CN113237847B - Nondestructive testing method and system for hexanitrohexaazaisowurtzitane crystal form - Google Patents
Nondestructive testing method and system for hexanitrohexaazaisowurtzitane crystal form Download PDFInfo
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Abstract
The invention relates to a nondestructive testing method and a nondestructive testing system for a hexanitrohexaazaisowurtzitane crystal form. The invention applies the terahertz spectrum technology to the field of explosive crystal form detection so as to realize nondestructive detection of the crystal form of a typical single-substance explosive CL-20 sample.
Description
Technical Field
The invention relates to the technical field of explosive crystal form identification, in particular to an in-situ terahertz nondestructive testing method and system for a hexanitrohexaazaisowurtzitane crystal form.
Background
Hexanitrohexaazaisowurtzitane (CL-20, HNIW) is a typical cage type multi-ammonium nitrate high-energy explosive, is an elementary explosive which is discovered to date and has the highest energy and the strongest power, and is applied to the fields of propellants, mixed explosives, propellant powder and the like by gradually replacing traditional energetic compounds such as HMX and the like. Although CL-20 has a wide application prospect, in the life cycle of CL-20, such as processing, storage, transportation, use and the like, the CL-20 is usually stimulated by extreme conditions, such as high temperature, high pressure, impact, shock wave and the like, and the stimulation of the extreme conditions can cause explosive crystals to generate a series of crystal form transformations. The transformation of crystal form can directly result in the change of unit cell volume, crystal density, chemical stability, etc., thereby affecting the energy and sensitivity and reducing the safety of the material. The existing research results show that at normal temperature, the transformation activation energy between the four crystal forms of CL-20 is very small, and the phenomenon of crystal form transformation is easy to occur, so that the storage, use and other processes of the CL-20 are influenced insignificantly. Therefore, effective detection and identification of the CL-20 crystal form is of great significance to the design of advanced weapons, long-term storage of explosives, and safety assessment.
The currently generally adopted explosive crystal form analysis methods include infrared spectroscopy, Raman spectroscopy, X-ray diffraction technology and the like, the principle of the infrared spectroscopy technology is that the infrared absorption spectrum of a substance can be obtained by detecting the condition that infrared rays are absorbed by utilizing the principle that molecules can selectively absorb infrared rays with certain wavelengths so as to cause the transition of vibration energy levels and rotation energy levels in the molecules. The principle of the Raman spectrum technology is to analyze a scattering spectrum with different incident light frequencies by utilizing a Raman scattering effect so as to obtain information on molecular vibration and rotation and apply the information to molecular structure research. The principle of the X-ray diffraction technology is that when X-rays enter a crystal, the X-rays scattered by different atoms interfere with each other to generate diffraction, the position and the intensity of the spatial distribution of the diffraction rays are closely related to the crystal structure, and material information is obtained through analysis of the diffraction results. These methods have defects, such as too high photon energy, possibly causing ionization reaction, damaging the test sample (especially metastable substances such as elementary explosive) and affecting the test result, even causing threat to the safety of equipment and personnel.
Disclosure of Invention
The invention aims to provide a nondestructive testing method and a nondestructive testing system for a hexanitrohexaazaisowurtzitane crystal form, which are used for realizing nondestructive testing of the hexanitrohexaazaisowurtzitane crystal form.
In order to achieve the purpose, the invention provides the following scheme:
a nondestructive testing method for a crystal form of hexanitrohexaazaisowurtzitane, which comprises the following steps:
acquiring a terahertz spectrum of a sample to be detected;
processing the terahertz spectrum to obtain absorption coefficient data of the sample to be detected;
drawing an absorption spectrogram of the sample to be detected according to the absorption coefficient data;
acquiring absorption spectrograms of a plurality of standard samples; each of the standard samples is a crystal form of hexanitrohexaazaisowurtzitane;
and comparing the absorption spectrogram of the sample to be detected with the absorption spectrogram of the standard sample to determine the crystal form of the sample to be detected.
A non-destructive testing system for a crystalline form of hexanitrohexaazaisowurtzitane, the testing system comprising:
the terahertz spectrum acquisition module is used for acquiring a terahertz spectrum of a sample to be detected;
the terahertz spectrum processing module is used for processing the terahertz spectrum to obtain absorption coefficient data of the sample to be detected;
the absorption spectrogram drawing module is used for drawing an absorption spectrogram of the sample to be detected according to the absorption coefficient data;
the crystal form determining module is used for acquiring absorption spectrograms of a plurality of standard samples; each of the standard samples is a crystal form of hexanitrohexaazaisowurtzitane; and comparing the absorption spectrogram of the sample to be detected with the absorption spectrogram of the standard sample to determine the crystal form of the sample to be detected.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
according to the nondestructive testing method and system for the crystal form of the hexanitrohexaazaisowurtzitane, the terahertz spectrum of a sample to be tested is obtained, the terahertz spectrum is processed, the absorption spectrogram of the sample to be tested is drawn, and finally the absorption spectrogram of the sample to be tested and the absorption spectrogram of a standard sample are compared to determine the crystal form of the sample to be tested. The invention applies the terahertz spectrum technology to the field of explosive crystal form detection so as to realize nondestructive detection of the crystal form of a typical single-substance explosive CL-20 sample. The terahertz wave band is located between microwave and infrared light waves in the electromagnetic spectrum, the frequency position is 0.1-10THz, the photon energy of the terahertz wave band is about 4.1 millielectron volts, and the terahertz wave band is only 1/108 of the photon energy of X-ray, and compared with other wave band spectrums, the terahertz wave band has excellent low-energy characteristics. The detection and identification of the CL-20 crystal form are realized by utilizing the terahertz time-domain spectroscopy technology, the damage to a sample to be detected caused by overhigh radiation energy can be effectively prevented, the adverse effect on a test result is prevented, and the nondestructive detection is realized.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is a flowchart of a nondestructive testing method provided in embodiment 1 of the present invention.
