Rapid detection spectrum system for macroscopic parameters of energetic material
Technical Field
The invention relates to a rapid detection spectrum system for macroscopic parameters of an energetic material, and belongs to the field of energetic material detection.
Background
At present, novel high-performance energetic materials continuously emerge, different energetic materials need to be reasonably evaluated by detecting the explosion performance of the materials, the research means of the structure-activity relationship of the energetic materials is few at present, scientific instruments are absent, the research requirements of safe production and the materials are considered, the measurement and analysis of the energetic materials need a new method and a new device for rapid and real-time consumption of trace samples, and the wide requirements of rapid detection of explosive parameters and structure-activity relationship research are met. The basic parameters and information obtained by the interaction of laser and trace explosives are a good technical choice: therefore, higher requirements are provided for evaluation and research means of energetic materials and explosives, and a detection technology which is quicker, safe, reliable, simple and feasible is urgently needed to support rapid detection, performance evaluation and mechanism research of various energetic materials so as to fill up the industrial blank.
The macroscopic indexes measured in the invention comprise explosion velocity, laser sensitivity and element types and contents in the sample. The device comprises an igniter, a semi-closed exploder, a pressure relief sheet and other accessories, and a certain amount of tested propellant powder and an igniter charge are loaded into the semi-closed exploder with a copper sheet pressure relief sheet at the end port during the experiment. The semi-closed exploder is a test system for researching the pressure change rule of gunpowder when burning under the constant volume condition. The prior art method for measuring macroscopic performance parameters needs a large amount of samples and is completed by artificial explosion. The cost is extremely high, the controllability is poor, and the risk is strong; therefore, a rapid, safe and intelligent explosive evaluation and analysis system is urgently needed.
Disclosure of Invention
The invention aims to solve the problems that the performance evaluation of the existing high-performance energetic material needs a large amount of manual intervention of samples for measuring macroscopic indexes such as explosion speed, sensitivity and the like, and has high risk, poor controllability, low detection accuracy and the like, and provides a rapid detection spectrum system for macroscopic parameters of the energetic material.
The purpose of the invention is realized by the following technical scheme.
The system for rapidly detecting the macroscopic parameters of the energetic material comprises: the device comprises an LIPS light source, a closed air chamber, an LIPS spectrum collection system, a laser heterodyne interference speed measurement module, a gas detection module and a dynamic image acquisition module; the whole system is supposed to integrate all modules, and the relation between the laser spectrum and the explosive parameters is established through an intelligent algorithm, so that the rapid detection and the efficiency analysis of macroscopic performance parameters are realized.
Connection relation: a fifth laser window lens is arranged on the left side of the closed gas chamber and made of fused quartz, the transmission spectrum range is 190nm-2400nm, the position of a laser spot is positioned in the center of fused quartz glass, a focusing lens is arranged in front of a sample, and LIPS light source beams are focused on the sample to generate plasma; a sample is placed on an electric three-dimensional platform, the electric three-dimensional platform and the LIPS light source synchronously work, and the electric three-dimensional platform and the LIPS light source are triggered by one channel of a delay pulse generator; the LIBS spectrum collection system is connected with the Z-axis direction of the closed air chamber through a flange plate and comprises a double-lens collection mirror group, an optical fiber, a spectrometer and a computer. A dynamic image acquisition module is arranged in the positive X-axis direction of the closed air chamber, a third window lens is arranged on the surface of the closed air chamber in the positive X-axis direction, and an ICCD24 is used for acquiring dynamic images; the laser heterodyne interference speed measurement method is characterized in that a laser heterodyne interference speed measurement module is arranged in the negative X-axis direction of a closed air chamber, the incident direction of a 632.8nm laser is the positive X-axis direction, a first half-mirror is arranged in front of the laser, a laser beam is divided into two vertical beams, one beam is a detection light, the other beam is a reference light, an avalanche diode is added at the position where the detection light and the reference light are converged, and the signal of the avalanche diode is connected into an oscilloscope. The gas detection module is externally connected with a vacuum six-way flange detection cavity, the detection cavity is formed by splicing the vacuum six-way flanges, the length of the detection cavity can be changed according to requirements, one detection cavity is provided with an electrochemical gas sensing array module, sensors are annularly arranged in a flange plate, and the flange plate can be connected with the vacuum six-way flange; the sample chamber is connected with the molecular pump through a stainless steel vacuum tube, a pressure gauge and a vacuum valve are arranged on the vacuum tube, the vacuum degree of the whole device can be observed and controlled, the lower part of the sample chamber is provided with an air inlet, and the upper part of the sample chamber is provided with an air outlet which can be used for discharging gas products; the gas sensor is externally connected with a display screen and used for displaying the gas concentration in real time.
