CN108414552B - Method for detecting thermal stability of polymer bonded explosive - Google Patents
Method for detecting thermal stability of polymer bonded explosive Download PDFInfo
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- CN108414552B CN108414552B CN201810274545.XA CN201810274545A CN108414552B CN 108414552 B CN108414552 B CN 108414552B CN 201810274545 A CN201810274545 A CN 201810274545A CN 108414552 B CN108414552 B CN 108414552B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/201—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials by measuring small-angle scattering
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Abstract
The invention discloses a method for detecting the thermal stability of a polymer bonded explosive, which is characterized by comprising the following steps: the thermal stability of the microstructure of the polymer bound explosive was examined. The method comprises the following steps: preparing the formed PBX explosive into a sheet PBX sample, carrying out an in-situ temperature-changing neutron or X-photon small scattering experiment in a proper q range to obtain a change curve of the counting rate of scattered neutrons or X-photons along with the temperature, and then judging the thermal stability of the PBX explosive microstructure by analyzing the relative and absolute changes of the counting rate of the scattered neutrons or X-photons along with the temperature. The method can detect the influence of a small amount of relative overall microstructure thermal stability in the PBX, and is an effective method for detecting the microstructure thermal stability of the complex multi-component PBX material. The change of the scattering neutron or X-photon counting rate along with the temperature provided by the method is an important basis for deeply researching the structure-effect relationship between the thermal stability of the PBX explosive microstructure and various macroscopic properties.
Description
Technical Field
The invention relates to a method for detecting the thermal stability of a polymer bonded explosive, in particular to a method for detecting the thermal stability of a microstructure of a polymer bonded explosive.
Background
A Polymer bound Explosive (PBX Explosive) is a highly filled composite material (the filling amount is usually more than 90%) prepared from single Explosive crystals, a high Polymer binder and a plurality of additives through a series of complex processes. The PBX explosive has excellent comprehensive performance in safety performance, technological performance, mechanical performance, machining performance, physical and chemical stability and other aspects and is widely applied in the fields of national defense technology weaponry and national economy. The prepared and molded PBX explosive part can bear a series of temperature loads in the subsequent aging treatment, processing, assembly, transportation, storage, service and final detonation processes, the related temperature range can be changed from minus 100 ℃ to above minus 200 ℃, and the molded PBX explosive is required to have good temperature environment adaptability.
However, on the one hand, the complexity of the formulation of the PBX explosive itself (the different types of PBX explosive components can be increased from 2 to more than 10), in particular where the difference in thermo-physical properties between the explosive crystals and the polymeric binders is large, makes the thermal behaviour of the composite very complex; on the other hand, the content of each component in the PBX explosive formula is greatly different, for example, the content of explosive crystals and additives is different by more than two orders of magnitude, so that the contribution of a small amount of phase (such as an adhesive, a plasticizer, a desensitizer and the like) to the thermal stability influence of the microstructure of the PBX composite material is difficult to detect by a traditional thermal analysis method.
Currently, the common thermal analysis methods mainly include dynamic thermomechanical analysis (DMA), thermomechanical analysis (TMA), thermal constant analysis (thermal expansion coefficient measurement, etc.), thermogravimetric and simultaneous thermal analysis (TG-DSC), differential scanning thermal analysis (TG-DSC), thermal conductivity measurement, etc. However, the thermal physical parameters measured by a thermal constant analysis method, a thermogravimetric and synchronous thermal analysis method, a differential scanning thermal analysis method and a thermal conductivity method are mainly influenced by a main phase (explosive crystal) in the PBX, have small changes in a certain temperature range, and are not easy to directly give a small amount of influence on the thermal stability of a PBX microstructure; since PBX explosives are brittle materials (tensile breaking strength is within several MPa), detection means based on changes in mechanical constants, such as DMA and TMA, are also not suitable.
Disclosure of Invention
In order to overcome the defects of the conventional PBX explosive thermal stability detection method, the invention provides a method capable of detecting the thermal stability of a PBX explosive microstructure, and particularly capable of detecting the influence of a small amount of adhesives, other additives and the like on the thermal stability of the PBX explosive microstructure.