FIG. 2 is an absorption spectrum of epsilon-CL-20 provided in example 1 of the invention.
FIG. 3 is an absorption spectrum of gamma-CL-20 provided in example 1 of the present invention.
FIG. 4 is an absorption spectrum of a sample to be tested for CL-20 at 25 ℃ provided in example 1 of the invention.
FIG. 5 is an absorption spectrum of a sample CL-20 to be tested at 100 ℃ provided in example 1 of the invention.
FIG. 6 is an absorption spectrum of a sample to be tested for CL-20 at 140 ℃ provided in example 1 of the invention.
FIG. 7 is an absorption spectrum of a sample to be tested for CL-20 at 180 ℃ provided in example 1 of the invention.
FIG. 8 is a comparative analysis chart of the absorption spectra of a sample CL-20 to be tested at 25 ℃ provided in example 1 of the invention.
FIG. 9 is a comparative analysis chart of the absorption spectra of the CL-20 samples to be tested at 100 ℃ provided in example 1 of the invention.
FIG. 10 is a comparative analysis chart of the absorption spectra of the CL-20 samples to be tested at 140 ℃ provided in example 1 of the invention.
FIG. 11 is a comparative analysis chart of the absorption spectra of the CL-20 samples to be tested at 180 ℃ provided in example 1 of the invention.
Fig. 12 is a system block diagram of a nondestructive inspection system provided in embodiment 2 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a nondestructive testing method and a nondestructive testing system for a hexanitrohexaazaisowurtzitane crystal form, which are used for realizing nondestructive testing of the hexanitrohexaazaisowurtzitane crystal form.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example 1:
this example is used to provide a nondestructive testing method for a crystal form of hexanitrohexaazaisowurtzitane, as shown in fig. 1, the testing method includes the following steps:
s1: acquiring a terahertz spectrum of a sample to be detected;
before the terahertz spectrum of the sample to be detected is obtained, the sample to be detected needs to be prepared, and the specific preparation process comprises the following steps: 480mg of sample dispersant (such as PTFE) and 84mg of CL-20 drug to be tested are weighed out to the nearest 0.1mg by an electronic balance. The accuracy of the electronic balance may be as high as 0.1mg, and specifically, an AUW120D type electronic balance may be used. Held in clean test paper and poured carefully into the center of an agate mortar, respectively. And (3) taking an agate mortar grinding rod to properly grind the powder around the center of the mortar from inside to outside clockwise for 3-5 minutes, slightly scraping the powder spread at the bottom of the mortar to the center by using a horn spoon after grinding, grinding again, circulating for 3-5 times to completely and uniformly mix the two materials, weighing 470mg of mixed medicine after grinding, placing the mixed medicine in clean test paper, and taking the mixed medicine as the medicine to be pressed, wherein the concentration is 0.1 mg. The drug to be pressed is carefully poured into a phi 13 metal pressing die along the crease of the test paper, so that the drug is prevented from being scattered and adhered to the test paper. And slightly shaking the die to keep the medicine powder flat, sealing the die, placing the die at the center of a tabletting point of a tabletting machine, pressurizing to 200MPa, and maintaining the pressure for 2 minutes. And releasing the pressure of the tablet press after the pressure maintaining time is over, taking out a circular sheet sample with the diameter of 13mm, sealing and storing the sample by using a small plastic sample bag to obtain a sample to be detected, and standing the sample in a dry environment at normal temperature and normal pressure to release the pressure for one day. After the sample pressing was completed, the mold was washed with absolute ethanol for the next use. And after the pressure of the sample to be measured is released, respectively measuring the central thickness of the sample to be measured by a screw micrometer and marking the central thickness, measuring the thickness for multiple times and then averaging to obtain the thickness of the sample to be measured, wherein the unit is millimeter, and one decimal is reserved.
S1 may include: firstly, a terahertz time-domain spectroscopy system is used for collecting a terahertz spectrum of dry air, and then the terahertz spectrum of a sample to be detected is collected by the terahertz time-domain spectroscopy system.
