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The learning process must be based on the aim to facilitate the formation of college students metacognitive skills so that the learning process for conceptual change can occur. The aim of the study was describing the validation of Problem-Solving based teaching materials for the exploration of conceptual change and metacognitive skills theoretically and empirically. Research and Development (R & D) design was utilized in the research method. This study involved three experts for theoretical validation and 31 college students for empirical validation. The instrument used for this study was the validation sheet and questionnaire of college students- perception of problem-solving based teaching materials. The research obtained findings: (a) Theoretical validity from the expert has met the valid and very valid include the construct validities categories and the content validities as well as reliable, (b) empirical validity of the college students perception of the teaching materials based problem-solving includes the construct validities and content validities, all of them have valid and very valid categories. From this study, it can be concluded that the Problem-Solving based teaching materials were feasible and suitable for use on the exploration of conceptual change and metacognitive skills.