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A composite fiber nitrocellulose/glycidyl azide polymer/nanometer 1,3,5‑triamino‑2,4,6‑trinitrobenzene(NC/GAP/nano‑TATB) with three‑dimensional structure was prepared by electrospinning method. Differential scanning calorimeter(DSC) and online thermal‑infrared spectrometry(TG‑IR) measurement were conducted to probe the low temperature thermochemical properties of the composite fiber. Result indicates that there is only one exothermic peak existing in its DSC curve, which means that NC, GAP, and nano‑TATB decomposed simultaneously rather than decomposed individually. The activation energy (Ea) of NC/GAP/nano‑TATB (208.1 kJ·mol-1) is lower than nano‑TATB (228.9 kJ·mol-1), and the rate constant (k) of NC/GAP/nano‑TATB (1.70 s-1) is higher than nano‑TATB (0.92 s-1). The composite fiber is easier to be activated and will decompose faster than nano‑TATB. The main products for thermal decomposition of NC/GAP/nano‑TATB include CO2, N2O, NO, CO, NO2 and H2O, meanwhile, fragments like ─CH─, ─CH2O, and C─O─C were also detected. Moreover, the energetic performance and sensitivity of the composite fiber have been detailedly evaluated and compared with that of NC/GAP and nano‑TATB. Combustion temperature (Tc) of NC/GAP/nano‑TATB is up to 1583 ℃ and the addition of nano‑TATB is favorable to the reduction of impact sensitivity.“,”采用静电纺丝法制备了具有三维网络结构的硝化纤维素/聚叠氮缩水甘油醚/三氨基三硝基苯(NC/GAP/nano‑TATB)复合纤维。采用差示扫描量热法(DSC)和热红外法(TG‑IR)对复合纤维的低温热化学性能进行了研究。结果显示，每条曲线上只有一个放热峰，，NC、GAP和nano‑TATB同时分解，而非单独分解。NC/GAP/nano‑TATB(208.1 kJ·mol-1)的活化能(Ea)低于nano‑TATB (228.9 kJ·mol-1)，NC/GAP/nano‑TATB (1.70 s-1)的速率常数(k)高于nano‑TATB(0.92 s-1)。复合纤维比纳米TATB更容易被活化，分解速度更快。NC/GAP/nano‑TATB热分解的主要产物为CO2、N2O、NO、CO、NO2、H2O，同时检测到─CH─、─CH2O、─C─O─C─片段。对比了复合纤维和NC/GAP和nano‑TATB的能量和敏感性。NC/GAP/nano‑TATB的燃烧室温度(Tc)高达1583℃，纳米TATB的加入有利于降低冲击敏感度。