A combustion reaction cell array for studying the ignition performance of energetic materials and its application

Abstract

The present invention discloses a combustion reaction pool array for studying the ignition performance of energetic materials and its application. A carrier is provided, and a plurality of pits are provided on the carrier in an array distribution; the diameter of the pits is at least 2 to 10 times the diameter of the sample particles, so that each pit can accommodate 2 to 10 sample particles. Compared with the commonly used milligram-level powder pile laser ignition, the combustion reaction pool array of the present invention can control the number of particles in the sample particle pile, and when conducting laser ignition and combustion mechanism research, the interaction between particles can be clearly observed; the number of particles in the particle pile can be limited by controlling the pit size in the pit array to avoid triggering an explosion, which is convenient for observing the combustion characteristics of the sample particle energy release process and its interaction form, and can also restrain the sample particles, which is conducive to observing the characteristics of the entire combustion process of the sample.

Description

Technical Field

[0001] The invention belongs to the technical field of energetic material testing, and in particular relates to a combustion reaction pool array for studying the ignition performance of an energetic material pile and an application thereof. Background Art

[0002] The energy release of energetic materials is mainly carried out through two ways: combustion and explosion, which directly determine the energy level of energetic materials. Among them, the utilization of energetic materials combustion energy release involves many applications, such as rocket propellants, gun propellants, pyrotechnics, and automotive safety gas devices. In-depth understanding of the combustion characteristics of energetic materials and the exploration of the physical changes and chemical reaction mechanisms of materials during the combustion process are of great significance for understanding the characteristics of energetic materials combustion energy release, revealing the relationship between the composition, structure and performance of energetic materials, and designing and developing new energetic materials. During the combustion process, solid energetic material particles not only interact with the gas phase, but also have a strong particle group effect, such as particle agglomeration and sintering. In order to deeply reveal the interaction of particle groups and the combustion mechanism during the combustion process, it is necessary to study the ignition and combustion performance of several solid fuel particle piles that are easy to spatially resolve, which is of great significance for characterizing the properties of energetic materials and evaluating their combustion performance.

[0003] At present, laser ignition experiments on energetic materials are mainly divided into powder pile laser ignition and single particle laser ignition. In powder pile laser ignition experiments, milligram-level powder samples are often gathered together, and then a laser beam is focused on the surface of the powder pile to carry out laser ignition experiments to study the particle group interaction and combustion mechanism of solid energetic material particles in the form of powder piles. However, the problems with using powder pile samples to study combustion performance and mechanism are: 1) The powder pile is composed of tens of thousands of sample particles. When conducting laser ignition research on powder samples, it is difficult to clearly observe the interaction between particles; 2) Laser ignition experiments on energetic material powder piles often cause explosions due to the excessive concentration of energy inside the powder pile due to the simultaneous release of energy by a large number of sample particles, which is not conducive to observing the combustion characteristics of the sample particle energy release process and its interaction form. At the same time, the explosion will cause the sample to fly away, resulting in incomplete ignition and combustion reactions, making it difficult to observe all the characteristics of the sample combustion process; 3) Currently, laser ignition experiments are often carried out on milligram-level energetic material samples, but due to their stacking method and the sample container in the experiment, the specific number of samples involved in the ignition and combustion process is difficult to accurately quantify; 4) Because the number of samples in the ignition and combustion process is difficult to accurately quantify, the combustion product is a mixture of the original sample and the combustion product. Experimental analysis of the combustion product may lead to incorrect conclusions, and it is also impossible to correspond the combustion products of the energetic material with the phenomena in its combustion process. Summary of the invention

[0004] Based on the above-mentioned purpose, the present invention provides a combustion reaction pool array and its application for studying the ignition performance of energetic materials, which solves the problems that it is difficult to clearly observe the interaction between particles in the existing research on the ignition performance of energetic material particle piles, it is difficult to accurately quantify the amount of samples participating in the combustion process, and it is impossible to correspond and associate the combustion products of the energetic material powder pile with the phenomena in its combustion process.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] A combustion reaction pool array for studying the ignition performance of energetic materials comprises a carrier on which a plurality of pits are arranged in an array; the diameter of the pits is at least 2 to 10 times the diameter of the sample particles, so that each pit can accommodate 2 to 10 sample particles.