The method for detecting the thermal stability of the polymer bonded explosive provided by the invention comprises the following steps: preparing the formed PBX explosive into a sheet PBX sample with the thickness of 0.01-50 mm, preferably 0.1-10 mm; then, placing the sheet PBX sample at a small scattering spectrometer sample with an in-situ temperature changing device; then the temperature is increased at the temperature range of 4K to 573K, the temperature rise rate of 0.01K/min to 1000K/min and the temperature is increased at the wavelength of 0.0002nm-1～10 nm-1Carrying out in-situ temperature-changing small-angle scattering experiments on the PBX sample within the scattering vector q range, and collecting and recording the temperature of the sample and the change of all scattered neutrons or X photon counts on a detector along with the time; converting the change of all the scattered neutrons or X-photon counts along with time into a change curve of the scattered neutrons or X-photon counts along with time according to the time interval of 0.001 s-36000 s, preferably 0.1 s-3600 s; converting the change curve of the counting rate of the scattered neutrons or the X photons along with time into a change curve of the counting rate of the scattered neutrons or the X photons along with temperature; and analyzing the change of the scattered neutron or X-photon counting rate along with the temperature to obtain the thermal stability of the PBX explosive microstructure.
The small-angle scattering spectrometer is one or more of a neutron or X-photon small-angle scattering spectrometer, an X-ray small-angle scattering spectrometer, a neutron or X-photon ultra-small-angle scattering spectrometer, an X-ray ultra-small-angle scattering spectrometer and a spin echo neutron or X-photon small-angle scattering spectrometer.
The temperature range is 4K-573K, and in practice, a proper temperature range is selected according to the property of PBX material and research requirement, and 173K-473K is preferred.
The heating rate is 0.01K/min-1000K/min, and in practice, the proper heating rate is selected according to the attribute of PBX material and research requirement, and the optimal heating rate is 0.1K/min-50K/min.
The scattering vector q is in the range of 0.0002nm-1～10 nm-1In practice, the appropriate Q range is selected based on the characteristics of the PBX material, the characteristics of the low angle scattering device used and the research requirements.
The change of the scattered neutron or X-photon counting rate along with the temperature refers to one or more of the relative change and the absolute change of the scattered neutron or X-photon counting rate along with the change of the temperature.
Because the detection method involves the operation of energetic materials and the temperature rise and reduction experiment, safety operation regulations and cautions related to energetic materials and high and low temperature operations are necessarily observed in all experimental processes, particularly, the selection of the temperature range is reasonably selected by combining with the common knowledge of the properties of related materials, and related operations are completed by qualified personnel and in specific places.
In practical application, as long as the thickness, the temperature range, the heating rate and the scattering vector q range of the PBX explosive sample are reasonably selected and the time interval of the counting rate of scattered neutrons or X photons or X-ray photons is properly selected, the change curve of the counting rate of scattered neutrons or X photons with good quality along with the temperature can be obtained according to the steps, and then the thermal stability characteristic of the PBX explosive microstructure is obtained through analysis.
The method for detecting the thermal stability of the PBX explosive microstructure has the following advantages:
(a) the method is very simple in preparation, only an original sample is processed into a sheet with a proper size, and signal distortion caused by PBX sample damage in tests such as SEM (scanning electron microscope) does not exist;
(b) the method can measure the influence of the binder and other small additives in the PBX explosive on the PBX microstructure, and the traditional thermal analysis methods such as DSC, TG, DMA and the like are easily covered by the main phase of the explosive crystal, so that signals of a small number of phases are covered;
(c) the neutron or X-ray small-angle scattering in the invention is a transmission type test, and particularly, the sample size in the neutron or X-ray small-angle scattering test is in the centimeter level, so that very valuable statistical average information of a bulk phase can be given;
(d) the thermal stability of the PBX explosive microstructure obtained in the invention can be used for researching the series influence rules and structure-activity relationship of the PBX explosive microstructure on mechanical property, detonation combustion performance of the microstructure, accelerated aging mechanism, safety performance and the like, can also be used for researching PBX processing process parameter optimization research, environmental adaptability evaluation and the like, and is an important basis for deeply researching the structure-activity relationship between the thermal stability and the macroscopic property of the PBX explosive microstructure.
(e) The method for detecting the thermal stability of the PBX explosive microstructure can also be popularized to the detection research of other composite material systems.
Drawings
Figure 1 is a typical two-dimensional neutron or X-photon small angle scattering image of a series of contrast-shifted PBX samples in example 1;
figure 2 is an absolute intensity scattering curve for a series of contrast-shifted PBX samples in example 1;
FIG. 3 is a graph showing the change of the interface areas with molding pressure in the PBX according to example 1;
FIG. 4 is a DSC curve of a sample of PBX1 from example 1;
FIG. 5 is a TG curve of a sample of PBX1 from example 1;
FIG. 6 is a graph of the count rate of scattered neutrons and the temperature as a function of time in example 2;
FIG. 7 is a graph of the rate of scattered neutrons versus temperature in example 2;
FIG. 8 is a graph of the count rate of scattered neutrons and the temperature as a function of time in example 3;
FIG. 9 is a graph of the count rate of scattered neutrons versus temperature in example 3;
FIG. 10 is a graph of the count rate of scattered neutrons or X-photons as a function of temperature in example 4.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the following examples. In the following examples, the methods are all conventional methods unless otherwise specified. The PBX explosives used in the examples described below are all available commercially or custom synthesized by a particular entity.
