Near infrared (NIR) spectroscope and X-ray diffractometry have been used for rapid prediction of the microfibril angle (MFA) which is one of the important factors affecting wood properties. Wood property evaluation in breeding and resource evaluation requires effective and rapid analysis methods for thousands of samples. In the experiment, all samples from increment cores with moisture content of 60% to 150% were used for measuring MFA by X-ray scanning diffractometry. Then, a partial least squares regression (PLS) model was built based on NIR data and MFA measured. As a result, a strong linear relationship was found between NIR spectroscope fitted and X-ray measured with coefficient of calibration 0.95 and prediction model rate 0.88. NIR estimating is in consist with X-ray determining closely, which indicates that NIR spectroscopy can be successfully used to estimate MFA of increment cores of Chinese fir. Near infrared (NIR) spectroscope and X-ray diffractometry have been used for rapid prediction of the microfibril angle (MFA) which is one of the important factors affecting wood properties. Wood property evaluation in breeding and resource evaluation requires effective and rapid analysis methods for Thousands of samples. In the experiment, all samples from increment cores with moisture content of 60% to 150% were used for measuring MFA by X-ray scanning diffractometry. Then, a partial least squares regression (PLS) model was built on NIR As a result, a strong linear relationship was found between NIR spectroscope fitted and X-ray measured with coefficient of calibration 0.95 and prediction model rate 0.88. NIR estimation is in consist with X-ray determines closely, which indicates that NIR spectroscopy can be successfully used to estimate MFA of increment cores of Chinese fir.