CN109470577A - The method of TATB base PBX internal stress is characterized under power-heat effect - Google Patents

The method of TATB base PBX internal stress is characterized under power-heat effect Download PDF

Info

Publication number
CN109470577A
CN109470577A CN201811319457.3A CN201811319457A CN109470577A CN 109470577 A CN109470577 A CN 109470577A CN 201811319457 A CN201811319457 A CN 201811319457A CN 109470577 A CN109470577 A CN 109470577A
Authority
CN
China
Prior art keywords
tatb
pbx
stress
lattice
diffraction
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201811319457.3A
Other languages
Chinese (zh)
Other versions
CN109470577B (en
Inventor
徐尧
刘晨
肖盼
戴斌
杨占锋
李丽
李海宁
何荣芳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institute of Chemical Material of CAEP
Original Assignee
Institute of Chemical Material of CAEP
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Institute of Chemical Material of CAEP filed Critical Institute of Chemical Material of CAEP
Priority to CN201811319457.3A priority Critical patent/CN109470577B/en
Publication of CN109470577A publication Critical patent/CN109470577A/en
Application granted granted Critical
Publication of CN109470577B publication Critical patent/CN109470577B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • G01N3/18—Performing tests at high or low temperatures
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
    • G01N23/046—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material using tomography, e.g. computed tomography [CT]
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/201—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials by measuring small-angle scattering
    • G01N23/202—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials by measuring small-angle scattering using neutrons
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
    • G01N23/2076—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions for spectrometry, i.e. using an analysing crystal, e.g. for measuring X-ray fluorescence spectrum of a sample with wavelength-dispersion, i.e. WDXFS
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
    • G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0058—Kind of property studied
    • G01N2203/0069—Fatigue, creep, strain-stress relations or elastic constants
    • G01N2203/0075—Strain-stress relations or elastic constants
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02—Details not specific for a particular testing method
    • G01N2203/022—Environment of the test
    • G01N2203/0222—Temperature
    • G01N2203/0228—Low temperature; Cooling means
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02—Details not specific for a particular testing method
    • G01N2203/06—Indicating or recording means; Sensing means
    • G01N2203/0641—Indicating or recording means; Sensing means using optical, X-ray, ultraviolet, infrared or similar detectors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02—Details not specific for a particular testing method
    • G01N2203/06—Indicating or recording means; Sensing means
    • G01N2203/067—Parameter measured for estimating the property
    • G01N2203/0676—Force, weight, load, energy, speed or acceleration
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02—Details not specific for a particular testing method
    • G01N2203/06—Indicating or recording means; Sensing means
    • G01N2203/067—Parameter measured for estimating the property
    • G01N2203/0682—Spatial dimension, e.g. length, area, angle

Abstract

The invention discloses the methods that TATB base PBX internal stress is characterized under power-heat effect, include the following steps: to carry out PBX mechanical stress in situ/thermal stress load, the lattice lattice parameter of TATB crystal is obtained using neutron diffraction techniques, obtains mechanical stress, the relationship of temperature and TATB lattice lattice parameter；Meanwhile the microscopical structure of PBX is obtained using internal microstructure characterization technique；The performance inflection point of PBX, TATB crystal response Behavior law inside the final PBX obtained under coupling thermal and mechanical effect are obtained by mechanical stress, the relationship of temperature and TATB lattice lattice parameter and microscopical structure.Neutron diffraction techniques are introduced energetic material research field for the first time by the present invention, the lattice parameters such as displacement, widthization, the asymmetry at TATB crystal diffraction peak in PBX under non-intrusion type Nondestructive observation mechanical stress/thermal stress provide the parameter on basis for the macro property assessment of energetic material.

Description

The method of TATB base PBX internal stress is characterized under power-heat effect
Technical field
The present invention relates to a kind of characterizing methods of explosive internal stress, and in particular to TATB base is characterized under a kind of power-heat effect The method of plastic bonded explosive internal stress.
Background technique
TATB (1,3,5- triamido -2,4,6- trinitrobenzen) is that the currently the only insensitiveness approved by U.S. Department of Energy is fried Medicine has good safety and stability because its mechanical sensitivity and heat sensitivity are lower.With TATB powder crystal (TATB Powder crystals) be base plastic bonded explosive (Polymer bonded explosive, PBX) it is military at home and abroad Device industry is used widely, and at home and abroad always around its structural safety performance, mechanical property and Study on Detonation Performance It is hot spot.