The LIPS spectrum collection system collects plasma induced by LIPS light source irradiating on a sample in real time, then the plasma is coupled into an optical fiber through a double-lens collection mirror group, and the optical fiber is transmitted to a spectrometer to obtain a spectrum, so that the content of elements in the sample is quantitatively analyzed;
the double-lens collecting lens group is connected by adopting a dragon type structure;
the sealed gas chamber is filled with sample, vacuum space, and protective gas such as He and N2Ar, protecting the sample;
the laser heterodyne interference speed measurement module is used for indirectly measuring the speed of laser induced shock waves by measuring the shock wave disturbance on the surface of a sample after the LIPS light source acts on the energetic material;
the heterodyne interference speed measurement module comprises a 632.8nm laser which is synchronously triggered with the LIPS light source, and 2 mu s delay time is set between the two lasers so as to ensure that the 632.8nm laser acts on the shock wave disturbance of the plasma after the LIPS light source acts on a sample to generate the plasma;
the dynamic image acquisition module comprises an ICCD (integrated compact disc), can realize high-resolution image display of laser-induced plasma wing and sample ablation conditions, so as to perform nanosecond-level time-resolved image display of substance plasma, and is used with a laser heterodyne interference speed measurement module to measure the laser-induced shock wave speed so as to obtain detonation velocity information;
the airtight air chamber is the square structure who has transparent window, and transparent window includes: a first window lens, a second window lens, a third window lens, a fourth window lens and a fifth window lens; the sample is fixedly arranged on the electric three-dimensional table; the LIPS light source irradiates the surface of the sample through a fifth window lens and a focusing lens; the second reflector reflects the 632.8nm laser beam acting on the disturbance to the second half-mirror; the second half mirror has two functions, wherein the first function is to transmit the light reflected by the second mirror to the avalanche diode with the rising edge of 30ps ultrafast response after transmitting the light, record voltage signals, and the light path of the light is signal light, and the second function is to reflect the 632.8nm laser to the first mirror through the first half mirror, then to the second half mirror, and then to the avalanche diode, and the light is used as reference light;
the gas detection module includes: the device comprises a stainless steel vacuum tube, a vacuum valve, a gas pressure gauge, an electrochemical gas sensing array module and a vacuum six-way flange detection cavity; the closed air chamber is connected with the molecular pump through a stainless steel vacuum tube, a pressure gauge and a vacuum valve are arranged on the vacuum tube, the vacuum degree of the whole device can be observed and controlled, an air inlet is arranged at the lower part of the sample chamber, an air outlet is arranged at the upper part of the sample chamber, and the sample chamber can be used for exhausting gas products;
the electrochemical sensor is not triggered to work, but is turned on at the beginning of the test, so that the sensor is always in a working state;
the intelligent algorithm is based on partial differential least squares (PLS) combined with a Principal Component Analysis (PCA) model, improves detection precision and measurement repeatability by utilizing wavelet transformation and a neural network algorithm, reduces detection limit, extracts effective spectral data characteristic quantity by utilizing machine learning and an artificial intelligent algorithm (an artificial neural network and a tree algorithm), establishes the relation between a laser spectrum and explosive parameters (element content and macroscopic detonation parameters), calculates by using a first principle and corrects the data model by using a C-J equation, and obtains a reasonable detonation velocity and sensitivity prediction algorithm;
the detection process is as follows:
the first step is as follows: opening the vacuum valve, starting the molecular pump to pump vacuum, and displaying the current vacuum degree of 10 by the gas pressure gauge- 3When pa, the vacuum valve and the molecular pump are closed, and the whole system can keep the current vacuum degree for 2 hours;
