Critical behavior of gelation probed by the dynamics of latex spheres G. C. Fadda and D. Lairez* Laboratoire Le ´on Brillouin, CEA-CNRS, CEA/Saclay, 91191 Gif-sur-Yvette cedex, France J. Pelta ERRMECE, Universite ´ de Cergy-Pontoise, 95302 Cergy-Pontoise cedex, France Received 21 November 2000; published 23 May 2001 We report a quasielastic light scattering study of the dynamics of large latex probe particles ( R =225 nm) in gelatin solution undergoing gelation. We show that by focusing on the short-time and long-time behavior of the autocorrelation function, it is possible to simply interpret out data in terms of the divergence of the viscosity and emergence of the shear elastic modulus near the gel point. Our crude analysis allows us to grasp the critical behavior of gelation and to obtain the two critical exponents of the transport properties. DOI: 10.1103/PhysRevE.63.061405 PACS numbers: 82.70.Gg, 47.50.+d, 83.10.Pp I. INTRODUCTION The use of spherical probe particles to study viscoelastic properties of polymer solutions has been suggested for a long time 1,2. The basic idea is that in a semidilute solution of linear chains, sufficiently small particles freely move in the solution whereas larger particles would be trapped in the polymer transient network. Thus, the dynamics of probe par- ticles is expected to be governed either by the solvent vis- cosity, or by the macroscopic viscosity, depending on their size R compared to the correlation length T of concentration fluctuations. A suitable technique to study such dynamics of probe particles is quasielastic light scattering, which has been extensively used on various physicochemical systems. According to the wide literature on this subject it appears that some complications may occur. For instance, a complex signal is sometime observed due to the contribution of the matrix and of the probe particles to the total light scattered intensity 3. In addition, strong interactions between poly- mers in solution and particles, are sometimes reported which may cause adsorption of chains on the particles and particles aggregation 4,5. However, it has been shown that, as soon as these complications are avoided, the basic idea is well founded. In particular for R / 1, the long-time dynamics of probe particles is slowed down and governed by the macro- scopic viscosity 6–9rather than the solvent viscosity. Compared to rheology, the study of thermal fluctuations of concentration of probe particles for the investigation of weak structures is very attractive 10, because it guarantees the structure integrity. In particular, the use of probe particles for the study of gelation looks very tempting and has been already reported. Gelation 11is a critical phenomenon of connectivity occurring when molecules randomly connect to- gether leading at the gel point to a giant cluster: the gel. The understanding of quasielastic light scattering results obtained on gelling systems is much less clear as those obtained in semidilute solutions. On the one hand, gelation essentially produces a wide polydisperse population of clusters, which is responsible for complex relation processes. Therefore the analysis of the dynamical structure factor of probe particles in terms of time distribution is not quite obvious. On the other hand, above the gel point, fluctuations tend to be frozen at long-time because the solution becomes solid. This ap- pears through a decrease in amplitude of the scattered inten- sity fluctuations. The most often used approach to account for this behavior invokes a loss of ergodicity 12–14. The physical meaning of this approach consists in splitting the probe particles population into two parts: the first being free to diffuse in the medium, the second being trapped in the network and motionless. The scattered intensity has thus two contributions: a time fluctuating or quasielastic part and a constant or elastic part. Quasielastic light scattering tech- nique consists in measuring the autocorrelation function of the scattered intensity. Consequently it also shows the two contributions. The first corresponds to the autocorrelation of the fluctuating part of the scattered intensity and the second to the correlation of this fluctuating part with the elastic scat- tering that acts as a local oscillator signal. In terms of the light scattering language, this amounts to mix a self-beating and a heterodyne contribution. Such an analysis calls for two remarks. First, the splitting of the probe particles population into two parts seems somewhat arbitrary and unsatisfactory. Second, above the gel point as fluctuations become more and more frozen the increasing heterodyne part leads at short time to a slowed dynamics while quite the opposite is experi- mentally observed 15. In this paper, we present an analysis of quasielastic light scattering results from probe particles during gelation of a gelatin solution. We deliberately consider the simplest case, that is: 1very large spherical and monodisperse latex par- ticles radius R =225 nm; 2negligible thermodynamic in- teractions of probe particles between them or with the ma- trix; 3a negligible contribution of the matrix to the scattered intensity; 4measurements performed at qR =1 with R / T 1. We show that, neglecting the nonergodicity and focusing on the short-time and long-time behaviors of the measured relaxation function, it is possible to simply interpret our data in terms of the divergence of the viscosity and emergence of a shear elastic modulus near the gel point. Our crude analysis allows us to grasp the critical behavior of gelation and to obtain the two critical exponents of the trans- port properties. *Author to whom correspondence should be addressed. PHYSICAL REVIEW E, VOLUME 63, 061405 1063-651X/2001/636/0614059/$20.00 ©2001 The American Physical Society 63 061405-1