TATB base PBX is TATB that TATB explosive crystal and bonding agent are granulated into certain grain size distribution with water suspension method Grain (TATB granules) compression moulding afterwards.Because ambient pressure acts in forming process, different degrees of elastoplasticity occurs and becomes Shape can put aside certain elastic strain energy after pressure removal, generate internal stress.The performance difference of TATB explosive crystal and binder Very big, this makes PBX be different from traditional particles filled formula composite material, there is some special mechanical properties, from a large amount of thin sights It is a kind of fragile material containing initial damage that observation and experiment of machanics result, which can be seen that PBX,.PBX adds in cold-heat treatment, machinery Will receive various mechanical, temperature loading effects in work, transport, use and storage process, inside all there may be internal stress. Internal stress will cause initial damage and further develop, with reinforcement fracture, interfacial detachment, binder matrix cracking, deformation twins with And the forms such as shear band deteriorate the mechanical property of explosive, decline the strength and stiffness of structure.Under lasting load effect, Various forms of damages meeting further growths, polymerization, form macroscopic cracking, eventually lead to material damage.
TATB base PBX is polycrystalline, the multiple solutions, heterogeneous, low-intensity by the bonding aggregation of numerous TATB powder crystals Complex system, intensity are lower (compression strength is less than 45MPa, and tensile strength is less than 10MPa).Internal stress will affect inside PBX The mechanical behavior of each component, and the change of the mechanical behavior of each component is its changed principal element of macroscopic view inside PBX.It is right The research of PBX system mechanical behavior must be possible to establish more accurate mechanical model from microscopical structure:
(1) TATB has plane molecular structure, and crystal category anorthic system has the layer structure similar to graphite, It there are stronger hydrogen bond action between same layer TATB molecule, is tightly combined, and acts on very weak between different layer, this anisotropy makes Multi-crystal system response mechanism becomes complicated.TATB crystal belongs to fragile material, and as the high polymer of binder with very good Toughness, larger deformation can be born, can play the role of cohering blasting explosive granules and transmitting stress.TATB crystal structure is not right Claim, under the conditions of temperature increases, anisotropic expansion will occur, the anisotropic expansion of crystal is to lead to PBX thermal deformation, inside The key factor of micro-crack etc..The mechanical behavior of each component has codetermined the macro property of PBX system inside PBX.
(2) PBX (PBX comprising TATB base) substance mechanical characteristic is generally built upon constitutive relationship of stress-strain basis On, not careful consideration explosive crystal, binder, deterrent and plasticizer etc. carefully see factor, each inside PBX under power-heat effect The mechanical response characteristic of having differences property of component, therefore study extraneous thermal stress, the lower inside the PBX TATB strain of mechanical stress effect Response pattern is of great significance, and intensification is energetic material to the understanding of such compound system structure and performance change by this Macro property assessment and material microstructure simulation provide the parameter on basis.
In conclusion TATB base PBX belongs to typical polycrystalline multiple solutions heterogeneous material, the lower (compression strength of intensity Less than 45MPa, tensile strength be less than 10MPa), PBX system carefully see each component thermal response with diversity and difference it is obvious, it is comprehensive It takes a group photo and rings macro-mechanical property, studying these has very important science and engineering significance.
Summary of the invention
The purpose of the present invention is to provide one kind by carrying out PBX neutron diffraction lattice parameter experimental study, establishes mechanical It is brilliant to obtain TATB inside the PBX under power-thermal coupling effect for stress, thermal stress and TATB crystal neutron diffraction lattice parameter relationship The method of body respondent behavior rule.
The present invention is implemented as follows:
The method that TATB base PBX internal stress is characterized under power-heat effect, includes the following steps:
Mechanical stress in situ/thermal stress load is carried out to PBX, the lattice-site of TATB crystal is obtained using neutron diffraction techniques Battle array parameter, obtains mechanical stress, the relationship of temperature and TATB lattice lattice parameter；
Meanwhile the microscopical structure of PBX is obtained using internal microstructure characterization technique；
It is turned by the performance that mechanical stress, the relationship of temperature and TATB lattice lattice parameter and microscopical structure obtain PBX Point, the final inside the PBX TATB crystal response Behavior law obtained under coupling thermal and mechanical effect.