EXAMPLE 1 testing of the thermal stability of sample PBX1 microstructures
Selecting the formed PBX1 explosive to prepare a sheet PBX sample with the thickness of 1mm and the diameter of phi =10 mm; then, placing the sheet PBX sample at a neutron small scattering spectrometer sample with an in-situ temperature changing device in the Mianyang research pile, as shown in figure 1; then under the condition of a layout in which the sample and the detector are 5.2 meters apart (corresponding to a scattering vector q ranging from 0.08 nm)-1～0.8 nm-1) Carrying out an in-situ temperature-changing neutron small-angle scattering experiment, heating from 303K to 433K at a heating rate of 1K/min, keeping for 5min at 433K, then cooling to 303K at a cooling rate of 1K/min, and collecting and recording the temperature of a sample and the change of all scattered neutron counts on a detector along with time; converting the change of all the scattered neutron counts along with time into a change curve of the scattered neutron count rate along with time according to a time interval of 60s, as shown in FIG. 2; converting the change curve of the scattering neutron counting rate along with time into a change curve of the scattering neutron relative counting rate along with temperature (100 is normalized by the 1-minute counting rate at the initial 303K), and showing in figure 3; analyzing the absolute and relative changes of the scattering neutron count rate with temperature as shown in fig. 3, it can be seen that the microstructure of the PBX1 sample is relatively stable around 303K to 340K, and there is a dip in the range of 340K to 360K, which indicates that the PBX explosive microstructure is unstable in this temperature range, and there is no significant change in the DSC and TG curves of the sample in the same temperature range.
EXAMPLE 2 testing of the thermal stability of sample PBX2 microstructures
Selecting the formed PBX2 explosive to prepare a sheet PBX sample with the thickness of 3mm and the diameter of phi =10 mm; then, placing the sheet PBX sample at a neutron small scattering spectrometer sample with an in-situ temperature changing device in the Mianyang research pile; then at 0.08nm-1～0.8 nm-1The in-situ temperature-changing neutron small-angle scattering experiment is carried out within the scattering vector q range, the temperature is increased from 293K to 393K at the temperature increasing rate of 1K/min, the temperature is kept for 5min at 393K, then the temperature is reduced to 293K at the temperature decreasing rate of 1K/min, and the change of the temperature of a sample and the count of all scattered neutrons on a detector along with the time is collected and recorded; converting all the scattered neutron counts into a variation curve of the scattered neutron count rate along with time according to a time interval of 60s, as shown in FIG. 6; converting the change curve of the count rate of the scattered neutrons or the X-photons along with time into a change curve of the relative count rate of the scattered neutrons or the X-photons along with temperature (normalized by a 1-minute count rate at an initial 293K rule 100), as shown in FIG. 7; analyzing the absolute and relative change of the scattering neutron count rate with temperature as shown in fig. 7, it can be seen that the microstructure of the PBX2 sample has a continuous decrease in the range of 330K to 390K, indicating that the microstructure of the PBX explosive as a whole changes with the increase of temperature all the time, and the change of the temperature decrease process is smaller.
Example 3 testing of the thermal stability of sample PBX3 microstructures
Selecting a molded PBX3 explosive to prepare a sheet PBX sample with the thickness of 1mm and the diameter of phi =10 mm; then, placing the sheet PBX sample at a neutron small scattering spectrometer sample with an in-situ temperature changing device in the Mianyang research pile; then at 0.08nm-1～0.8nm-1The in-situ temperature-changing neutron small-angle scattering experiment is carried out within the scattering vector q range, the temperature is increased from 293K to 393K at the heating rate of 1K/min, the temperature is kept for 5min at 393K, then the temperature is reduced to 293K at the heating rate of 1K/min, and the temperature of a sample and the change of all scattered neutron counts on a detector along with the time are collected and recorded; converting all the scattered neutron counts into a change curve of the scattered neutron or X-ray photon count rate along with time according to a time interval of 60s, as shown in FIG. 8; converting the variation curve of the scattering neutron counting rate with time into a variation curve of the scattering neutron relative counting rate with temperature (100 by using an initial 1-minute counting rate gauge at 293K), and displaying the variation curve in FIG. 9; analyzing the absolute and relative changes of the scattering neutron count rate with temperature as shown in fig. 9, it can be seen that the microstructure of the PBX3 sample was substantially stable during the 293K to 393K down cycle,maintaining a reversible state.