Specifically, a Z-3 terahertz time-domain spectroscopy system is used for collecting terahertz spectrum of a sample to be tested, and the test parameters of the terahertz time-domain spectroscopy system are as follows: the central wavelength of the laser is 800nm, the total laser power energy is 650nW, the pump light energy is 100mW, the detection light energy is 20mW, the scanning starting point of the Z-3 terahertz time-domain spectroscopy system is 50ps, the scanning length is 60ps, the scanning speed of the translation stage is 0.61mm/s, and the spectrum is obtained by continuously scanning for 2 times to calculate the average. The test environment of the terahertz time-domain spectroscopy system is normal temperature and normal pressure, and the relative humidity is less than 3%. The specific spectrum testing steps are as follows: firstly, the normal test environment is ensured, specifically, the indoor environment is normal temperature and normal pressure, and the relative humidity is about 45%. The internal environment of the Z-3 terahertz time-domain spectroscopy system is normal temperature and normal pressure, and the relative humidity is less than 3%; secondly, turning on the laser; starting a Z-3 terahertz time-domain spectroscopy system; testing the terahertz spectrum of the dry air and storing data to obtain the terahertz spectrum of the dry air; placing a sample to be tested; sixthly, repeating disturbance to the test environment at intervals of ten minutes; seventhly, testing the terahertz spectrum of the sample to be tested and storing data to obtain the terahertz spectrum of the sample to be tested; closing the Z-3 terahertz time-domain spectroscopy system; ninthly, turning off the laser.
S2: processing the terahertz spectrum to obtain absorption coefficient data of the sample to be detected;
for convenience of description, firstly, the terahertz spectrum data of the dry air is recorded as a reference signal E ref (t) recording the terahertz spectrum data of the sample to be detected as a sample signal E sam (t)。
S2 may include:
for reference signal E ref (t) and sample signal E sam (t) respectively carrying out fast Fourier transform to obtain frequency domain reference data E ref (ω) and frequency domain sample data E sam (ω); the number of FFT transform points is 4096;
from frequency-domain reference data E ref (ω) and frequency domain sample data E sam And (omega) calculating the absorption coefficient data of the sample to be detected. Specifically, the reference data E is first obtained according to the frequency domain ref (ω) and frequency domain sample data E sam (ω) the amplitude ratio and phase difference of each transformed point are calculated. And calculating the refractive index of each conversion point according to the phase difference, and calculating the absorption coefficient of each conversion point according to the amplitude ratio and the refractive index to obtain the absorption coefficient data of the sample to be measured.
For any one transformation point, the amplitude ratio is calculated as follows:
in formula 1, ρ (ω) is the amplitude ratio; a. the sam The amplitude of the frequency domain sample data corresponding to the transformation point; a. the ref The amplitude of the frequency domain reference data corresponding to the transformation point; ω is the angular frequency, ω is 2 pi f, and f is the frequency corresponding to the transform point.
The calculation formula of the phase difference is as follows:
in the formula 2, the first step is,
is the phase difference;
the phase angle of the frequency domain sample data corresponding to the transformation point;
is the phase angle of the frequency domain reference data corresponding to the transform point.
The calculation formula of the refractive index is as follows:
in formula 3, n (ω) is a refractive index; c is the speed of light in air; d is the thickness of the sample to be measured.
The absorption coefficient is calculated as follows:
in formula 4, α (ω) is an absorption coefficient.
S3: drawing an absorption spectrogram of the sample to be detected according to the absorption coefficient data;
specifically, the absorption coefficient data is smoothed by a Savitzky-Golay method in Origin (2018 version) software to obtain the smoothed absorption coefficient data. The parameters are set to window point number 33, polynomial order number 5. The basic processing steps are as follows: "analysis" → "signal processing" → "smoothing" → "open dialog" → "parameter setting →" determination ".
And then drawing an absorption spectrum chart of the sample to be measured by using Origin (2018 edition) according to the smoothed absorption coefficient data.
S4: acquiring absorption spectrograms of a plurality of standard samples; each of the standard samples is a crystal form of hexanitrohexaazaisowurtzitane;
the embodiment also comprises the step of preparing a standard sample by using the method S1, and only replacing the CL-20 medicine to be tested with a standard crystal form medicine. After the standard sample is obtained, the terahertz spectrum of the dry air and the terahertz spectrum of the standard sample are collected by the terahertz time-domain spectroscopy system. And then calculating the absorption coefficient data of the standard sample by using the method S2, and drawing the absorption spectrogram of the standard sample by using the method S3 to obtain the absorption spectrogram of the standard sample.
S5: and comparing the absorption spectrogram of the sample to be detected with the absorption spectrogram of the standard sample to determine the crystal form of the sample to be detected.
CL-20 of different crystal forms corresponds to different fingerprint spectrums, the absorption spectrogram of a sample to be detected and the absorption spectrogram of a standard sample are compared and analyzed, the absorption spectrogram of the sample to be detected and the absorption spectrogram of the standard sample are compared to carry out characteristic absorption peak identification, and the CL-20 crystal form can be determined according with the related absorption peak frequency position and the absorption intensity.
Since the measured signal-to-noise ratio of terahertz in the frequency range less than 3THz is greater than 10000, in order to further improve the comparison speed and accuracy, in this embodiment, before performing comparison analysis on the absorption spectrogram, the absorption spectrogram of the sample to be detected and the absorption spectrogram of the standard sample can be respectively intercepted according to the preset frequency range, so as to obtain the intercepted absorption spectrogram of the sample to be detected and the intercepted absorption spectrogram of the standard sample, where the preset frequency range is an effective frequency range of 0.4-2.0 THz. And then comparing the intercepted absorption spectrogram of the sample to be detected with the intercepted absorption spectrogram of the standard sample to determine the crystal form of the sample to be detected.