the second step is that: turning on a delay pulse generator, an LIPS light source, a 632.8nm laser, an ICCD, an avalanche diode, an oscilloscope, an electrochemical gas sensing array module and an electric three-dimensional platform, adjusting the delay pulse generator to be in an internal trigger mode, and adjusting the rest instruments to be in an external trigger mode;
the third step: starting a delay pulse generator, and enabling an LIPS light source to emit a beam of pulse laser to vertically hit the surface of a sample to generate plasma and a sample decomposition product;
the fourth step: measuring the state of the energetic material under different energies by adjusting the LIPS light source energy; the plasma light is received by the double-lens collection mirror group and transmitted to the spectrograph through the optical fiber, and real-time spectrum display is obtained on the computer. Meanwhile, the ICCD in the dynamic image acquisition module starts to work to shoot laser plasma wings in different time states, computer image display is carried out, and the excitation state is analyzed. The gas sensing module is always in a working state, the types and the concentrations of gases at different positions are respectively recorded, and the laser heterodyne interference module measures shock wave disturbance;
the fifth step: and analyzing the acquired spectral data, plasma images, oscilloscope data and the state of the energetic material under different energies to obtain the content of energetic material elements, the types of energetic material elements, the explosion velocity of the energetic material, the laser sensitivity of the energetic material and the time-resolved gas product of the energetic material.
Advantageous effects
1. According to the invention, the LIPS light source acts on the energetic material to induce detonation, the macroscopic detonation parameters are obtained through the micro-region spectrum and the dynamic spectrum image, the rapid and intelligent measurement of the explosion parameters is realized by utilizing the laser-induced detonation micro-region spectrum technology, the quantitative relation between the components and the explosion parameters can be synchronously obtained, and a basis is provided for the performance improvement of the energetic material. The system integrates an LIPS spectrum collection system, a gas detection module, a laser heterodyne interference speed measurement module and the like, and establishes the relation between the laser spectrum and the explosive parameters through an intelligent algorithm to realize the rapid detection and the efficiency analysis of the explosive parameters. The novel method and the intelligent test analysis system are simple, easy, safe and reliable and are provided for the research and parameter test of energetic materials.
2. According to the system for rapidly detecting and analyzing the macroscopic performance parameters of the energetic material based on the micro-area laser induced detonation spectroscopy technology, the vacuum flange is used as a device component, the research on the gas product of the energetic material under high vacuum degree can be realized, the assembling characteristic of the experimental device is increased, the experimental device can be improved according to specific experimental requirements, and the application is wider.
Drawings
FIG. 1 is a schematic diagram of a system for rapidly detecting macroscopic performance parameters of energetic materials based on micro-region laser-induced detonation spectroscopy technology according to the present invention;
FIG. 2 is a schematic diagram of a gas detection module;
FIG. 3 is a schematic diagram of a laser heterodyne interferometric velocity module;
FIG. 4 is a schematic diagram of a LIPS spectral collection system;
FIG. 5 is a schematic view of a closed gas cell;
fig. 6 is a schematic diagram of a dynamic image acquisition module.
Wherein, 1-stainless steel vacuum tube, 2-vacuum valve, 3-gas pressure gauge, 4-electrochemical gas sensing array module, 5-vacuum six-way flange detection cavity, 6-first module cavity, 7-632.8nm laser, 8-first semi-transparent semi-reflecting mirror, 9-first reflecting mirror, 10-second module cavity, 11-double lens collecting mirror group, 12-spectrometer, 13-airtight gas chamber, 14 first window lens, 15-electric three-dimensional stage, 16-second reflector, 17-second window lens, 18-third window lens, 19-avalanche diode, 20-second half-mirror, 21-fourth window lens, 22-fifth window lens, 23-focusing lens, 24-ICCD, 25-LIPS light source.