EXAMPLE 4 testing of the thermal stability of sample PBX4 microstructures
Selecting the formed PBX4 explosive to prepare a sheet PBX sample with the thickness of 1mm and the diameter of phi =10 mm; then, placing the sheet PBX sample at a neutron small scattering spectrometer sample with an in-situ temperature changing device in the Mianyang research pile; then at 0.08nm-1～0.8 nm-1An in-situ temperature-changing neutron small-angle scattering experiment is carried out within the scattering vector q range, the temperature is increased from 303K to 453K at the temperature increasing rate of 10K/min, the temperature is respectively maintained for 20min at 303K, 313K, 333K, 353K, 373K, 393K, 413K, 433K and 453K, then the temperature is reduced to 293K at the temperature increasing rate of 10K/min, the temperature is respectively maintained for 20min at 303K, 313K, 333K, 353K, 373K, 393K, 413K, 433K and 453K, and the temperature of the sample and the change of all scattered neutron counts on a detector along with the time are collected and recorded; converting the change of all the scattered neutron counts along with the time into a change curve of the scattered neutron count rate along with the time according to the time interval of 1200s, as shown in FIG. 10; converting the change curve of the scattering neutron counting rate along with time into a change curve of the scattering neutron relative counting rate along with temperature; analyzing the absolute and relative changes of the scattering neutron count rate with temperature as shown in fig. 10, it can be seen that the microstructure of the PBX4 sample undergoes irreversible changes during the temperature cycling from 303K to 453K.
EXAMPLE 5 testing of the thermal stability of sample PBX5 microstructures
Selecting a formed PBX5 explosive to prepare a sheet PBX sample with the thickness of 0.01mm and the diameter of phi =50 mm; then, placing the sheet PBX sample at an ultra-small angle neutron spectrometer sample with an in-situ temperature changing device; then at 0.0002nm-1～0.005nm-1The in-situ temperature-changing ultra-small angle neutron scattering experiment is carried out within the scattering vector q range, the temperature is increased from 293K to 393K at the temperature increasing rate of 0.01K/min, the temperature is kept for 5min at 393K, then the temperature is reduced to 293K at the temperature decreasing rate of 0.01K/min, and the temperature of a sample and the change of all scattered neutron counts on a detector along with the time are collected and recorded; converting all the scattered neutron counts into a variation curve of the scattered neutron count rate along with time according to a time interval of 36000 s; scattering the neutronsConverting the change curve of the counting rate along with time into a change curve of the relative counting rate of the scattered neutrons along with temperature; analysis of the absolute and relative changes in the scattered neutron count rate with temperature revealed that the microstructure of this PBX5 sample changed during the 293K to 393K temperature ramp up and down cycles.
EXAMPLE 6 testing of the thermal stability of sample PBX6 microstructures
Selecting a molded PBX5 explosive to prepare a sheet PBX sample with the thickness of 1mm and the diameter of phi =10 mm; then, placing the sheet PBX sample at a spin echo neutron small-angle spectrometer sample with an in-situ temperature changing device; then at 0.003nm-1～10 nm-1An in-situ temperature-changing spin echo small-angle neutron scattering experiment is carried out within the scattering vector q range, the temperature is increased from 293K to 573K at the temperature increase rate of 1K/min, the temperature is kept for 5min at 573K, and then the temperature is reduced to 293K at the temperature decrease rate of 1K/min; carrying out in-situ temperature-changing ultra-small angle neutron scattering experiments on the PBX sample, and acquiring and recording the temperature of the sample and the change of all scattered neutron counts on a detector along with time; converting all the scattered neutron counts into a variation curve of the scattered neutron count rate along with time according to a time interval of 60 s; converting the change curve of the scattering neutron counting rate along with time into a change curve of the scattering neutron relative counting rate along with temperature; analysis of the absolute and relative changes in the scattered neutron count rate with temperature revealed that the microstructure of this PBX6 sample changed during the 293K to 573K temperature ramp up and down cycles.