[0007] Optionally, the interval between adjacent pits is 1 μm to 1000 μm, the pore size of the pits is 1 μm to 1000 μm, and the depth of the pits is 500 nm to 500 μm.

[0008] Optionally, the pit is a circular pit.

[0009] Optionally, the carrier is a glass slide, which is rectangular, 5 to 10 cm long, 1 to 3 cm wide, and 0.5 to 1.5 mm thick, and the array-distributed pits are arranged at the center of the glass slide.

[0010] The combustion reaction pool array for studying the ignition performance of energetic materials described in any one of the present invention is used for studying the ignition performance of energetic material particle piles.

[0011] Optionally, the method includes the following steps:

[0012] Step 1, loading sample particles into the pits, with one pit containing more than two sample particles;

[0013] Step 2, positioning and marking the particle pile sample in the pit under a scanning electron microscope;

[0014] Step 3, performing laser focusing and ignition tests on the particle pile sample under an optical microscope, and using a high-speed camera to record the combustion reaction process of the particle pile sample;

[0015] Step 4, after completing the ignition test, perform morphological analysis and energy spectrum detection on the combustion products in the pits under a scanning electron microscope to obtain the morphological structure and chemical composition of the combustion products, and match the combustion process of the particle pile sample with the combustion products according to the pit marks in step 2.

[0016] Optionally, the number of sample particles is 2 to 10.

[0017] Optionally, step 1 specifically includes: taking sample particles, scattering them on the carrier at the positions where pits are arranged in an array, taking another carrier, contacting one side of the carrier with the sample carrier, and moving in a square along the length of the sample carrier, removing excess sample particles on the surface of the sample carrier, and leaving only the sample particles in the pits, with 2 to 10 sample particles left in one pit.

[0018] Optionally, the step 2 specifically includes: sending the carrier processed in step 1 into a scanning electron microscope sample chamber, finding pits with 2 to 10 sample particles by observing the pit morphology under a high-magnification field of view, and marking the positions of these pits;

[0019] Optionally, step 3 specifically includes: placing the marked combustion reaction pool array under a microscope, adjusting the focal length of the microscope to make the sample particles in the pits clearly imaged, adjusting the laser power according to the laser ignition test steps, turning on the laser to perform a laser ignition test on the sample particles, and using a high-speed camera to record the combustion reaction process.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] (1) Compared with milligram-level powder piles, the combustion reaction pool array of the present invention can control the number of particles in the sample particle pile, and can clearly observe the interaction between particles when conducting laser ignition and combustion mechanism research.

[0022] (2) In the present invention, the number of particles in the particle pile is limited by controlling the size of the pits in the pit array, thereby avoiding the explosion phenomenon, making it easier to observe the combustion characteristics of the sample particle energy release process and their interaction forms. At the same time, the sample particles can be bound, which is beneficial to observing the overall combustion process characteristics of the sample.

[0023] (3) In the present invention, the number of particles in the particle pile is limited by controlling the size of the pits in the pit array, so that the number of samples participating in the ignition and combustion process can be accurately quantified;

[0024] (4) By marking the pits, the combustion process of the energetic material particle pile can be analyzed, and the microstructure observation and chemical composition analysis of the specific position of the combustion products corresponding to the particle pile can be realized. This is conducive to the corresponding correlation analysis of the combustion products of the energetic material particle pile and the phenomena in its combustion process, and further reveals the combustion mechanism of the energetic material particle pile combustion process. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] The accompanying drawings are used to provide a further understanding of the present disclosure and constitute a part of the specification. Together with the following specific embodiments, they are used to explain the present disclosure but do not constitute a limitation of the present disclosure. In the accompanying drawings:

[0026] Figure 1 It is a schematic diagram of the structure of a glass slide etched with a combustion reaction pool array according to an embodiment of the present invention;

[0027] Figure 2 It is a structural schematic diagram of a combustion reaction pool array recorded in an embodiment of the present invention;

[0028] Figure 3 is a SEM image of the pit array of the energetic material particle pile laser ignition combustion reaction pool described in Example 2 of the present invention;

[0029] Figure 4 It is an optical microscope image of a sample particle pile of a single pit in the laser ignition pit array of the energetic material particle pile recorded in Example 2 of the present invention;

[0030] Figure 5 This is a SEM image of a sample particle pile combustion product of a single pit in the energetic material particle pile laser ignition pit array as described in Example 2 of the present invention;

[0031] Figure 6 is the EDS spectrum of the sample particle pile combustion product of a single pit recorded in Example 2 of the present invention;

[0032] Figure 7 This is a diagram of the laser ignition process of the energetic material particle pile described in Example 2 of the present invention;

[0033] Figure 8 This is a diagram of the laser ignition process of a milligram-scale powder pile. DETAILED DESCRIPTION

[0034] The "sample particles" in the present invention refer to particles of energetic materials to be ignited.

[0035] In the present invention, "the pit diameter is at least 2 to 10 times the diameter of the sample particles" means that the pit diameter is larger than the maximum diameter of the sample particles, so that 2 to 10 sample particles can be accommodated in the pit. When the sample particles have different diameters and are irregular in shape, the pit diameter is about 2 to 10 times the average diameter of the sample particles.

[0036] The present invention first discloses a combustion reaction pool array for studying the ignition performance of energetic materials, which is mainly used to study the ignition performance of energetic material particle piles. The combustion reaction pool array is located on the surface of a glass slide, and a plurality of pits are arranged on the glass slide. The pits have a certain depth but do not penetrate along the thickness of the glass slide, and the pit diameter is at least 2 to 10 times the diameter of the sample particles, so that each pit can accommodate 2 to 10 sample particles. Compared with the commonly used milligram-level powder pile laser ignition, the combustion reaction pool array of the present invention can control the number of particles in the sample particle pile, and when conducting laser ignition and combustion mechanism research, the interaction between particles can be clearly observed; the number of particles in the particle pile can be limited by controlling the pit size in the pit array to avoid causing explosions, which is convenient for observing the combustion characteristics and interaction forms of the sample particle energy release process, and at the same time, the sample particles can be bound, which is conducive to observing the characteristics of the entire combustion process of the sample; the number of samples specifically involved in the ignition and combustion process can be accurately quantified; by marking the pits, the combustion process analysis of the energetic material particle pile and the microstructure observation and chemical composition analysis of the specific position of the combustion product corresponding to the particle pile can be realized. It is helpful to conduct corresponding correlation analysis between the combustion products of energetic material particle piles and the phenomena in their combustion process, and further reveal the combustion mechanism of the energetic material particle pile combustion process.

[0037] In the present disclosure, multiple pits are distributed in an array for easy positioning. The pit diameter is 1 μm to 1000 μm, the pit depth is 500 nm to 500 μm; the spacing between adjacent pits is 1 μm to 1000 μm. If the spacing is too close, the combustion products in the adjacent pits will interfere with each other; if the spacing is too large, optical microscope observation is inconvenient and positioning is difficult.

[0038] Best is to mark the pits distributed in the array. The specific method is: etching a number on each pit in the first row and each pit in the first column of the pit array. For example, in the following embodiment of the present invention, it is a 10*10 pit array, so it is marked as 1, 2, 3,...10, so that each pit is numbered: 1-1, 1-2,..., 1-10; 2-1, 2-2,..., 2-10; ...; 10-1, 10-2,..., 10-10.

[0039] In the present disclosure, the pit is circular. On the one hand, the circular shape is more adaptable to the shape of sample particles, that is, it is convenient for different shapes, and on the other hand, it is convenient for processing.

