CN-121978284-A - Sensitivity test system and method for milligram-grade to sub-milligram-grade energetic material

CN121978284ACN 121978284 ACN121978284 ACN 121978284ACN-121978284-A

Abstract

The invention discloses a sensitivity test system and a sensitivity test method for milligram-grade to sub-milligram-grade energetic materials, and belongs to the field of material testing. The invention provides a sensitivity test system for an energetic material, which aims at solving the problems of high sample consumption and high result error rate of the existing energetic material test, and comprises a pressure loading module for applying dynamic pressure to the energetic material, a common optical path module for collecting at least two different wavelengths of light and separating the different wavelengths of light paths to different functional components in the functional component module, a functional component module for in-situ observing the structural evolution and reaction phenomena of the energetic material under pressure loading, and a synchronous control module for ensuring the time synchronism of the pressure loading module, the common optical path module and the functional component module during working. The invention realizes accurate measurement of the sensitivity of milligram or even sub-milligram energy-containing materials, has objective test results and high repeatability, and provides a powerful means for rapid safety evaluation and initiation mechanism research of novel energy-containing materials.

Inventors

SU LEI
YUAN CHAOSHENG
ZHANG JIAQING
XU JIAN
SHI FENGYUAN

Assignees

上海前瞻物质科学研究院

Dates

Publication Date: 20260505
Application Date: 20260407

Claims (10)

