Abstract
Small-angle X-ray scattering (SAXS) is an effective method to obtain microstructural information of materials. However, due to the influence of crystal surface effects, SAXS has a deviation in the characterization of the crystal microstructure. In order to solve the influence of crystal surface effect on the internal defect signal, the microstructure of Octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) crystal was characterized by soaking the sample in the matching solution. We found that the absolute scattering intensity, specific surface and volume fraction of the sample in the matching solution are significantly lower than the initial sample, which solves the influence of the crystal surface effect on the test results. Comparing the scattering results of the samples in different electron density matching solutions, it was found that the best result was obtained when using GPL-107 perfluoropolyether (PFPE) matching solution and the same law was obtained by controlling the experiment with 2,4,6,8,10,12-hexanitrohexaazaisowurtzitane (CL-20) crystal. The fitting density was calculated according to the theoretical density and void volume fraction of the sample, and the calculated results are close to the test results of Particle Density Distribution Analyzer (PDDA). Based on this paper, we provide a method to obtain the correct information of crystal microstructure.
Highlights
With the continuous requirements of industry and academia, many advanced materials with excellent properties have been developed and applied in production practice gradually [1,2,3]
The results show that the volume fraction the crystal without the addition of a matching solution
In order to obtain the true volume fraction of the crystal voids, we studied the influence of the electron density difference between the HMX crystal and the matching solution on the scattering signal
Summary
With the continuous requirements of industry and academia, many advanced materials with excellent properties have been developed and applied in production practice gradually [1,2,3]. It used an accelerated beam of electrons, which passes through a very thin specimen to enable a scientist to observe features such as structure and morphology It provides higher resolution images than SEM. SAXS has been widely used as an advanced means for obtaining specific information on the number and size distribution of internal defects of materials, such as polymer materials [4,5,6,7,8,9], nanocomposites [10,11,12] and energetic materials [13,14,15,16,17,18,19,20,21] It is still very challenging for characterizing the crystal powder accuracy by SAXS. The real scattering data of the inner structure of the explosive crystal were obtained by correcting the absolute scattering intensity of the sample and comparing the change of the specific surface and volume fraction of the voids
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