Further scheme is:
The neutron diffraction techniques, specifically:
Using neutron stress diffraction screen, PBX external environment is controlled are as follows: -55 DEG C to 200 DEG C of temperature, mechanical stress 0MPa ~40Mpa obtains the inside PBX TATB lattice lattice parameter under composite force, thermal environment.
Further scheme is:
The relationship of mechanical stress, temperature and TATB lattice lattice parameter, obtains particular by following method:
The change of stress and temperature will lead to the change of spacing of lattice, and neutron diffraction measures the lattice between crystallographic plane Spacing, so that elastic strain is exported, then according to strain calculation stress and thermal expansion coefficient.When crystalline material by with its crystal face When the radiation exposure of spacing close-spaced wavelength, ray will be diffracted to form specific bragg peak, the angle that diffracted ray generates It is provided by Bragg diffraction law:
2dhkl sinθhkl=λ (1)
In formula: λ is beam wavelength；dhklFor (hkl) interplanar distance for generating bragg peak；θhklFor Bragg angle.
The observation position of diffraction maximum and incident beam are at 2 θhklAngle, strain measurement are on the direction of Scattering of Vector, it divides equally The angle of incident beam and diffracted beam.The variation for measuring interplanar distance d from sample can calculate the size of strain stress:
In formula, d0For the interplanar distance value of unstressed standard sample.
To the neutron that stationary reactor generates, the neutron beam of a certain fixed wave length, sample interplanar distance are selected with monochromator Variation (Δ d) can cause corresponding diffraction maximum peak position offset (Δ θ).The diffraction of a certain crystal face of sample is measured in this way Peak, and determine using Gauss/Lorentz lorentz's fit procedure the peak position of diffraction maximum.Therefore elastic strain are as follows:
In formula, θ0For the peak position at the Bragg diffraction peak of unstressed standard sample.
When known to principal direction, the measurement in 3 directions determines a complete stress tensor enough.
In formula, E is elasticity modulus, and v is Poisson's ratio, εxx、εyyAnd εzzIt is the bullet that 3 directions in space are measured from sample respectively Property strain.
Obtaining TATB explosive crystal mechanical stress/temperature under rarefaction with TATB crystal neutron diffraction lattice parameter is Linear relationship.
Further scheme is:
The internal microstructure characterization technique includes: that scanning electron microscope (SEM) technology, Microfocus X-ray x-ray tomography are swept Retouch (μ CT) technology, neutron small angle scattering (SANS) technology etc..
Scanning electron microscope (SEM) technology is a kind of common observation method, be commonly used to the material of 10nm~1mm into Row microscopic sdIBM-2+2q.p.approach is, it can be achieved that the high-precision of PBX section is observed.
Microfocus X-ray x-ray tomography (μ CT) technology is that a kind of lossless acquisition material internal (Asia) micro-meter scale of energy is three-dimensional The technology of structural information.It can realize that PBX underbead crack, hole etc. lack in conjunction with the FInite Element and image digitization correlation method of CT image Fall into Accurate Model and displacement field precise measurement.
Neutron small angle scattering (SANS) technology is a kind of powerful that quantitatively characterizing can be carried out to material porosity rate, it can To differentiate an open and close porosity, to obtain whole porosities and the more accurate measurement result of surface area.Carry out the small angle of neutron Diffraction characterization technique research realizes the quantitative analysis of PBX Micro-v oid.
Above-mentioned technology is the more mature prior art at present, and the present invention can choose one of them or several obtain Obtain the microscopical structure of PBX.For the field conventional scheme that bases on practicality of above-mentioned technology, details are not described herein again.
Further scheme is:
The performance inflection point is the inflection point of the PBX microscopical structure variation obtained by internal microstructure characterization technique.
Characteristic and innovation of the invention is that neutron diffraction techniques are introduced energetic material research field for the first time, non-to invade Enter under formula Nondestructive observation mechanical stress/thermal stress the dot matrix such as displacement, widthization, the asymmetry at TATB crystal diffraction peak in PBX to join Number, TATB crystal and binder are in different mechanical stress loads and temperature load phase from meso-scale research PBX system Role, analyses in depth the respondent behaviors such as lattice strain, the thermal expansion of TATB crystal and TATB crystal and binder are mutual The thermodynamics Evolution of function, for energetic material macro property assessment provide basis parameter, will be disclose PBX this Kind has the characteristics that the primary innovation of the high fillibility Compound Material Engineering meso-scale research mode of multiple dimensioned, unordered micro-structure.