1. A sensitivity test system for milligram-to sub-milligram-grade energetic materials, comprising: the pressure loading module is used for applying dynamic pressure to the energetic sample; the public light path module is used for collecting at least two kinds of light with different wavelengths and separating the light paths with different wavelengths to different functional components in the functional component module; the functional component module is used for in-situ observation of structural evolution and reaction phenomena of the energetic sample under pressure loading; And the synchronous control module is used for ensuring the time synchronism of the pressure loading module, the public light path module and the functional component module during working.
2. The sensitivity test system according to claim 1, wherein the pressure loading module comprises a diamond anvil cell for placing the energetic sample, a brake for dynamically loading and unloading the diamond anvil cell during operation, and a pretensioner for initially centering and statically pretensioning the diamond anvil cell prior to operation, and wherein the brake is electrically connected to a power amplifier, and wherein the power amplifier is electrically connected to the function generator.
3. The sensitivity test system for milligram-grade to sub-milligram-grade energetic materials according to claim 2, further comprising a support, wherein a diamond anvil is arranged on the support, a brake is connected under the support in a threaded manner, and the brake is a piezoelectric ceramic actuator with an annular structure.
4. The sensitivity test system for milligram-level to sub-milligram-level energetic materials according to claim 2, wherein the public light path module comprises a first-level polychromatic beam splitter, a second-level polychromatic beam splitter, a third-level polychromatic beam splitter and an objective lens which are sequentially arranged along the same optical axis, and the objective lens is close to the pressure loading module; wherein the first-stage polychromatic beam splitter, the second-stage polychromatic beam splitter and the third-stage polychromatic beam splitter respectively correspond to light with different wavelengths; meanwhile, the first-stage polychromatic beam splitter, the second-stage polychromatic beam splitter and the third-stage polychromatic beam splitter respectively separate corresponding light paths to different functional components in the functional component module.
5. The sensitivity test system for milligram-level to sub-milligram-level energetic materials according to claim 4, wherein the first-level polychromatic beam splitter is highly reflective to middle infrared light, the second-level polychromatic beam splitter is highly reflective to visible light, and the third-level polychromatic beam splitter is highly reflective to specific laser wavelength; The reflecting surfaces of the first-stage polychromatic beam splitter, the second-stage polychromatic beam splitter and the third-stage polychromatic beam splitter respectively form an included angle of 45 degrees with the same optical axis, and the center of the same optical axis and the center of a sample cavity of the diamond anvil cell are coaxially and confocal arranged; The focus center of the objective lens is aligned with the center of the sample cavity of the diamond anvil cell.
6. The sensitivity test system for milligram-to sub-milligram-grade energetic materials according to claim 4, wherein the functional component module comprises an infrared spectrum measuring component, a Raman spectrum measuring component, a fluorescence spectrum measuring component and a high-speed imaging component; the infrared spectrum measuring assembly emits infrared light to perform transmission excitation on the energetic sample, transmission signals are collected by the objective lens and then transmitted to the first-stage polychromatic beam splitter, and the transmission signals are reflected to an infrared detector in the infrared spectrum measuring assembly by the first-stage polychromatic beam splitter; The generated Raman scattered light returns along the original path, sequentially passes through the first-stage polychromatic beam splitter, the second-stage polychromatic beam splitter and the third-stage polychromatic beam splitter, and then is reflected to a Raman spectrum detector in the Raman spectrum measurement assembly through the Raman/fluorescence beam splitter; The fluorescence spectrum measuring assembly emits laser, and the generated fluorescence signal returns along the original path and is reflected to a fluorescence detector in the fluorescence spectrum measuring assembly through the Raman/fluorescence beam splitter after sequentially passing through the first-stage polychromatic beam splitter, the second-stage polychromatic beam splitter and the third-stage polychromatic beam splitter; The high-speed imaging component is arranged on the reflecting light path side of the second-stage polychromatic beam splitter, directly collects the morphology and luminous images of the energetic sample in the pressure loading process, and receives the images after being reflected by the second-stage polychromatic beam splitter by a high-speed camera in the high-speed imaging component.
7. The sensitivity test system for milligram-level to sub-milligram-level energetic materials according to claim 6, wherein the infrared spectrum measurement component comprises an infrared light source, a filtering unit and an infrared detector, and the infrared light source is arranged on the transmission light path side of the first-level polychromatic beam splitter; The Raman spectrum measurement assembly comprises a pulse laser, a Raman/fluorescence beam splitter, a Raman filter and a spectrum detector, wherein the pulse laser is arranged on the reflecting light path side of the third-stage polychromatic beam splitter; The fluorescence spectrum measuring assembly comprises a pulse laser, a Raman/fluorescence beam splitter, a fluorescence filter and a fluorescence detector, wherein the Raman spectrum measuring assembly and the fluorescence spectrum measuring assembly share the same pulse laser and Raman/fluorescence beam splitter; The high-speed imaging component comprises an optical filter and a high-speed camera, and the optical filter and the high-speed camera are arranged on the reflecting light path side of the second-stage polychromatic beam splitter.
8. The system for testing the sensitivity of the milligram-level to sub-milligram-level energetic material according to claim 1 or 7, wherein the synchronous control module comprises a time sequence controller and a multi-channel shielding cable, and the timing trigger and the clock signals are sent to the components in the pressure loading module, the public optical path module and the functional assembly module through the multi-channel shielding cable to ensure the time synchronism of all actions and collection.
9. A method of using a sensitivity testing system according to any one of claims 1-8 for milligram-grade to sub-milligram-grade energetic materials, comprising the steps of: S1, loading an energetic sample to be measured and a ruby pressure scale into a sealed sample cavity in a pressure loading module; S2, triggering a pressure loading module to apply controllable pressure to the sample through a synchronous control module, and simultaneously triggering a functional component module to acquire a pressure signal, a molecular structure signal and a morphology image signal in the pressure loading process in real time through the synchronous control module; and S3, analyzing and judging sensitivity parameters of the energetic sample based on the acquired synchronous pressure signals, molecular structure signals and morphology image signals.
10. A method according to claim 9 using a milligram to sub-milligram energetic material sensitivity test system according to any one of claims 1 to 8, wherein: the step S3 specifically includes: By fitting the displacement of ruby fluorescence peaks, inverting and recording the change curve of the pressure in the sample cavity along with time in real time, and determining the pressure amplitude and the loading rate of dynamic loading; judging the chemical decomposition starting point and degree of the energetic sample by analyzing the characteristic peak changes of the infrared absorption spectrum and the Raman spectrum of the sample in the dynamic process; analyzing the appearance, color or luminescence mutation of the sample recorded by high-speed imaging to prove the occurrence of chemical reaction; determining a critical pressure value P R for inducing sample decomposition and a corresponding instantaneous loading rate V by utilizing the synchronous time stamp; The dynamic sensitivity factor S under the dynamic loading condition is calculated according to the formula S=P R .V and is used as a key index for quantitatively evaluating the impact sensitivity of the energetic material.