[0040] In the present disclosure, the pits are prepared by laser / chemical induced etching rapid prototyping technology; similarly, the marks are also formed by laser / chemical etching technology. After the pit etching is completed, the entire slide is placed in an organic solvent such as acetone for ultrasonic cleaning and then blown dry. The laser uses a focused ultraviolet laser and a fiber laser with high beam quality.

[0041] In the present disclosure, the glass slide is rectangular, 5 to 10 cm long, 1 to 3 cm wide, and 0.5 to 1.5 cm thick, so as to be easily matched with the sample stage of an electron scanning microscope; the plurality of pits are arranged at the center of the glass slide.

[0042] The glass slide of the present invention is made of a light-transmitting glass sheet, preferably borosilicate glass or quartz, which has good high temperature resistance and is not easily damaged when the energetic material burns.

[0043] The combustion reaction pool array of the present invention can be used for combustion performance tests of all energetic material particle piles and the like.

[0044] The present invention also discloses the application of the combustion reaction pool array for laser ignition of energetic material particle piles. The reaction pool array is used for laser ignition combustion performance testing of energetic material particle piles. The specific process includes the following steps:

[0045] Step 1, loading sample particles into the pits on the glass slide, wherein there are more than 2 sample particles in one pit, and 2 to 10 particles are optimal;

[0046] Step 2, positioning and marking the particle pile sample in the pit under a scanning electron microscope;

[0047] Step 3, performing laser focusing and ignition tests on the particle pile sample under an optical microscope, and using a high-speed camera to record the combustion reaction process of the particle pile sample;

[0048] Step 4, after completing the ignition test, perform morphological analysis and energy spectrum detection on the combustion products in the pits under a scanning electron microscope to obtain the morphological structure and chemical composition of the combustion products, and match the combustion process of the particle pile sample with the combustion products according to the pit marks in step 2.

[0049] In the present disclosure, step 1 specifically includes: taking sample particles, sprinkling them on the position where the pit is set on the slide, taking another slide, contacting one side of it with the sample slide, and moving it in a square along the length of the sample slide, removing excess sample particles on the surface of the sample slide, leaving only the sample particle pile in the pit, so that there are about 2 to 10 sample particles left in one pit.

[0050] In the present disclosure, step 2 specifically includes: sending the sample stage processed in step 1 into the sample chamber of the scanning electron microscope, observing the pit morphology under the high-magnification field of view, finding pits with only about 2 to 10 sample particles, and marking the positions of these pits.

[0051] It should be noted that if the sample is not conductive, the glass slide containing the sample needs to be gold-sprayed before being placed into the sample chamber of the scanning electron microscope.

[0052] In the present disclosure, step 3 specifically includes: placing the combustion reaction pool array under a microscope, adjusting the focal length of the microscope to make the particle pile in the pit clearly imaged, adjusting the laser power according to the laser ignition test steps, turning on the laser to perform a laser ignition test on the particle pile sample, and using a high-speed camera to record the combustion reaction process.

[0053] Specific embodiments of the present invention are given below. It should be noted that the present invention is not limited to the following specific embodiments, and all equivalent changes made on the basis of the technical solution of this application fall within the protection scope of the present invention.

[0054] Embodiment 1:

[0055] The combustion reaction pool array disclosed in this embodiment for studying the ignition performance of energetic material particle piles, such as Figure 1 and Figure 2 As shown, the sample stage includes a glass slide, which is made of quartz and has a thickness of 0.5 mm. A pit is processed at the center of the glass slide by laser / chemical induced etching rapid prototyping technology. The pits of this embodiment are distributed in an array to form a 10*10 pit array, each pit is a circular hole, the aperture of the pit is 300 μm, the depth of the pit is 100 μm, and the spacing between adjacent pits is 200 μm.