Detailed description of the invention
Fig. 1 is method flow schematic diagram of the invention；
Fig. 2 is neutron diffraction-original position power-heat effect synchronous scanning schematic diagram of one embodiment of the invention.
Specific embodiment
The present invention is further illustrated in the following with reference to the drawings and specific embodiments.
As shown in Fig. 1, the present invention provides a kind of methods that TATB base PBX internal stress is characterized under power-heat effect, including Following steps:
Mechanical stress in situ/thermal stress load is carried out to PBX, the lattice-site of TATB crystal is obtained using neutron diffraction techniques Battle array parameter, obtains mechanical stress, the relationship of temperature and TATB lattice lattice parameter；
Meanwhile the microscopical structure of PBX is obtained using internal microstructure characterization technique；
It is turned by the performance that mechanical stress, the relationship of temperature and TATB lattice lattice parameter and microscopical structure obtain PBX Point, the final inside the PBX TATB crystal response Behavior law obtained under coupling thermal and mechanical effect.
Each specific steps of the invention are described in detail below.
(1) PBX in situ neutron diffraction under power, heat condition
PBX belongs to low-intensity material, and compressive strength is less than 45MPa, tensile strength is less than 10MPa；PBX Performance Assessment temperature Range is -55 DEG C~200 DEG C；In addition PBX is suitable for carrying out small sample test there are also risk of explosion under the condition of high temperature；In adding Requirement of the sub- diffraction method to homeostatic reaction neutron pile.The present invention is based on China Engineering Physics Research Institute's nuclear physics and chemical research Neutron stress diffraction screen, realize in composite force, thermal environment (- 55 DEG C of temperature~200 DEG C, mechanical stress 0MPa~ 40MPa) TATB lattice lattice parameter nondestructive characterisation (NDC) inside PBX.
Wherein, neutron stress diffraction screen is using in Inst. of Nuclear Physics and Chemistry, Chinese Engineering Physics Research Ins Sub- stress diffraction screen, spectrometer resolution ax d/d are 0.2%, 50 μ ε of strain resolution, neutron streaming intensity at sample position: Neutron wavelength range: 0.12nm~0.28nm, specification (sampling) body is adjusted in 4.7 × 106n ﹒ cm-2 ﹒ s-1 (heap power 20MW) Product range: 0.5mm × 0.5mm × 0.5mm~5mm × 5mm × 20mm, sample stage maximum capacity: 500kg has 5 freedom degrees (X-Y moves horizontally ± 300mm, and Z goes up and down 500mm, 0 °~360 ° of rotation, ± 30 ° of inclinations), can use diffraction angular region: 0 °~ 140°.According to " the neutron diffraction side of non-destructive testing measurement residual stress 26140-2010/ISO/TS of GB/T 21432:2005 Method " neutron diffraction internal stress measuring is carried out to sample, the spacing of lattice between crystallographic plane is measured by neutron diffraction, from crystalline substance Compartment away from change, export elastic strain, then according to strain calculation stress.
The working principle of neutron stress diffraction screen has in above-mentioned national standard to be introduced in detail.
It, can be using the conventional experimental provision that can be realized heating power loading effect, as long as can guarantee PBX in the present invention In situ neutron diffraction is carried out within the scope of the temperature and mechanical stress met the requirements.
In order to realize in mechanical load environment inside (mechanical stress 0MPa~40MPa) PBX TATB lattice lattice parameter without Damage characterization, it is desirable that mechanical load unit is with the stretching in 2mm*2mm*2mm-30mm*30mm*30mm sample size range, pressure Contracting (uniaxial compression/disk compression), 3 points, four kinds of load load capabilities of four-point bending, provide replaceable fixture；Mechanical loading Ability (stretching/compressing) is not less than 5KN, accuracy of reading 1%, and loading force minimum resolution amount is not more than 1N；Jaw travel is not small In 20mm, velocity of displacement range is 0.1mm/min to 2mm/min.
In order to realize in high/low temperature loading environment, TATB lattice lattice parameter is lossless inside (- 55 DEG C of temperature~200 DEG C) PBX Characterization, it is desirable that 200 DEG C of -55 DEG C~﹢ of high/low temperature loading unit high/low temperature loading range, accuracy of reading are not more than 1 DEG C, temperature fluctuation No more than 1 DEG C, temperature hold-time is not less than 20 hours, provides the settling mode of automatic temperature-adjusting control.
