

II.2.4 – Caractérisation de la surface des pigments

II.2.4.1 – Caractérisation de la surface des pigments par XPS

II.2.4.2 – Caractérisation de la surface des pigments par ToF-SIMS

II.2.5 – Caractérisation de la surface de l’alumine par AFM.

II.3 – Conclusion

Chapitre III Les polymères utilisés pour traiter les pigments

III.1 – Choix des polymères et données fournisseurs

III.2 – Caractérisation des polymères

III.2.1 – Concentration des émulsions

III.2.2 – Analyse RMN en solution

III.2.3 – Caractérisation par spectrométrie infrarouge

III.2.4 – Caractérisation par ToF-SIMS

III.2.5 – Caractérisation par XPS

III.3 – Conclusion.

Chapitre IV Le traitement de l’alumine par les polymères

IV.1 – Mode opératoire

IV.2 – Effets du traitement de surface sur les propriétés de l’oxyde d’aluminium

IV.2.1 – Effet sur la sédimentation

IV.2.2 – Effet sur la mouillabilité de la surface du pigment

IV.3 – Analyse thermogravimétrique de l’alumine traitée

IV.3.1 – Méthode expérimentale

IV.3.2 – Etude de la perte de masse des alumines

IV.3.2.1 – Alumine initiale

IV.3.2.2 – Alumine traitée

IV.3.2.3 – Analyse par chromatographie gazeuse et spectrométrie de masse

IV.3.2.4 – Alumines lavées

IV.3.2.5 – Discussion et conclusion

IV.4 – Analyse des traitements polymère par spectroscopie infrarouge

IV.4.1 – Introduction

IV.4.2 – Méthode expérimentale

IV.4.3 – Etalonnage de la méthode quantitative par analyse FTIR de l’alumine

IV.4.4 – Méthode de mesure du relargage du polymère à partir de l’alumine par des solvants

IV.5 – Étude par XPS de la chimisorption de polymères sur l’alumine lamellaire

IV.5.1 – Calcul d’une épaisseur théorique

IV.5.2 – Analyse d’une poudre par XPS

IV.5.3 – Analyse quantitative d’une poudre par XPS

IV.5.3.1 – Influence de la microtopographie de la surface

IV.5.3.2 – Calcul des concentrations atomiques

IV.5.4 – Chimisorption du polymère B sur l’alumine lamellaire

IV.5.5 – Chimisorption du polymère A sur l’alumine lamellaire

IV.5.6 – Discussion

IV.5.7 – Action d’un solvant

IV.6 – Observations par AFM

IV.7 – Conclusion

Chapitre V Étude de la chimisorption de polymères sur des oxydes de fer et de titane

V.1 – Effets du traitement de surface sur les propriétés des oxydes de fer et de titane

V.1.1 – Effet sur la sédimentation

V.1.2 – Effet sur la mouillabilité de la surface du pigment

V.2 – Analyse infrarouge du traitement d’oxydes de fer et de titane

V.3 – Modélisation quantique des spectres infrarouge des polymères chimisorbés

V.4 – Étude par XPS des polymères sur les oxydes de fer et de titane

V.5 – Discussion

Conclusion.

Références bibliographiques

Annexe 1 Microscopie électronique à balayage MEB

Annexe 2 Analyses TOF-SIMS

Annexe 3 Microscopie à force atomique AFM

Annexe 4 Diffraction des Rayons X

Annexe 5 Spectroscopie de photoélectrons XPS

Annexe 6 Spectroscopie infrarouge à Transformée de Fourie

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