[0056] At the same time, numbers 1, 2, 3, ... 10 are etched on each pit in the first row and each pit in the first column of the pit array for marking, such as Figure 2 As shown, each pit is numbered as follows: 1-1, 1-2, …, 1-10; 2-1, 2-2, …, 2-10; …; 10-1, 10-2, …, 10-10.

[0057] After the pit processing is completed, the glass slide is ultrasonically cleaned with acetone solvent for 10 minutes, and finally a combustion reaction pool array for studying the ignition performance of energetic material particle piles is obtained.

[0058] The hole diameter and hole depth of the pit of the sample stage of the present invention can be adjusted according to the average particle diameter of the sample particles, and are not limited to the above-mentioned embodiment.

[0059] Embodiment 2:

[0060] The experimental method for studying the ignition performance of energetic material particle pile disclosed in this embodiment uses the glass slide with a combustion reaction pool array on the surface as described in Example 1 as the sample stage of this experiment. The energetic material in this embodiment is AlH3 powder, and the average particle size D of the AlH3 powder is 50 =47μm. The test process specifically includes:

[0061] Step 1: Load sample particles into the pits on the slide, and there are 2 to 10 sample particles in one pit, specifically:

[0062] Take AlH3 powder particles with a spoon and evenly sprinkle them on the pit array position in the center of the sample stage. Lightly knock the sample stage against the table to ensure that the sample particles fall into the pits. Then take another slide, put one side of it in contact with the sample slide, and move it along the length of the sample slide in a square shape to remove the excess sample particles on the surface of the sample slide, leaving only the sample particles in the pits, so that there are about 2 to 10 sample particles in one pit. Figure 1 It is a pile of AlH3 particles in a single pit of the pit array, with 3 to 5 particles and a roughly square shape.

[0063] Step 2: Position and mark the single particle sample in the pit under a scanning electron microscope, specifically:

[0064] The reaction pool array slide containing the sample is sprayed with gold and sent into the sample chamber of the scanning electron microscope. By observing the pit morphology under the high-magnification field of view, the position of the pit with only one sample particle is marked, and the sample is positioned and marked by numbering each pit in the pit array 1-1, 1-2, ..., 1-10; 2-1, 2-2, ..., 2-10; ...; 10-1, 10-2, ..., 10-10.

[0065] like Figure 3 This is a scanning electron microscope image of a pit array slide. The position of the sample particles in each pit can be calibrated based on the above numbers.

[0066] Step 3: Perform laser focusing and ignition tests on single particle samples under an optical microscope, and use a high-speed camera to record the combustion process of the particle pile sample, specifically:

[0067] Place the glass slide under an optical microscope for an ignition test. According to the pit mark in step 2, adjust the focal length to make the image of the AlH3 particle pile sample in the pit clear. According to the laser ignition test steps, adjust the laser power, turn on the laser to perform a laser ignition experiment on the particle pile sample, and use a high-speed camera to record the combustion process.

[0068] Figure 7 This is the laser ignition process of the AlH3 sample in this embodiment. The figure shows the complete combustion process of the AlH3 sample particle pile, from particle ignition, to the formation of a diffusion flame (35.2ms), adjacent sample particles gradually ignite, aggregate-merge-melt (35.6~38.4ms), until finally forming spherical combustion particles (39.4~41ms). The interaction between the sample particles during the laser ignition process can be clearly observed.

[0069] Figure 8The figure shows the laser ignition process of a milligram-level AlH3 powder pile. The figure shows a violent jet combustion flame of the powder pile. The reason is that during the laser heating process, AlH3 releases hydrogen, which causes the internal pressure of the particles to increase. The released hydrogen burns and explodes to produce a jet airflow, and the AlH3 sample particles fly out of the sample powder pile container. During this combustion process, it is difficult to clearly observe the interaction between the particles, and it is also difficult to determine the amount of sample actually participating in the combustion reaction.