Terahertz (THz) waves refer to electromagnetic radiation with a frequency in the range of 0.1-10THz (wavelength 3mm-30um), between the microwave and infrared bands. The terahertz wave spectrum detection technology of the substance has great application value in the fields of military, medicine, astronomy, safety detection and the like. Terahertz spectrum detection technology has many advantages: (1) the terahertz spectrum has high measurement precision, the signal-to-noise ratio of the terahertz spectrum in the frequency range smaller than 3THz is greater than 10000, the interference of background radiation noise can be effectively inhibited, and the micro change of the sample composition can be effectively identified and analyzed; (2) the terahertz frequency band photon energy is very low, about 4.1meV (millielectron volt), is only one 108 times of the X-ray photon energy, is lower than the bond energy of various chemical bonds, cannot cause damage to a measured object due to photoionization, and can realize non-ionization and high-sensitivity detection on organic matters; (3) the terahertz coherent measurement technology can directly measure the amplitude and phase of an electric field, so that optical parameters such as the refractive index, the absorption coefficient, the extinction coefficient, the dielectric constant and the like of a sample to be measured can be conveniently extracted; (4) the terahertz waveband contains abundant physical and chemical information, and most of vibration and rotation energy level transitions of polar molecules and biomacromolecules are in the terahertz waveband, such as low-frequency oscillation of crystal lattices, rotation and vibration transition of dipoles and the like. Therefore, the terahertz technology has unique advantages in the aspect of explosive structure characterization and is expected to become an important technical means for explosive crystal transformation detection. Although belonging to a part of vibration spectrum, in terms of explosive crystal form analysis, terahertz spectrum has the following advantages compared with infrared spectrum and raman spectrum: the terahertz spectrum is caused by lattice vibration and low-energy hydrogen bond vibration, is more sensitive to molecular configuration difference, and is more suitable for crystal form analysis. The terahertz spectrum is sensitive to temperature and can be used for crystal form analysis in a heating or cooling environment. The terahertz spectrum is low in energy, so that degradation or transformation of a sample in the testing process can be avoided, and nondestructive testing is realized. And fourthly, the terahertz absorption spectra of different crystal forms CL-20 have obvious response difference in absorption peak frequency and absorption peak intensity, and the crystal form analysis can be better completed by utilizing the terahertz spectrum detection technology.
In the embodiment, based on the advantages of the terahertz spectrum detection technology, in the identification process of the hexanitrohexaazaisowurtzitane crystal form, the terahertz spectrum of the sample to be detected is obtained, the terahertz spectrum is processed to obtain absorption coefficient data, an absorption spectrogram is drawn based on the absorption coefficient data, and the crystal form of the sample to be detected is determined by comparing the absorption spectrogram. In the embodiment, the terahertz spectrum technology is applied to the field of explosive crystal form detection so as to realize nondestructive detection of a typical single-substance explosive CL-20 sample crystal form. The terahertz wave band is located between microwave and infrared light waves in the electromagnetic spectrum, the frequency position is 0.1-10THz, the photon energy of the terahertz wave band is about 4.1 millielectron volts, and the terahertz wave band is only 1/108 of the photon energy of X-ray, and compared with other wave band spectrums, the terahertz wave band has excellent low-energy characteristics. The detection and identification of the CL-20 crystal form are realized by utilizing the terahertz time-domain spectroscopy technology, the damage to a sample to be detected caused by overhigh radiation energy can be effectively prevented, the adverse effect on a test result is prevented, and the nondestructive detection is realized. In addition, the existing crystal form identification method is not sensitive enough to the crystal form/conformation of the crystal, and cannot represent the difference among different crystal forms from the angle of weak interaction force among molecules, but the embodiment utilizes the sensitive characteristic of the terahertz technology to the difference of the explosive molecular configuration, so that the spectrum detection result is more intuitive, and the crystal form detection and analysis are facilitated. The existing research shows that the structure of explosive molecules and related environmental information are closely related to weak acting force among molecules, such as hydrogen bond vibration of a low energy state, low-frequency vibration of crystal lattices in crystals, rotation and vibration transition of dipoles, skeleton vibration of macromolecules and the like, and the vibration frequency of the weak acting force is mainly concentrated in a terahertz frequency band. Different explosive crystal forms have obvious differential response in the aspects of characteristic absorption peak frequency positions and absorption intensity, so that the detection and identification of the CL-20 crystal form are realized by utilizing the terahertz spectrum, the result is more visual, and the identification precision is higher.
