ESA instrumentation setup TINOX Technical Service
Titanium dioxide can be utilized in various applications such as pigment base in paints, coatings, plastics and laminates. During both, the production process at the TiO2 producer and the manufacturing process of paints, coatings and composite materials, avoiding the coagulation and agglomeration of the TiO2 dispersion is important. Surface chemistry of the TiO2 dispersion can be controlled during the measurement of Electrokinetic Sonic Amplitude (ESA) by regulating the pH value e.g. for avoiding flocculation of dispersion. This means: the zeta potential of the dispersion should not be or close to zero. Zeta potential is a dimension of the effective surface charge of particles and the interaction between the particles with ions in solution and particles among each other. Characterising the absolute surface charge (in an aqueous dispersion) of the TiO2pigment, negative or positive in the unit [mV], gives a decisive parameter for an ultimate application of the product. The zeta potential depends on the kind of solvent, the nature and amount of the ions in solution (specific conductivity), and the pH value. It is also the main factor determining the stability of the whole dispersion.
The applied materials and measurement techniques are listed as follows. The measurement of the TiO2 dispersion was carried out at TINOX CHEMIE GMBH Düsseldorf. Five TiO2-pigments grades with different post-treatments in aqueous dispersion were tested.
Aqueous TiO2 dispersion 10% wt, 0.1 M HCl and 0.1 M NaOH (p. A.)
ESA measuring system with programmable titrator. Hyper sensitive probe with 500kHz measuring frequency
ESA measuring cell, pH sensor, conductivity and temperature sensor, adjustable stirrer to prevent precipitation during measurement
Measuring the Electrokinetic Sonic Amplitude ESA delivers a clear distinction of the electrostatic properties of various grades of TiO2 in aqueous dispersions.
The measurement results in figure above shows that different TiO2 grades differ in isoelectric point IEP and with regard to their zeta potential significantly from each other. Handling TiO2 dispersions in a range beyond the IEP avoids any kind of flocculation. Choosing pH values in an extreme area could be a disadvantage regarding both, the electrostatic property of the pigment surface and the ionic charge in the dispersion. With increasing ratio of Al2O3/SiO2 posttreatment of TiO2 base material the isoelectric point IEP shifts to alkaline pH. With increasing SiO2 posttreatment the positive surface charge decrease.
Experienced users and specialists know well that, for example, Al2O3 and SiO2 compounds have been used for decades in TiO2 posttreatment processes. However, improvements have been made repeatedly in the type of post-treatment. E.g. in the targeted control of shell texture (dense, continuous), structure (heterogeneous, homogeneous), layer thickness, et cetera.
The added value of current study lies in the method. TINOX Technical-Service uses measurement systems for highly concentrated technical formulations. During technical process dispersions are often found to be highly concentrated, muddy, colored, tempered, or electrostatically affected by additive formulations. Sedimentation is often inhibited by powerful agitators in large scale treatment containers. All these process conditions have been reported in the stability analysis showed in this article.
Surface chemistry of TiO2 dispersion can be controlled during the measurement in a simultaneously and recording manner by regulating the pH value, adding additives and stirring conditions like in process. Therefore ESA-technique is a valuable tool for TINOX TiO2 product intensivication.
Electrokinetic Sonic Amplitude (ESA) measurements of highly concentrated dispersions are special measurement methods. The ESA technique has been developed for a whole range of different applications.
During the technical process dispersions are often found to be highly concentrated, muddy, coloured, tempered, or electrostatically affected by additive formulations. Sedimentation is often inhibited by powerful agitators in the large scale treatment containers. All these process conditions mentioned before can be involved in the stability analysis via ESA. The results of the analysed highly concentrated samples correlate directly with the electro kinetic properties of the dispersed particle in both, the raw material and the final product.
The ESA method is an electro acoustic measuring technique for characterising the charge stability of particles in dispersion. An oscillating voltage, generated by an AC source, is applied to a suspension, dispersion, or emulsion. Charged particles in dispersion vibrate with the frequency of an applied electric field. One or more frequencies can be applied. Sound waves are generated by the particle oscillation at these frequencies. The amplitude of these sound waves gives the Electrokinetic Sonic Amplitude (ESA). The ESA signal is proportional to the dynamic mobility of the particle which in turn is proportional to the zeta potential of the particles in dispersion. For the use of this effect a certain density difference between the dispersion medium and the particle is required. For evaluable signals the density difference has to be at least 0.2 g/cm3. The measurements can be carried out with dispersions in aqueous- and alcoholic solutions and paste-like formulations.