CN116879026A - TATB/fluororubber interface micromechanics behavior testing method - Google Patents
TATB/fluororubber interface micromechanics behavior testing method Download PDFInfo
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- 238000012360 testing method Methods 0.000 title claims abstract description 52
- JDFUJAMTCCQARF-UHFFFAOYSA-N tatb Chemical compound NC1=C([N+]([O-])=O)C(N)=C([N+]([O-])=O)C(N)=C1[N+]([O-])=O JDFUJAMTCCQARF-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229920001973 fluoroelastomer Polymers 0.000 title claims abstract description 11
- 238000001237 Raman spectrum Methods 0.000 claims abstract description 16
- 239000000853 adhesive Substances 0.000 claims abstract description 12
- 230000001070 adhesive effect Effects 0.000 claims abstract description 12
- 238000005259 measurement Methods 0.000 claims abstract description 9
- 238000006073 displacement reaction Methods 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims description 32
- 238000001069 Raman spectroscopy Methods 0.000 claims description 22
- 239000002360 explosive Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 230000010287 polarization Effects 0.000 claims description 16
- 239000011230 binding agent Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 6
- 238000004528 spin coating Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 230000004044 response Effects 0.000 claims description 2
- 238000001228 spectrum Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 238000004458 analytical method Methods 0.000 abstract description 6
- 230000008859 change Effects 0.000 abstract description 6
- 239000002131 composite material Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 125000003277 amino group Chemical group 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000794 confocal Raman spectroscopy Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005474 detonation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011326 mechanical measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/02—Details
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/02—Details
- G01N3/06—Special adaptations of indicating or recording means
- G01N3/068—Special adaptations of indicating or recording means with optical indicating or recording means
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- General Physics & Mathematics (AREA)
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a TATB/fluororubber interface micromechanics behavior testing method, which is a brand new testing method for evaluating the microcosmic appearance and interface mechanics of an energetic material, wherein the interface mechanics behavior of PBX (private branch exchange) of different structural adhesive components is researched, so that the relative change of the interface stress can be obtained, the accuracy is high, the stress-strain change analysis can be obtained at the same time, the micro tensile force is applied to a PBX test sample, and the measurement of the force (displacement) load of the sample and the acquisition of a Raman spectrum are realized.
Description
Technical Field
The invention relates to the technical field of stress measurement, in particular to a TATB/fluororubber interface micromechanics behavior test method.
Background
A polymer bonded explosive (PBX) is essentially a polymer based composite material with highly filled explosive particles, the mechanical properties of which depend primarily on the internal binder and the interfacial properties between the explosive and the binder. The interface microstructure is a two-dimensional region where the physical and chemical properties of the mixed explosive are mutated, and is an origin region which leads to debonding and cracking of the explosive, but the interface microstructure is complex, the composition of the transition layer region is difficult to confirm, and an effective characterization means is not available at present. The components of the PBX have specificity, namely the explosive crystals are in a highly filled state and the modulus of the explosive crystals is far higher than that of the adhesive, the forming process of the PBX has complexity, namely the press-fit product is required to be formed by granulation and high-temperature high-pressure pressing, a large number of interfaces exist in the PBX, the structure is extremely complex, and jump of thermophysical properties and mechanical properties can be necessarily caused at the interfaces. Therefore, the research on the interface effect of the explosive crystal and the binder has important significance for evaluating and improving the mechanical property, detonation property and safety property of the PBX explosive.
Although the interfacial debonding process of explosive crystals can be described to a certain extent purely from a mechanical point of view, since reliable visual analysis and quantitative characterization of the interfacial effect between the explosive crystals and the binder are not implemented, the explanation of crack formation and interfacial enhancement modification operation of PBX explosive components is not clear and accurate. Advanced analysis means and characterization technology are urgently needed to directly observe and quantitatively analyze the interface effect between explosive crystals and binder in PBX so as to fully understand the interface bonding effect and debonding cause of explosive crystals.
The microscopic Raman spectrum measurement technology is a new technology developed in recent years for measuring microscale experiments, and the microscopic Raman spectrum measurement technology realizes measurement and characterization of mechanical parameters such as strain, stress and the like by measuring the change of the frequency shift position of a characteristic peak in Raman spectra before and after deformation of a measured object and utilizing the strain-frequency shift analysis relation of corresponding materials, and has the characteristics of no damage, non-contact, micron-sized spatial resolution, sensitivity to intrinsic stress and extrinsic stress and the like. The method is applied to interface research of the energetic material, and provides another brand new test method for evaluating microscopic interface mechanics of the energetic material. However, the energetic material belongs to a special dangerous material, has a large number of interfaces and large brittleness, is difficult to determine the stress direction and the stress component of the composite material, and has not yet a testing method for measuring the micro stress of the interface of the energetic material PBX, thereby bringing a plurality of difficulties for the mechanical measurement of micro Raman.