The nondestructive testing method can also be used for carrying out crystal form identification on samples to be tested at different temperatures, when the terahertz spectrum of the samples to be tested is collected by utilizing the terahertz time-domain spectroscopy system, the preset environment temperature is applied to the samples to be tested, the terahertz spectrum of the samples to be tested at the preset environment temperature is obtained, and then the terahertz spectrum at the preset environment temperature is processed by utilizing the method, so that the crystal form of the samples to be tested at the preset environment temperature can be obtained. Here, the process is described in detail with reference to a specific example. The following example shows an in-situ terahertz nondestructive testing method for a crystalline form of CL-20 in a temperature rising process, which comprises the following steps:
step one, preparing a standard reference sample and a sample to be tested:
480mg PTFE and 84mg epsilon-CL-20 drugs were weighed to 0.1mg each on an AUW120D electronic balance and carefully poured into the center of the bottom of an agate mortar. Taking an agate mortar grinding rod to properly grind the agate mortar grinding rod clockwise for 3-5 minutes along the periphery of the central powder medicine of the mortar, slightly scraping the medicine spread at the bottom of the mortar to the center by using a horn spoon after grinding, grinding again, circulating the grinding process for 3-5 times to completely and uniformly mix PTFE and epsilon-CL-20, weighing 470mg of mixed medicine after grinding is finished, placing the mixed medicine by using clean test paper, accurately weighing the mixed medicine to 0.1mg, and recording the mixed medicine as a first medicine to be pressed.
480mg of PTFE and 84mg of gamma-CL-20 are respectively weighed to be accurate to 0.1mg, 470mg of mixed medicine is weighed after the materials are ground and mixed evenly by adopting the method, the mixed medicine is contained by clean test paper to be accurate to 0.1mg, and the mixed medicine is marked as a second medicine to be pressed. 480mg of PTFE and 84mg of CL-20 to be tested are respectively weighed to be accurate to 0.1mg, 470mg of mixed medicine is weighed after the above method is adopted for grinding and mixing evenly and is contained by clean test paper to be accurate to 0.1mg, and the obtained product is recorded as a third medicine to be pressed.
And carefully pouring the to-be-pressed medicine into a phi 13 metal pressing die along the crease of the test paper to ensure that the medicine is not scattered and adhered to the test paper. And slightly shaking the die to keep the medicine powder flat, sealing the die, placing the die at the center of a tabletting point of a tabletting machine, manually pressurizing to 200MPa, and maintaining the pressure for 2 minutes. And releasing the pressure of the tablet press after the pressure maintaining time is over, taking out a circular sheet sample with the diameter of 13mm, sealing and storing the sample by using a small plastic sample bag, recording the sample as a standard sample I, and standing the sample in a normal-temperature normal-pressure drying environment to release the pressure for one day. And measuring the central thickness of the standard sample I by a screw micrometer for three times after the pressure of the standard sample I is released, and averaging to obtain the thickness of the standard sample I, wherein the unit is millimeter, and one decimal is reserved. After the sample pressing was completed, the mold was cleaned with alcohol for the next use. Pressing the second and third medicines to be pressed into circular sheet samples with the diameter of 13mm by the same method, sealing and storing the circular sheet samples by using plastic sample bags, respectively recording the circular sheet samples as a second standard sample and a to-be-detected sample, standing the circular sheet samples in the same environment for one day to release the pressure, and obtaining the thicknesses of the second standard sample and the to-be-detected sample by the method after the pressure is released.
Step two, collecting the terahertz spectrum of the standard sample:
the terahertz spectrum of a standard sample is acquired by using a Z-3 terahertz time-domain spectroscopy system, the test parameters of the terahertz time-domain spectroscopy system are that the central wavelength of a laser is 800nm, the total laser power energy is 650nW, the pump light energy in the system is 100mW, the detection light energy is 20mW, the scanning starting point of the Z-3 terahertz time-domain spectroscopy system is 50ps, the scanning length is 60ps, the scanning speed of a translation stage is 0.61mm/s, and the spectrum is obtained by continuously scanning for 2 times and averaging. The test environment of the system is normal temperature and normal pressure, and the relative humidity is less than 3%.
The specific spectrum testing steps are as follows: firstly, ensuring that a test environment is normal, specifically, an indoor environment is normal temperature and normal pressure, the relative humidity is about 45%, an internal environment of a Z-3 terahertz time-domain spectroscopy system is normal temperature and normal pressure, and the relative humidity is less than 3%; secondly, turning on the laser; starting a Z-3 terahertz time-domain spectroscopy system; testing the terahertz spectrum of the dry air and storing data; placing a first standard sample; sixthly, repeating disturbance to the test environment at intervals of ten minutes; seventhly, acquiring a terahertz spectrum of the standard sample I and storing data; repeating the step 5 → 7 to obtain the spectral data of the standard sample II; and ninthly, blocking the light outlet of the laser and detecting a pause system.
Step three, applying an environmental temperature to the sample to be tested, and simultaneously collecting the terahertz spectrum of the sample to be tested:
firstly, a sample to be measured is placed on the innermost gasket of the contact type metal electric heating device, the cover layer of the electric heating device is carefully rotated and sealed, and the electric heating device does not excessively extrude the sample to be measured. And then placing the electric heating device at a terahertz wave focusing point of a Z-3 transmission type terahertz time-domain spectroscopy system, so that the terahertz wave penetrates through a sample to be detected positioned at a light inlet window of the electric heating device. And (5) continuing system detection, and ensuring that the test parameters and the system test environment of the terahertz time-domain spectroscopy system are the same as those in the second step.
