Duas amostras diferentes de partículas monodispersas de sílica de Stöber foram examinadas por microscopia eletrônica de transmissão analítica, utilizando-se diferentes tipos de imagens: campo-claro, campo escuro, imagens espectrais e mapas de distribuição elementar. As partículas (141 e 36 nm de diâmetro efetivo) contêm domínios de relação elementar O/Si e, portanto, de grau de hidratação muito variável, que coexistem com partículas medindo poucos nanômetros de diâmetro e com relação O/Si elevada, que aparecem dispersas no fundo das imagens. As imagens de campo claro e de perda de energia revelam que as partículas maiores possuem uma morfologia do tipo caroço-casca e as cascas das partículas possuem uma quantidade maior de domínios com razão O/Si maior, comparada com o interior da partícula, o que é atribuído ao acúmulo de domínios mais hidratados na casca, e também à presença de compostos de carbono, contaminantes da sílica. Por outro lado, as partículas menores (diâmetro efetivo = 36 nm) não são esféricas nem têm morfologia caroço-casca, embora também sejam formadas por domínios de composições químicas muito diferentes. Os vários mecanismos de formação de partículas apresentados na literatura são discutidos, considerando-se estes novos resultados.Two different samples of monodisperse Stöber silica particles were examined in the analytical transmission electron microscope, using different imaging modes: bright-field, dark-field, energyloss and elemental distribution maps. The particles (effective diameters = 141 and 36 nm) are formed by domains of variable O/Si ratio, which is consistent with a variable degree of hydration, and they coexist with particles with a high O/Si ratio measuring a few nanometers only, which appear dispersed in the picture background. Bright-field and energy-loss images of the larger particles show a core-and-shell morphology, and the shells have a higher amount of high-O/Si domains as well as contaminating carbon compounds. On the other hand, the smaller particles (effective diameter = 36 nm) are also formed by distinct domains, but their morphology is neither spherical or core-and-shell. The mechanisms for particle formation presented in the literature are discussed, considering the present findings.Keywords: colloidal silica, transmission electron microscopy, energy-filtered imaging, silica particle microchemistry J. Braz. Chem. Soc., Vol. 12, No. 4, 519-525, 2001. Printed in Brazil ©2001 Soc. Bras. Química 0103 -5053 $6.00+0.00
IntroductionUniform fine particles are interesting as model systems in the study of adsorption and catalysis, as well as in the study of size-dependent solid state properties such as quantum confinement 1 and superplasticity 2,3 . There have been significant achievements concerning the preparation of uniform colloid dispersions, both inorganic 4 and organic 5 . However, uniformity has often been considered only in relationship to particle size and shape, and little information is currently available concerning the uniformity of chemical composition of particl...