Disclosure of Invention
The invention aims to provide a TATB/fluororubber interface micromechanics behavior testing method for solving the problems, provides a sample testing method and a stress analysis method, belongs to a new method and new application established in energetic material micromechanics behavior research by utilizing a micro Raman technology, and provides a new opportunity for researching the interface effect of explosive crystals and adhesives and PBX mechanical enhancement.
The invention realizes the above purpose through the following technical scheme:
a preparation method of a PBX microstress test sample comprises the steps of uniformly mixing TATB explosive particles and a binder according to a mass ratio of 1:5-10, and spin-coating to form a film to prepare a double-cantilever beam test sample to be tested, wherein the thickness of the double-cantilever beam test sample is not more than 1cm, and the width of the double-cantilever beam test sample is not more than 1 cm.
Further, the particle size of the TATB particles is not less than 20 microns;
the adhesive is ethyl acetate solution of F2314, F2313 or F2311, and the concentration of F2314, F2313 or F2311 in the adhesive is 8-10%;
the test piece is dumbbell-shaped, and is cut into the shape with the aspect ratio of not more than 0.8 by laser after spin coating film forming: 1.
The invention also provides a TATB/fluororubber interface micromechanics behavior testing method, which comprises the following steps:
step 1, setting an initial stretching deformation amount and a deformation rate by using a micromechanics loading table, stretching a test piece, and reading the deformation amount of the test piece by using a displacement sensor;
step 2, placing the micromechanics loading table in a confocal Raman spectrum system, and carrying out Raman test on a test piece applied with load by utilizing the confocal Raman spectrum system, wherein the test range is not less than 50-3500cm -1 The test microscopic region is the interface between TATB crystal and the adhesive, and acquires a TATB Raman signal to obtain a Raman spectroscopy response signal at the interface between TATB and the adhesive, and calculates the loadThe spectrum shift difference value below;
step 3, measuring a {002} crystal face which is preferred by TATB in a sample, positioning the upper plane of TATB single crystal particles by using a confocal microscope, establishing a sample coordinate system on the {002} crystal face to be measured, carrying out Raman test on the test piece applied with load, adjusting focusing by a focusing lens, focusing on the {002} crystal face by using the microscope, and controlling a scattering signal to be polarized light on a common light path;
step 4, constructing a relational expression between a Raman spectrum movement increment in Raman spectrum information and the stress of the {002} crystal face of the TATB to be detected, wherein the relational expression between stress components in the sample stretching process is as follows:
wherein the method comprises the steps ofθ is the included angle between the polarization direction of the incident light and the polarization direction of the scattered light and the X-axis direction, respectively, and is takenIs a polarization angle combination; />Indicating that the polarization angle combination is +.>An increment of the frequency shift of the acquired raman spectrum relative to its unstressed state; sigma (sigma) x Is positive stress component in X-axis direction, sigma y For positive stress component in Y-axis direction, τ xy Is a shear stress component; />Respectively representing the polarization angle combination as +.>Time sigma x 、σ y And τ xy A constant factor of linear relationship with raman shift delta;
step 5, calibrating the micro-mechanical loading table by using a light spring to obtain the load coefficient of the mechanical loading table, and taking the load coefficient as the standard load for judging initial deformation; solving the equation set of the step 4 to obtain the equation set of the to-be-detected {110} crystal face stress component expression expressed by the raman frequency shift increment under three different polarization angle combinations of the measuring point; substituting the measured Raman frequency shift increment under three different polarization angle combinations of the measuring point into the stress component expression equation set to obtain the stress component, and combining a displacement sensor to obtain an apparent stress-strain curve.
Further, in the step 1, an initial stretching deformation amount and a deformation rate are set, and the additional load and the deformation become uniform.
In the step 3, the sample coordinate system is a space rectangular coordinate system, the X-axis direction and the Y-axis direction of the sample coordinate system are orthogonal directions in the {002} crystal face to be measured, and the Z-axis direction is an external normal direction; the angular polarization Raman light path is adopted during measurement, the incident laser is 532nm, and the incident laser and the Z-axis direction form opposite directions; the controller is a polarizer; the microscope numerical aperture was 0.45.
In a further scheme, in the step 4, the test piece is dumbbell-shaped, and the stress component of the test piece can be simplified into:
the positive stress component in the Y-axis direction is equivalent to the positive stress component in the X-axis direction, so that the positive stress in the X-axis direction is written as 2 times, and the positive stress in the Z-axis direction is polarized and deviated, and is regarded as a reduction term.
