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Polycarboxylate-type superplasticizers with different side chains and approximative degree of polymerization are synthesized. The microstructures of Polycarboxylate-type superplasticizers in water are studied by fluorescent probe technique, dynamic light scattering (DLS), transmission electron microscopy (TEM) and the self-assembly technique. The results indicate that the formation of hydrophobic microenvironment in PC solution is confirmed. The higher the ratio of long side chains of PC, the stronger the hydrophobic microenvironment formed in PC solution. The Z-Average diameters of aggregation formed in PC solution increase with the increasing of long side chains content. In addition, the size and shape of aggregation is not of uniform distribution, and the reason for this is that association interaction of hydrogen bonding occurs among PC molecules or in the interior of single PC molecule.