In this study, we explored the relationships among employees experience of volunteer, subjective well-being and Interpersonal Citizenship Behavior, and to analyze the moderating effect of work-family conflict. Analysis of 224 valid questionnaires were obtained the following findings: First, the volunteers experienced employees, their subjective well-being and Interpersonal Citizenship Behavior were higher than non-volunteers experience; Second, employees work-family conflict and subjective well-being has a negative relations; Finally, the employees of the low work-family conflict, their volunteer experience will help improve Interpersonal Citizenship Behavior, but a high work-family conflict, volunteer experiences no help to improve Interpersonal Citizenship Behavior. We discuss theoretical and practical implications about research findings.