The invention has the beneficial effects that:
according to the TATB/fluororubber interface micromechanics behavior testing method, interface mechanics behavior research is carried out on PBX of different structural adhesive components, so that the relative change of interface stress can be obtained, the accuracy is high, the stress-strain change analysis can be obtained at the same time, the measurement of the force (displacement) load of a sample and the acquisition of a Raman spectrum are realized while the micro tensile force is applied to a PBX sample, and the method is a brand-new testing method for evaluating the microcosmic appearance and the interface mechanics of an energetic material.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following description will briefly explain the practical drawings required in the embodiments or the prior art description, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a microscopic view of {002} crystal plane to be measured of a TATB-based PBX material of the present invention;
FIG. 2 is a Raman diagram of a PBX material with TATB compounded by different adhesives (F2314, F2313, F2311) under microstress loading;
FIG. 3 is a drawing process of a TATB/F2314 composite of the present invention;
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, based on the examples herein, which are within the scope of the invention as defined by the claims, will be within the scope of the invention as defined by the claims.
Example 1:
uniformly mixing TATB explosive particles with the particle size of 20 micrometers and a binder in a mass ratio of 1:10, and spin-coating to form a film to prepare a dumbbell-type double-cantilever beam test piece with the thickness of 0.5mm and the width of 0.6 mm. The binder was dissolved in ethyl acetate in advance, and the dilution ratio was 8%. And (3) applying stretching to the test piece by using a micromechanics loading table according to the initial stretching deformation quantity and the deformation rate of the equipment, and reading the deformation quantity of the test piece by using a displacement sensor. Before the micro-mechanical loading platform is used, mechanical calibration is needed. The elasticity of the light spring is zeroed before testing. The additional load and deformation become uniform. The micromechanic loading stage is placed in a confocal raman spectroscopy system. As shown in fig. 1, a confocal microscope is used for finding {002} crystal face measurement of TATB, a confocal microscope is used for locating TATB but a plane on crystal particles, a sample coordinate system is established on the {002} crystal face to be detected, the sample coordinate system is a space rectangular coordinate system, the X-axis direction and the Y-axis direction of the sample coordinate system are orthogonal directions in the {002} crystal face to be detected, and the Z-axis direction is an external normal direction.
Carrying out Raman test on a test piece applied with load by utilizing a confocal Raman spectrum system, wherein the test range is 50-3500cm -1 The test microscopic region is the interface between the TATB crystal and the adhesive, and mainly acquires a TATB Raman signal.
Example 2:
the composite materials of TATB and F2311, F2314, F2313 were prepared separately and subjected to raman testing as described in example 1. As shown in FIG. 2, the binding capacities of F2311, F2314 and F2313 and TATB before mechanical loading show a certain difference, and compared with a TATB powder sample, the TATB/F2314 compound has more obvious blue shift, which shows that the introduction of F2314 weakens the amino group and the C-NO in the TATB molecule 2 Hydrogen bond interactions of (a). The amino group of TATB and C-F of F2314 may have intermolecular hydrogen bonding, but the effect is not strong, and there is no obvious characteristic change on F2314. The F2311/TATB composite material has very good elasticity, and 100% of deformation begins to be debonded, but 166% of deformation is not broken; F2313/TATB phenomenon is similar to F2311/TATB;
F2314/TATB strength is higher, and when the fiber is stretched to 45% of deformation, obvious debonding phenomenon is seen, and 58.71% of deformation is broken.
Example 3:
as shown in FIG. 3, the full-process tensile test was carried out on the TATB/F2314 system with better strength performance according to the descriptions of example 1 and example 2, and the peak of the nitro group of TATB in the TATB/F2314 compound was shifted to a low wave number during the loading and stretching, and the maximum frequency shift was about 3.6cm -1 . A stress-strain curve of the composite material stretch is obtained. The composite material increases linearly with the strain at the initial stage of the tensile deformation, and then increases slowly until the interface becomes obviously debonded, and the stress begins to decrease. The whole stretching process can be similarly divided intoElasticity, strengthening and breaking. According to the stress-strain curve, based on a stress decoupling model established by the system based on the {002} crystal face to be detected, the effective strength limit of the system is 2.36Gpa.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims. In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further. Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (6)
1. A preparation method of a PBX microstress test sample is characterized in that TATB explosive particles and a binder are uniformly mixed according to a mass ratio of 1:5-10, and are spin-coated to form a film, so that a double-cantilever beam test sample to be tested with a thickness of not more than 1cm and a width of not more than 1cm is prepared.
