This work is focused on the optimization of critical process parameters for preparation of boron-containing phenolic resin (B-containing PR), including the molar ratios of formaldehyde/phenol and potassium borate/phenol, reaction time; and measurement of surface tension of B-containing PR solution and wettability between B-containing PR solution and carbon fibers. The effects of the formaldehyde/phenol and potassium borate/phenol molar ratios on the char yield of the B-containing PR was studied. The highest char yield of B-containing PR could be as high as 71% under optimal conditions (molar ratios of formaldehyde/phenol = 1.8 and potassium borate/phenol = 0.2, and reaction time = 13 h). The effect of concentration and tested temperature on the surface tension of B-containing PR solution was investigated, and the wettability between B-containing PR solution and carbon fibers was evaluated for the first time, providing useful theory and experimental data for the preparation of B-containing PR-based composites.