[0070] Step 4, after completing the ignition test, the glass slide containing AlH3 is sent back into the scanning electron microscope sample chamber, and the morphology analysis and energy spectrum detection of the combustion products in the pits are performed under a scanning electron microscope to obtain the morphology structure and chemical composition of the combustion products, and the combustion process of the particle pile sample is matched with the combustion products according to the pit marks in step 2.

[0071] Figure 5 This is a morphological structure diagram of the AlH3 particle pile combustion product of this embodiment, Figure 6 This is the EDS elemental analysis spectrum of the combustion product. It can be seen from the figure that the O element (wt%) is less than 40%, which is less than the theoretical content of O in Al2O3, indicating that the AlH3 particle pile is not completely burned.

[0072] It can be seen from the above embodiments that the sample stage of the present invention can be used to implement laser ignition and combustion tests of energetic materials in particle piles, and can also implement microstructure and chemical composition analysis of specific energetic material particle piles.

[0073] The preferred embodiments of the present disclosure are described in detail above in conjunction with the accompanying drawings; however, the present disclosure is not limited to the specific details in the above embodiments. Within the technical concept of the present disclosure, a variety of simple modifications can be made to the technical solution of the present disclosure, and these simple modifications all fall within the protection scope of the present disclosure.

[0074] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present disclosure will not further describe various possible combinations.

[0075] In addition, various embodiments of the present disclosure may be arbitrarily combined, and as long as they do not violate the concept of the present disclosure, they should also be regarded as the contents disclosed by the present disclosure.

Claims

1. Application of a combustion reaction pool array for studying the ignition performance of energetic materials to the ignition performance study of energetic material particle piles; The combustion reaction pool array for studying the ignition performance of energetic materials is provided with a carrier, and a plurality of pits are arranged on the carrier in an array distribution; the diameter of the pits is 2 to 10 times the diameter of the sample particles, so that each pit can accommodate 2 to 10 sample particles; the spacing between adjacent pits is 1 μm to 1000 μm, the pore size of the pits is 1 μm to 1000 μm, and the depth of the pits is 500 nm to 500 μm; the pits are circular pits; The carrier is a glass slide, which is rectangular, 5 to 10 cm long, 1 to 3 cm wide, and 0.5 to 1.5 mm thick, and the array-distributed pits are arranged at the center of the glass slide; The specific steps include: Step 1, loading sample particles into the pits, with one pit containing more than two sample particles; Step 2, positioning and marking the particle pile sample in the pit under a scanning electron microscope; Step 3, performing laser focusing and ignition tests on the particle pile sample under an optical microscope, and using a high-speed camera to record the combustion reaction process of the particle pile sample; Step 4, after completing the ignition test, perform morphological analysis and energy spectrum detection on the combustion products in the pits under a scanning electron microscope to obtain the morphological structure and chemical composition of the combustion products, and match the combustion process of the particle pile sample with the combustion products according to the pit marks in step 2.

2. The use according to claim 1, characterized in that: The number of the sample particles is 2 to 10.

3. The use according to claim 1 or 2, characterized in that: The step 1 specifically includes: taking sample particles, scattering them on the positions of the carrier where the pits are arranged in an array, taking another carrier, contacting one side of the carrier with the sample carrier, and moving in a square shape along the length of the sample carrier, removing excess sample particles on the surface of the sample carrier, and leaving only the sample particles in the pits, with 2 to 10 sample particles left in one pit.

4. The use according to claim 1 or 2, characterized in that: The step 2 specifically includes: sending the carrier processed in step 1 into the sample chamber of a scanning electron microscope, finding pits with 2 to 10 sample particles by observing the pit morphology under a high-magnification field of view, and marking the positions of these pits.

5. The use according to claim 1 or 2, characterized in that: The step 3 specifically includes: placing the marked combustion reaction pool array under a microscope, adjusting the focal length of the microscope to make the sample particles in the pits clearly imaged, adjusting the laser power according to the laser ignition test steps, turning on the laser to perform a laser ignition test on the sample particles, and using a high-speed camera to record the combustion reaction process.

Images