Description

Sensitivity test system and method for milligram-grade to sub-milligram-grade energetic material Technical Field The invention belongs to the technical field of safety performance test of energetic materials, and particularly relates to a sensitivity test system and method for milligram-grade to sub-milligram-grade energetic materials. Background The mechanical sensitivity, in particular the impact sensitivity, of energetic materials (such as explosives, propellants, etc.) is a central parameter for assessing the safety of their production, transportation, storage and use. Conventional sensitivity testing methods, such as drop hammer impact tests, typically require the consumption of tens of milligrams of sample, and most of the test results are binary qualitative or semi-quantitative determinations (i.e., "fire" or "no fire"), making it difficult to precisely quantify the sensitivity threshold of the material. In addition, the traditional method can not observe microstructure evolution and initial chemical reaction process of the material under impact load in situ, and severely restricts the deep research on the initiation mechanism. With the development of new energetic materials (e.g., nano energetic materials, energetic co-crystals, etc.), the amount of sample available is often very limited (in milligrams or less) at the early stages of material synthesis and screening. The traditional testing method cannot meet the requirements of research and development of modern energetic materials due to the inherent bottlenecks of large sample consumption, low testing precision, invisible process and the like. Therefore, developing a new technology for measuring sensitivity, which can realize micro dosage, high precision and quantification and has process observation capability, becomes a key technical problem to be solved in the field. The system and the method for representing the physical property based on dynamic loading are disclosed in China patent application No. CN202111532131.0, the publication date is 2022, 4 and 5, the system and the method comprise a dynamic loading device, a signal generating device and a physical property representing device which are sequentially connected, wherein the dynamic loading device is used for dynamically driving and rapidly realizing the change of pressure of a sample to be detected in a top anvil, the signal generating device is used for generating a voltage signal and synchronously transmitting the voltage signal to the dynamic loading device and the physical property representing device so as to synchronously realize the physical property representation and the dynamic loading, the physical property representing device is used for displaying the physical property representation of a sample to be detected under the pressure change based on the synchronous signal, the physical property representation and the dynamic loading are synchronously realized, and the microsecond time scale range of the physical property representing device is from seconds to microseconds. The patent has the defects that the sensitivity quantification and in-situ observation of the low-dose energetic material cannot be met by a general module, and the detection accuracy is general. For another example, chinese patent application number CN202311037400.5, published as 2023, 10 and 17, discloses a system and method for testing impact performance based on hopkinson bar. The impact performance testing system comprises a pulse laser, a spatial filter, a lens, a beam splitter, a reflecting mirror, a sample, a holographic imaging camera array module, an illumination system, a high-speed imaging camera array module and a Hopkinson bar which are sequentially connected. The method comprises the steps of generating fragment clouds after a sample is deformed, crushed, ignited and crushed in the process of the Hopkinson bar collision, capturing shock wave and fragment cloud information in the sample reaction process by using a holographic imaging camera array module, and capturing macroscopic data information in the sample reaction process by using a high-speed imaging camera array module. The disadvantage of this patent is that classical measurement difficulties exist when applying the hopkinson bar technique to small samples. Disclosure of Invention 1. Problems to be solved Aiming at the problems of high sample consumption and high error rate of the existing energetic material test, the invention provides a sensitivity test system and a sensitivity test method for milligram-level to sub-milligram-level energetic materials. The invention successfully realizes accurate and quantitative measurement of the sensitivity of milligram or even sub-milligram energetic materials, synchronously visualizes the dynamic response process, has objective and high repeatability of test results, thoroughly changes the limitation that the traditional method depends on large dosage, subjective judgment and appearance observation