A "Sandwich" type of neutron shielding composite reinforced by carbon fiber was currently studied in view of the rapidly growing need of nuclear protective materials. Comparison to Scanning Electron Microscopy (SEM) analysis of a variety of carbon fiber surface treatment, a new technology, named acetone-resin ultrasonic pretreatment was better to ensure that the carbon fiber and the resin glue were solidified effectively by diffusion as a whole, and also worked out the traditional problem about full impregnation of carbon fiber. Meanwhile, differential scanning calorimetry (DSC) and thermogravimetic analysis (TGA) of the composite filled with boron carbide were observed. The conclusion was that the effect of the acid anhydride type curing agent (B-570) was better than the polyamide type (TY-203) in the field of heat resistance, and the carbon fiber was helpful to improve the thermal stability of the composite when the adding content was 28.2%. In addition, the "Sandwich" type of neutron shielding composite was prepared for the tensile performance test. Compared to the boron carbide particles added directly into the composite, it has a huge performance improvement in the mechanical properties when the content of boron carbide filled with 20%, meanwhile it significantly upgrade the neutron shielding performance with spraying with 0.4 mm. Crown Copyright (C) 2013 Published by Elsevier B.V. All rights reserved.