Detailed Description
The invention is further described with reference to the following figures and examples.
Example 1
The system for rapidly detecting the macroscopic parameters of the energetic material comprises: the device comprises an LIPS light source 1, a closed air chamber 2, an LIPS spectrum collection system 3, a laser heterodyne interference speed measurement module 4, a gas detection module 5 and a dynamic image acquisition module 6; the whole system is supposed to integrate all modules, and the relation between the laser spectrum and the explosive parameters is established through an intelligent algorithm, so that the rapid detection and the efficiency analysis of macroscopic performance parameters are realized.
Connection relation: on the left side of the closed gas cell is a fifth window 22, the laser spot is located in the center of the window, a focusing lens 23 is placed in front of the sample to focus the LIPS light source 25 beam on the sample to generate plasma. The sample is placed on an electric three-dimensional table 15, works synchronously with an LIPS light source, and is connected with an LIBS spectrum collection system through a flange plate in the Z-axis direction of a closed air chamber, wherein the system comprises a double-lens collection mirror group 11, a spectrometer 12, an optical fiber and a computer. A dynamic image acquisition module is arranged in the positive X-axis direction of the closed air chamber, a third window lens 18 is arranged on the surface of the closed air chamber in the positive X-axis direction, and an ICCD24 is used for acquiring dynamic images; the laser heterodyne interference speed measurement module is arranged in the negative X-axis direction of the closed gas chamber, the incident direction of the laser is the positive X-axis direction, the first half-mirror 8 is arranged in front of the laser, the laser beam is divided into two vertical beams, one beam is a detection beam and the other beam is a reference beam, the avalanche diode 19 is added at the convergence position of the detection beam and the reference beam, and the signal of the detector is connected into the oscilloscope. The electrochemical gas sensor array module 4 is externally connected with a vacuum six-way flange detection cavity 5, the length of the detection cavity can be changed according to requirements, sensors in the electrochemical gas sensor array module are annularly arranged in a flange plate, and the flange plate can be connected with a vacuum six-way flange; the sample chamber is connected with the molecular pump through a stainless steel vacuum tube 1, a pressure gauge 3 and a vacuum valve 2 are arranged on the vacuum tube, the vacuum degree of the whole device can be observed and controlled, the lower part of the sample chamber is provided with an air inlet, and the upper part of the sample chamber is provided with an air outlet, so that gas products can be discharged; the electrochemical gas sensing array module is externally connected with a display screen and is used for displaying the gas concentration in real time. The instrument timing control is performed by a time delay pulse generator.
The sample chamber is a closed chamber, and the volume of the sample chamber is 300mm multiplied by 400 mm; the device is provided with a flow meter and a pressure gauge, and can be used for measuring laser-induced plasma spectra in different buffer gases and pressure environments;
the electric three-dimensional table is placed in the closed air chamber, a sample table with an aluminum plate as a base is placed on the translation table, and a sample is placed on the sample table;
the laser window is made of fused quartz, and the transmitted spectral range can reach 190nm-2400 nm;
the outer size of the vacuum six-way flange detection cavity is a cube with the side length of 100mm, and the inner part of the vacuum six-way flange detection cavity is a cylindrical ventilation pipeline with the diameter of 50mm and the length of 50 mm;
the rotating speed of the molecular pump can reach nine ten thousand revolutions, and the vacuum degree of the sample chamber can be pumped to 10-3Pa, after the vacuum valve is closed, the whole device can keep the current vacuum degree for 2 h;
the time sequence control of the instrument is carried out through a delay pulse generator, four channels of the delay pulse generator are respectively connected with an LIPS light source, a spectrometer in an LIPS spectrum collection system, a 632.8nm laser in a laser heterodyne interference speed measurement module and a dynamic image acquisition module, a trigger signal is TTL, the load is 50 ohms, and the delay between the LIPS light source and the spectrometer is set to be 190 microseconds;
the avalanche diode is connected with a power supply for amplifying an electric signal, and the power supply is direct current 5V. Inputting the signal of the avalanche diode to an oscilloscope by using a BNC wire for displaying;
the ICCD camera for collecting the dynamic images adopts an external trigger mode, the resolution is 1024 multiplied by 256, the minimum set gate width is 2ns, and the ICCD camera is controlled and integrated by software, so that the high-resolution image display of the laser-induced plasma wing and the sample ablation condition can be realized, and the nanosecond-level time resolution image display of the material plasma can be realized;
the LIPS light source adopts Nd: YAG pulse laser with laser wavelength of 1064nm and pulse width of 7ns and single pulse laser energy of 50-250mJ @1064 nm. The high-resolution spectrometer system comprises a CCD detector, a blazed grating, a pulse trigger circuit, a signal receiving circuit and spectrometer software. The spectral range is 180nm-980nm, the resolution is less than 0.1nm, the minimum gate width integral setting time is 1ms, and the delay is adjustable.
