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Crystal structure transformation and step-by-step thermal decomposition behavior of dihydroxylammonium 5,5 '-bistetrazole-1,1 '-diolate

机译：晶体结构转化和二羟基铵5,5'-苄烷唑-1,1' - 二醇的逐步热分解行为

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摘要

The crystal structure transformation and step-by-step thermal decomposition behavior of dihydroxylammonium 5,5'-bistetrazole-1,10-diolate (TKX-50) under thermal stimulation were studied and the whole process included thermal expansion, primary decomposition and secondary decomposition. The thermal expansion and primary decomposition of TKX-50 were studied using in situ powder X-ray diffraction (in situ XRD) together with Rietveld refinement, by which the crystal structure transformation process can be accurately traced. The results showed that the thermal expansion of TKX-50 was anisotropic. In particular, the a-axis exhibited a negative thermal expansion (NTE) that may be attributed to the distortion of the six-membered ring, which results in H-transfer between the cation and dianion. The crystal structure of the intermediate product after primary decomposition was also obtained. The secondary decomposition process was analysed using thermogravimetric-differential scanning calorimetry (TG-DSC) due to the safety risk of TKX-50 analyzed by in situ XRD. The crystal structure transformation process from TKX-50 to the intermediate product under heat stimulation was deduced. Meanwhile, the morphological change of the whole process was obtained using hot stage microscopy (HSM). Combined with TG-FTIR technology, the gaseous decomposition products at each step were analysed and the thermal decomposition mechanism of TKX-50 was proposed. This study further reveals the thermal decomposition behavior of TKX-50 and is helpful for better understanding the thermal decomposition mechanism.
机译：进行了研究dihydroxylammonium下热刺激-联四唑·-1,10-二醇盐5,5'-（TKX-50）的晶体结构转变和一步一步的热分解行为，整个过程包括热膨胀，初级分解和二次分解。使用原位粉末X射线衍射（原位XRD）连同Rietveld修正，通过该晶体结构转变过程可以精确地跟踪TKX-50的热膨胀和初级分解进行了研究。结果表明，TKX-50的热膨胀是各向异性的。特别地，一个轴发挥可以归因于六元环的失真，这导致阳离子和二价阴离子之间H-传送的负热膨胀（NTE）。还获得初级分解后的中间产物的晶体结构。利用热重 - 差示扫描量热法（TG-DSC）的二次分解过程进行了分析，由于通过原位X射线衍射分析TKX-50的安全性风险。从TKX-50的晶体结构变换处理热刺激下的中间产物推导。同时，使用热台显微术（HSM），得到的全过程的形态变化。用TG-FTIR技术相结合，在每个步骤中的气态分解产物进行分析并提出TKX-50的热分解机制。本研究进一步揭示了TKX-50的热分解行为，是为了更好地理解热分解机制很有帮助。

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  • 来源
    《RSC Advances》 |2017年第77期|共9页
  • 作者

    Jia Jianhui; Liu Yu; Huang Shiliang; Xu Jinjiang; Li Shichun; Zhang Haobin; Cao Xiong;

  • 作者单位

    North Univ China Sch Environm &

    Safety Engn Taiyuan 030051 Shanxi Peoples R China;

    China Acad Engn Phys Inst Chem Mat Mianyang 621900 Peoples R China;

    China Acad Engn Phys Inst Chem Mat Mianyang 621900 Peoples R China;

    China Acad Engn Phys Inst Chem Mat Mianyang 621900 Peoples R China;

    China Acad Engn Phys Inst Chem Mat Mianyang 621900 Peoples R China;

    China Acad Engn Phys Inst Chem Mat Mianyang 621900 Peoples R China;

    North Univ China Sch Environm &

    Safety Engn Taiyuan 030051 Shanxi Peoples R China;

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