The environmental temperature is applied to the sample to be measured through an electric heating device temperature rise controller on the periphery of the system, the maximum temperature rise range is 25-300 ℃, the temperature rise range selected in the embodiment is 25-180 ℃, the precision is 1 ℃, the temperature rise rate is 10 ℃ per ten minutes, namely, the temperature is increased by 10 ℃ in a stepped mode every ten minutes, and the current actual sample temperature is observed through the temperature rise device controller. And when the display screen displays that the current temperature reaches the set temperature, continuously waiting for ten minutes to ensure that the sample reaches the set temperature. At the moment, the current terahertz time-domain spectral data can be stored through Z-3 system control software, and the terahertz spectral data detection and storage of the temperature nodes of 25 ℃, 100 ℃, 140 ℃ and 180 ℃ are completed through the same steps.
Step four, preprocessing an original spectrum, and extracting key parameters:
the method comprises the steps of dividing original spectrum data measured in the experimental process into two types for processing, taking spectrum data of dry air as reference signals, and taking spectrum data measured by a standard sample I, a standard sample II and a sample to be measured at each temperature node as sample signals respectively. And (3) performing fast Fourier transform on the reference signal and the sample signal respectively, wherein the number of FFT transform points is 4096, and obtaining frequency domain reference data and frequency domain sample data. And (3) calculating and obtaining the absorption coefficient data of the standard sample I, the standard sample II and the sample to be detected at each temperature node by using the formulas (1), (2), (3) and (4).
Step five, optimizing data, and drawing a spectrogram:
and (4) smoothing the absorption coefficient data obtained in the fourth step by a Savitzky-Golay method in Origin 2018 software, wherein parameters are set as window point number 33 and polynomial order number 5. The basic processing steps are as follows: "analysis" → "signal processing" → "smoothing" → "open dialog" → "parameter setting →" determination ".
And step six, comparing the spectrogram and identifying the crystal form.
Drawing the absorption coefficient data processed in the fifth step into an absorption spectrogram through Origin 2018 software, wherein the drawing is the absorption spectrogram of epsilon-CL-20 (a standard sample I), the drawing is the absorption spectrogram of gamma-CL-20 (a standard sample II), the drawing is the absorption spectrogram of a CL-20 sample to be tested at 25 ℃, the drawing is the absorption spectrogram of a CL-20 sample to be tested at 100 ℃, the drawing is the absorption spectrogram of a CL-20 sample to be tested at 140 ℃, and the drawing is the absorption spectrogram of a CL-20 sample to be tested at 180 ℃.
Intercepting an effective frequency range of 0.4-2.2THz for each absorption spectrogram, enabling CL-20 of different crystal forms to correspond to different fingerprint spectrums, comparing and analyzing the absorption spectrogram of each temperature node of a sample to be tested with epsilon-CL-20 and gamma-CL-20 absorption spectrograms obtained by a standard sample I and a standard sample II in the same coordinate system, wherein a graph 8 is an absorption spectrum comparison and analysis graph of the CL-20 sample to be tested at 25 ℃, a graph 9 is an absorption spectrum comparison and analysis graph of the CL-20 sample to be tested at 100 ℃, a graph 10 is an absorption spectrum comparison and analysis graph of the CL-20 sample to be tested at 140 ℃, and a graph 11 is an absorption spectrum comparison and analysis graph of the CL-20 sample to be tested at 180 ℃. And (5) carrying out characteristic absorption peak identification, and judging the crystal form of epsilon-CL-20, gamma-CL-20 or the mixed crystal form of epsilon-CL-20 or the gamma-CL-20 according with the frequency position and the absorption intensity of the characteristic absorption peak. The sample absorption peak frequency location statistics are shown in table 1.
TABLE 1
And (3) analysis results: the position and the intensity of the characteristic absorption peak of CL-20 to be detected at 25 ℃ completely accord with epsilon-CL-20, and the sample to be detected is in an epsilon crystal form. The characteristic absorption peak of CL-20 to be detected at 100 ℃ has red shift and weakened strength under the influence of temperature, but basically accords with epsilon-CL-20 and is an epsilon crystal form. The characteristic absorption peak of CL-20 to be detected at 140 ℃ also has red shift and weakening phenomena, and has an obvious rising trend at 1.5-1.6THz compared with the absorption spectrum at 100 ℃, and the characteristic absorption peak accords with the position of the characteristic absorption peak of gamma-CL-20, and at the moment, the main body of the sample is an epsilon crystal form but contains a small part of gamma crystal form. The CL-20 characteristic absorption peak to be detected at 180 ℃ accords with a gamma crystal form absorption spectrum, at the moment, the sample main body is in a gamma crystal form, but a slight bulge exists in 1.2-1.3THz, and trace epsilon crystal forms still exist.
