Sixbinary graft copolymers were synthesized, and their graft segregationin bulk was investigated. The copolymers were prepared by a one-potmethod involving the quantitative grafting of alkyne-end-functionalizedpoly(n-butyl acrylate) (PBA-CCH) and poly(2-cinnamoyloxyethylmethacrylate) (PCEMA-CCH) onto poly(3-azide-2-hydroxypropylmethacrylate) (P(GMA-N3)) via click chemistry. Of thesecopolymers, three had a total PBA and PCEMA molar grafting density gof ∼20%, and their PBA volume fractions VBamong PBA and PCEMA varied between 28% and57%. VBwas constant at ∼57%, while gvaried between 9.8% and 29.5% for the other three samples.Bulk films were obtained by slowly evaporating the solvent from castsolutions of these copolymers. These films were then annealed abovethe glass transition temperatures of PBA and PCEMA to facilitate graftsegregation. The graft segregation patterns were examined by performingtransmission electron microscopy (TEM) analysis of thin sections ofthese films. The TEM results suggested that the grafted PBA chainsformed a disordered wormlike phase in a PCEMA matrix at VB= 28%. At VB= 42% and 57%,PBA and PCEMA seemed to form alternating lamellae. In the former case,the PBA layers were thinner than the PCEMA layers, while the PBA layerswere thinner in the latter case. All three samples with VB∼ 57% probably possessed a lamellar morphology.The periodicity of the lamellae increased and the long-range orderingdeteriorated as gincreased. [ABSTRACT FROM AUTHOR]