The working process is as follows: placing the sample on an electric three-dimensional table with a closed air chamber of 300mm multiplied by 400mm, opening the
vacuum valve 2, starting the molecular pump to vacuumize, and displaying that the current vacuum degree is 10 when the
pressure gauge 10 displays that the current vacuum degree is 10
-3pa, the
vacuum valve 2 and the molecular pump are closed, and the whole system can keep the current vacuum degree for 2 hours. Opening a delay pulse generator, adjusting the trigger mode of an instrument to an internal trigger mode, wherein the frequency is 1Hz, 4 channels of the delay pulse generator are respectively connected with an LIPS light source, a 632.8nm laser, a spectrometer and an ICCD, an electric platform trigger line is connected to the LIPS light source trigger line by a tee joint, the two instruments are synchronously triggered, the LIPS light source adopts high-level triggering, and an electric three-dimensional platform adopts low-level triggering to ensure the coordinated operation of the machine; wherein the 632.8nm laser power is 20mW, and the LIPS light source adopts Nd: YAG pulse laser with laser wavelength of 1064nm and pulse width of 7 ns. The laser light passes through a
fifth window lens 22 at the right side of the sample chamber and is convergedAnd a
mirror 23 which is vertically incident on the sample, wherein the position of the converging
lens 23 is adjusted to ensure that the laser is just focused on the sample, and the sample is decomposed or excited by heat to generate a gas product. Gas products are gradually diffused into the detection cavity formed by connecting the vacuum six-way flanges on the right side of the closed air chamber through diffusion movement, an electrochemical gas sensor is arranged between every two adjacent vacuum six-way
flange detection cavities 5, and a response signal of the electrochemical gas sensor array is recorded and displayed by a computer. The sensor modules continuously diffusing gas respond in sequence, and the record shows that the response time of the first group of sensor modules is t1, the response time of the second group of sensor modules is t2, and the distance between the two groups of sensor modules is L1, so that the diffusion speed is
Besides, the specific composition and concentration information of the gas product can be qualitatively and quantitatively obtained through the type of the responding electrochemical sensor. The LIPS light source is focused on a sample to generate plasma, the plasma spectrum is collected through a double-lens
collection mirror group 11 and transmitted to a
spectrometer 12 through an optical fiber to obtain a spectrogram, and the element types and the element contents in the spectrum are obtained through an algorithm; the laser emitted by the 632.8nm laser in the synchronously-started laser heterodyne interference velocity measurement module irradiates the shock wave disturbance of the plasma, is reflected to the second half mirror through the second reflecting
mirror 16, transmits the signal light to the
avalanche diode 19, and reflects the other beam of reference light to the first reflecting
mirror 9 through the
first half mirror 8, then reflects the reference light to the
second half mirror 20, and reflects the reference light to the
avalanche diode 19. Finally, the reference light and the signal light are received by the avalanche diode and displayed on an oscilloscope; the dynamic acquisition module is used together with the LIPS technology and the laser heterodyne interference technology to measure the laser induced shock wave speed, so that detonation speed information is obtained.
The above detailed description is intended to illustrate the objects, aspects and advantages of the present invention, and it should be understood that the above detailed description is only exemplary of the present invention and is not intended to limit the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.