Example 2:
this example is used to provide a nondestructive testing system for a crystal form of hexanitrohexaazaisowurtzitane, as shown in fig. 12, the testing system includes:
the terahertz spectrum acquisition module M1 is used for acquiring a terahertz spectrum of a sample to be detected;
the terahertz spectrum processing module M2 is used for processing the terahertz spectrum to obtain absorption coefficient data of the sample to be detected;
an absorption spectrogram drawing module M3, configured to draw an absorption spectrogram of the sample to be detected according to the absorption coefficient data;
the crystal form determination module M4 is used for acquiring absorption spectrograms of a plurality of standard samples; each of the standard samples is a crystal form of hexanitrohexaazaisowurtzitane; and comparing the absorption spectrogram of the sample to be detected with the absorption spectrogram of the standard sample to determine the crystal form of the sample to be detected.
The system of the embodiment belongs to the cross field of explosives and spectroscopy, applies the terahertz time-domain spectroscopy technology to the field of crystal form identification of typical single-substance explosive hexanitrohexaazaisowurtzitane (CL-20), realizes non-contact nondestructive detection of the CL-20 crystal form, overcomes the defect that the existing spectroscopy detection technology is too high in energy and can damage a test sample, and improves the detection safety. The obtained detection result has obvious characteristic difference, low resolution difficulty and good effect, is an excellent CL-20 crystal form identification spectroscopy method, and has important significance for improving the quality control of the CL-20 life cycle and the safety of the use process.
In the present specification, the embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. For the system disclosed by the embodiment, the description is relatively simple because the system corresponds to the method disclosed by the embodiment, and the relevant points can be referred to the method part for description.
The principle and the embodiment of the present invention are explained by applying specific examples, and the above description of the embodiments is only used to help understanding the method and the core idea of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (5)
1. A nondestructive testing method for a crystal form of hexanitrohexaazaisowurtzitane is characterized by comprising the following steps:
acquiring a terahertz spectrum of a sample to be detected;
processing the terahertz spectrum to obtain absorption coefficient data of the sample to be detected;
drawing an absorption spectrogram of the sample to be detected according to the absorption coefficient data; the absorption coefficient data is the absorption coefficient of the sample to be detected at each conversion point; the absorption spectrogram is a graph of the variation of the absorption coefficient along with frequency;
the step of drawing the absorption spectrogram of the sample to be detected according to the absorption coefficient data specifically comprises the following steps: smoothing the absorption coefficient data by using a Savitzky-Golay method to obtain smoothed absorption coefficient data; drawing an absorption spectrogram of the sample to be detected by using Origin according to the smoothed absorption coefficient data;
acquiring absorption spectrograms of a plurality of standard samples; each of the standard samples is a crystal form of hexanitrohexaazaisowurtzitane;
comparing the absorption spectrogram of the sample to be detected with the absorption spectrogram of the standard sample to determine the crystal form of the sample to be detected;
the step of comparing the absorption spectrogram of the sample to be detected with the absorption spectrogram of the standard sample to determine the crystal form of the sample to be detected specifically comprises the following steps: respectively intercepting the absorption spectrogram of the sample to be detected and the absorption spectrogram of the standard sample according to a preset frequency range to obtain an intercepted absorption spectrogram of the sample to be detected and an intercepted absorption spectrogram of the standard sample; comparing the intercepted absorption spectrogram of the sample to be detected with the intercepted absorption spectrogram of the standard sample, and determining the crystal form of the sample to be detected; specifically comparing the intercepted absorption spectrogram of the sample to be detected with the intercepted absorption spectrogram of the standard sample, performing characteristic absorption peak identification, and determining the crystal form of the sample to be detected; the preset frequency range is 0.4-2.0 THz;
the method for acquiring the terahertz spectrum of the sample to be detected specifically comprises the following steps: collecting a terahertz spectrum of the dry air by using a terahertz time-domain spectroscopy system; collecting a terahertz spectrum of a sample to be detected by using the terahertz time-domain spectroscopy system; when the terahertz time-domain spectroscopy system is used for collecting the terahertz spectrum of a sample to be detected, applying a preset environment temperature to the sample to be detected to obtain the terahertz spectrum of the sample to be detected at the preset environment temperature so as to determine the crystal form of the sample to be detected at the preset environment temperature; the crystal form is a single crystal form or a mixed state of a plurality of crystal forms;
when the environmental temperature is applied to a sample to be detected, and the terahertz spectrum of the sample to be detected is collected, firstly, the sample to be detected is placed on the innermost gasket of the contact type metal electric heating device, the cover layer of the electric heating device is rotated and sealed, the sample to be detected is not excessively extruded by the electric heating device, and then the electric heating device is placed at the terahertz wave focusing point of the Z-3 transmission type terahertz time-domain spectroscopy system, so that terahertz waves penetrate through the sample to be detected positioned at the light inlet window of the electric heating device;
the method comprises the steps of applying an environmental temperature to a sample to be detected through an electric heating device temperature rise controller on the periphery of a system, increasing the temperature by 10 ℃ at intervals of ten minutes in a stepped mode, observing the current actual sample temperature through the temperature rise controller, continuously waiting for ten minutes to ensure that the sample reaches the set temperature after the current temperature reaches the set temperature, storing the current terahertz time-domain spectral data through Z-3 transmission type terahertz time-domain spectroscopy system control software, and carrying out crystal form identification on the sample to be detected at different temperatures.