2. The method of claim 1, wherein the TATB particles have a size of not less than 20 microns;
the adhesive is ethyl acetate solution of F2314, F2313 or F2311, and the concentration of F2314, F2313 or F2311 in the adhesive is 8-10%;
the test piece is dumbbell-shaped, and is cut into the shape with the aspect ratio of not more than 0.8 by laser after spin coating film forming: 1.
3. A TATB/fluororubber interface micromechanics behavior testing method is characterized by comprising the following steps:
step 1, setting an initial stretching deformation amount and a deformation rate by using a micromechanics loading table, stretching a test piece, and reading the deformation amount of the test piece by using a displacement sensor;
step 2, placing the micromechanics loading table in a confocal Raman spectrum system, and carrying out Raman test on a test piece applied with load by utilizing the confocal Raman spectrum system, wherein the test range is not less than 50-3500cm -1 The test microscopic region is the interface between the TATB crystal and the binder, and acquires a TATB Raman signal to obtain a Raman spectroscopy response signal at the interface between the TATB crystal and the binder, and calculates a spectrum displacement difference under load;
step 3, measuring a {002} crystal face which is preferred by TATB in a sample, positioning the upper plane of TATB single crystal particles by using a confocal microscope, establishing a sample coordinate system on the {002} crystal face to be measured, carrying out Raman test on the test piece applied with load, adjusting focusing by a focusing lens, focusing on the {002} crystal face by using the microscope, and controlling a scattering signal to be polarized light on a common light path;
step 4, constructing a relational expression between a Raman spectrum movement increment in Raman spectrum information and the stress of the {002} crystal face of the TATB to be detected, wherein the relational expression between stress components in the sample stretching process is as follows:
wherein the method comprises the steps ofThe included angles of the polarization direction of the incident light and the polarization direction of the scattered light and the X-axis direction are respectively +.>Is a polarization angle combination; />Indicating that the polarization angle combination is +.>An increment of the frequency shift of the acquired raman spectrum relative to its unstressed state; sigma (sigma) x Is positive stress component in X-axis direction, sigma y For positive stress component in Y-axis direction, τ xy Is a shear stress component;respectively representing the polarization angle combination as +.>Time sigma x 、σ y And τ xy A constant factor of linear relationship with raman shift delta;
step 5, calibrating the micro-mechanical loading table by using a light spring to obtain the load coefficient of the mechanical loading table, and taking the load coefficient as the standard load for judging initial deformation; solving the equation set of the step 4 to obtain the equation set of the to-be-detected {110} crystal face stress component expression expressed by the raman frequency shift increment under three different polarization angle combinations of the measuring point; substituting the measured Raman frequency shift increment under three different polarization angle combinations of the measuring point into the stress component expression equation set to obtain the stress component, and combining a displacement sensor to obtain an apparent stress-strain curve.
4. The method for testing the micro-mechanical behavior of the interface of TATB/fluororubber according to claim 1, wherein in the step 1, initial stretching deformation amount and deformation rate are set, and additional load and deformation are uniform.
5. The method for testing the micromechanics behavior of a TATB/fluororubber interface according to claim 1, wherein in the step 3, the sample coordinate system is a space rectangular coordinate system, the X-axis direction and the Y-axis direction of the sample coordinate system are orthogonal directions in the {002} crystal face to be tested, and the Z-axis direction is an external normal direction; the angular polarization Raman light path is adopted during measurement, the incident laser is 532nm, and the incident laser and the Z-axis direction form opposite directions; the controller is a polarizer; the microscope numerical aperture was 0.45.
6. The method for testing the micromechanics behavior of a TATB/fluororubber interface according to claim 1, wherein in the step 4, the test piece is dumbbell-shaped, and the stress component of the test piece can be simplified as:the positive stress component in the Y-axis direction is equivalent to the positive stress component in the X-axis direction, so that the positive stress in the X-axis direction is written as 2 times, and the positive stress in the Z-axis direction is polarized and deviated, and is regarded as a reduction term.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117169139A (en) * | 2023-11-02 | 2023-12-05 | 北京科技大学 | Glass curtain wall structural adhesive mechanical property identification method based on reflection hyperspectrum |
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| CN117169139A (en) * | 2023-11-02 | 2023-12-05 | 北京科技大学 | Glass curtain wall structural adhesive mechanical property identification method based on reflection hyperspectrum |
| CN117169139B (en) * | 2023-11-02 | 2024-01-26 | 北京科技大学 | Glass curtain wall structural adhesive mechanical property identification method based on reflection hyperspectrum |
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