EXAMPLE 7 testing of the thermal stability of sample PBX7 microstructures
Selecting a molded PBX7 explosive to prepare a sheet PBX sample with the thickness of 1mm and the diameter of phi =10 mm; then, placing the sheet PBX sample at an X-ray small-angle spectrometer sample with an in-situ temperature changing device; then at 0.01nm-1～0.1 nm-1The in-situ temperature-changing X-ray small-angle scattering experiment is carried out within the scattering vector q range, the temperature is increased from 4K to 573K at the temperature increasing rate of 1000K/min, the temperature is kept for 5min at 573K, then the temperature is reduced to 4K at the temperature decreasing rate of 1000K/min, and the temperature of a sample and the change of all scattered X-ray counts on a detector along with the time are collected and recorded; converting said all scattered X-photon counts into scatters at 0.001s intervalsThe variation curve of the X-ray photon counting rate along with time; converting the change curve of the scattering X-ray counting rate along with time into a change curve of the scattering X-ray relative counting rate along with temperature; analysis of the absolute and relative changes in the scattered X-photon count rates with temperature revealed changes in the microstructure of the PBX7 sample during the 4K to 573K rise and fall cycles.
EXAMPLE 8 testing of the thermal stability of sample PBX8 microstructures
Selecting a molded PBX8 explosive to prepare a sheet PBX sample with the thickness of 50mm and the diameter of phi =10 mm; then, placing the sheet PBX sample at an X-ray ultra-small angle spectrometer sample with an in-situ temperature changing device; then at 0.001nm-1～0.01 nm-1The in-situ temperature-changing X-ray ultra-small angle scattering experiment is carried out within the scattering vector q range, the temperature is increased from 293K to 393K at the temperature increasing rate of 1K/min, the temperature is kept for 5min at 393K, then the temperature is reduced to 293K at the temperature decreasing rate of 1K/min, and the temperature of a sample and the change of all scattered X-ray counts on a detector along with the time are collected and recorded; converting all the scattered X-photon counts into a change curve of the scattered X-photon count rate along with time according to a time interval of 60 s; converting the change curve of the scattering X-ray counting rate along with time into a change curve of the scattering X-ray relative counting rate along with temperature; analysis of the absolute and relative changes in the scattered X-photon count rates with temperature revealed that the microstructure of this PBX8 sample changed during the 293K to 393K temperature ramp up and down cycles.
Claims (7)
1. A method of testing the thermal stability of a polymer bound explosive, comprising: the method comprises the following steps:
preparing the formed PBX explosive into a sheet PBX sample with the thickness of 0.01-50 mm;
then, placing the sheet PBX sample at a neutron or X-photon small-angle scattering spectrometer sample with an in-situ temperature changing device;
then the temperature is increased at the temperature range of 4K to 573K, the temperature rise rate of 0.01K/min to 1000K/min and the temperature is increased at the wavelength of 0.0002nm-1～10 nm-1Carrying out in-situ temperature-changing small-angle scattering experiment on the PBX sample within the scattering vector q range, and collecting and recording the temperature of the sampleThe degree and the count of all scattered neutrons or X-photons on the detector over time;
then converting the change of all the scattered neutrons or X-photon counts along with time into a change curve of the scattered neutrons or X-photon counts along with time according to the time interval of 0.001 s-36000 s;
then converting the change curve of the scattering neutron or X-ray photon counting rate along with time into a change curve of the scattering neutron or X-ray photon counting rate along with temperature;
and then analyzing the change of the scattered neutron or X-ray counting rate along with the temperature to obtain the thermal stability of the PBX explosive microstructure.
2. The method of testing the thermal stability of a polymer bound explosive according to claim 1, wherein: the neutron or X-photon small-angle scattering spectrometer is more than one of a neutron small-angle scattering spectrometer, an X-ray small-angle scattering spectrometer, a neutron ultra small-angle scattering spectrometer, an X-ray ultra small-angle scattering spectrometer, a spin echo neutron or an X-photon small-angle scattering spectrometer.
3. The method of testing the thermal stability of a polymer bound explosive according to claim 1, wherein: the temperature range is 173K-473K according to the properties of PBX materials and research requirements.
4. The method of testing the thermal stability of a polymer bound explosive according to claim 1, wherein: the heating rate is selected to be 0.1K/min-50K/min according to the attribute of the PBX material and the research requirement.
5. The method of testing the thermal stability of a polymer bound explosive according to claim 1, wherein: the thickness of the sheet-shaped PBX sample is 0.1 mm-10 mm.
6. The method of testing the thermal stability of a polymer bound explosive according to claim 1, wherein: the time interval is 0.1 s-3600 s.
7. The method of testing the thermal stability of a polymer bound explosive according to claim 1, wherein: the change of the scattered neutron or X-ray photon counting rate along with the temperature refers to more than one of the relative change and the absolute change of the scattered neutron or X-ray photon counting rate along with the temperature change.
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