2. The nondestructive testing method for the crystal form of hexanitrohexaazaisowurtzitane according to claim 1, wherein the step of processing the terahertz spectrum to obtain the absorption coefficient data of the sample to be tested specifically comprises the following steps:
recording a terahertz spectrum of the dry air as a reference signal, and recording a terahertz spectrum of the sample to be detected as a sample signal;
performing fast Fourier transform on the reference signal and the sample signal respectively to obtain frequency domain reference data and frequency domain sample data;
and calculating the absorption coefficient data of the sample to be detected according to the frequency domain reference data and the frequency domain sample data.
3. The nondestructive testing method for the crystal form of hexanitrohexaazaisowurtzitane according to claim 2, wherein the calculating of the absorption coefficient data of the sample to be tested according to the frequency domain reference data and the frequency domain sample data specifically comprises:
calculating the amplitude ratio and the phase difference of each transformation point according to the frequency domain reference data and the frequency domain sample data;
and calculating the absorption coefficient of each transformation point according to the amplitude ratio and the phase difference to obtain the absorption coefficient data of the sample to be detected.
4. The method of claim 3, wherein the calculating the absorption coefficient at each transformation point according to the amplitude ratio and the phase difference comprises:
calculating the refractive index of each transformation point according to the phase difference;
and calculating the absorption coefficient of each transformation point according to the amplitude ratio and the refractive index.
5. A system for non-destructive testing of a crystalline form of hexanitrohexaazaisowurtzitane, comprising:
the terahertz spectrum acquisition module is used for acquiring a terahertz spectrum of a sample to be detected;
the terahertz spectrum processing module is used for processing the terahertz spectrum to obtain absorption coefficient data of the sample to be detected;
the absorption spectrogram drawing module is used for drawing an absorption spectrogram of the sample to be detected according to the absorption coefficient data; the step of drawing the absorption spectrogram of the sample to be detected according to the absorption coefficient data specifically comprises the following steps: smoothing the absorption coefficient data by using a Savitzky-Golay method to obtain smoothed absorption coefficient data; drawing an absorption spectrogram of the sample to be detected by using Origin according to the smoothed absorption coefficient data; the absorption coefficient data is the absorption coefficient of the sample to be detected at each conversion point; the absorption spectrogram is a graph of the variation of the absorption coefficient along with frequency;
the crystal form determining module is used for acquiring absorption spectrograms of a plurality of standard samples; each of the standard samples is a crystal form of hexanitrohexaazaisowurtzitane; comparing the absorption spectrogram of the sample to be detected with the absorption spectrogram of the standard sample to determine the crystal form of the sample to be detected;
the step of comparing the absorption spectrogram of the sample to be detected with the absorption spectrogram of the standard sample to determine the crystal form of the sample to be detected specifically comprises the following steps: respectively intercepting the absorption spectrogram of the sample to be detected and the absorption spectrogram of the standard sample according to a preset frequency range to obtain an intercepted absorption spectrogram of the sample to be detected and an intercepted absorption spectrogram of the standard sample; comparing the intercepted absorption spectrogram of the sample to be detected with the intercepted absorption spectrogram of the standard sample, and determining the crystal form of the sample to be detected; specifically comparing the intercepted absorption spectrogram of the sample to be detected with the intercepted absorption spectrogram of the standard sample, performing characteristic absorption peak identification, and determining the crystal form of the sample to be detected; the preset frequency range is 0.4-2.0 THz;
the method for acquiring the terahertz spectrum of the sample to be detected specifically comprises the following steps: collecting a terahertz spectrum of the dry air by using a terahertz time-domain spectroscopy system; collecting a terahertz spectrum of a sample to be detected by using the terahertz time-domain spectroscopy system; when the terahertz time-domain spectroscopy system is used for collecting the terahertz spectrum of a sample to be detected, applying a preset environment temperature to the sample to be detected to obtain the terahertz spectrum of the sample to be detected at the preset environment temperature so as to determine the crystal form of the sample to be detected at the preset environment temperature; the crystal form is a single crystal form or a mixed state of a plurality of crystal forms;
when the environmental temperature is applied to a sample to be detected, and the terahertz spectrum of the sample to be detected is collected, firstly, the sample to be detected is placed on the innermost gasket of the contact type metal electric heating device, the cover layer of the electric heating device is rotated and sealed, the sample to be detected is not excessively extruded by the electric heating device, and then the electric heating device is placed at the terahertz wave focusing point of the Z-3 transmission type terahertz time-domain spectroscopy system, so that terahertz waves penetrate through the sample to be detected positioned at the light inlet window of the electric heating device;
the temperature of a sample to be detected is applied by an electric heating device temperature rise controller on the periphery of the system, the temperature is increased by 10 ℃ every ten minutes in a step mode, the current actual sample temperature is observed by the temperature rise controller, when the current temperature reaches the set temperature, the sample is continuously waited for ten minutes to ensure that the sample reaches the set temperature, at the moment, the current terahertz time-domain spectroscopy data is stored by Z-3 transmission type terahertz time-domain spectroscopy system control software, and the crystal form identification can be carried out on the sample to be detected at different temperatures.
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