Based on the above-mentioned requirement for mechanical load (power load) and high/low temperature load (heat loads), those skilled in the art Heat, power can be loaded as long as can satisfy PBX according to the relevant heating power loading experimental apparatus of above-mentioned requirements designed, designed It is required that.
(3) mechanical stress/temperature and TATB crystal neutron diffraction lattice parameter relationship experiments are studied
The change of stress and temperature will lead to the change of spacing of lattice, and neutron diffraction measures the lattice between crystallographic plane Spacing, so that elastic strain is exported, then according to strain calculation stress and thermal expansion coefficient.When crystalline material by with its crystal face When the radiation exposure of spacing close-spaced wavelength, ray will be diffracted to form specific bragg peak, the angle that diffracted ray generates It is provided by Bragg diffraction law:
2dhkl sinθhkl=λ (1)
In formula: λ is beam wavelength；dhklFor (hkl) interplanar distance for generating bragg peak；θhklFor Bragg angle.
The observation position of diffraction maximum and incident beam are at 2 θhklAngle, strain measurement are on the direction of Scattering of Vector, it divides equally The angle of incident beam and diffracted beam.The variation for measuring interplanar distance d from sample can calculate the size of strain stress:
In formula, d0For the interplanar distance value of unstressed standard sample.
To the neutron that stationary reactor generates, the neutron beam of a certain fixed wave length, sample interplanar distance are selected with monochromator Variation (Δ d) can cause corresponding diffraction maximum peak position offset (Δ θ).The diffraction of a certain crystal face of sample is measured in this way Peak, and determine using Gauss/Lorentz lorentz's fit procedure the peak position of diffraction maximum.Therefore elastic strain are as follows:
In formula, θ0For the peak position at the Bragg diffraction peak of unstressed standard sample.
When known to principal direction, the measurement in 3 directions determines a complete stress tensor enough.
In formula, E is elasticity modulus, and v is Poisson's ratio, εxx、εyyAnd εzzIt is the bullet that 3 directions in space are measured from sample respectively Property strain.
TATB explosive crystal mechanical stress/temperature and TATB crystal neutron diffraction lattice parameter under rarefaction are linear Relationship；And power-thermal response of the TATB explosive crystal under polycrystalline compacting PBX system status is then more complicated.
(4) the accurate characterizing method of PBX microscopical structure
This project combination meso-scale precision characterizing method grasps the inflection point of microscopical structure variation, realizes to the inside PBX The Accurate Analysis of the different thermal response behaviors of TATB crystal provides experiment for the research of TATB crystal dynamics Behavior law and supports. Wherein:
Scanning electron microscope (SEM) technology is a kind of common observation method, be commonly used to the material of 10nm~1mm into Row microscopic sdIBM-2+2q.p.approach is, it can be achieved that the high-precision of PBX section is observed.
Microfocus X-ray x-ray tomography (μ CT) technology is that a kind of lossless acquisition material internal (Asia) micro-meter scale of energy is three-dimensional The technology of structural information.It can realize that PBX underbead crack, hole etc. lack in conjunction with the FInite Element and image digitization correlation method of CT image Fall into Accurate Model and displacement field precise measurement.
Neutron small angle scattering (SANS) technology is a kind of powerful that quantitatively characterizing can be carried out to material porosity rate, it can To differentiate an open and close porosity, to obtain whole porosities and the more accurate measurement result of surface area.Carry out the small angle of neutron Diffraction characterization technique research realizes the quantitative analysis of PBX Micro-v oid.
(5) TATB crystal response Behavior law research in the PBX under power-thermal coupling effect
Since PBX system is under mechanical stress and temperature action, TATB crystal and binder play different roles, special It is not highly-filled TATB crystal, characteristic and complicated system environment due to itself, in conjunction under Thermal-mechanical Coupling effect TATB lattice parameter, microscopical structure variation can more further investigate TATB crystal response Behavior law, assess for macro property The parameter on basis is provided.
The present invention is answered from loose TATB crystal mechanical stress/temperature-responsive research largely carrying out the original position PBX machinery On the basis of the mechanical response rule of its internal TATB crystal is tested and grasped in power load neutron diffraction, gradually to alternating temperature item in situ TATB Crystal study gos deep into PBX under part, and the accurate characterizing method development in conjunction with PBX microscopical structure is compound for Li-heat of PBX Load in situ and experimental data analytic technique, grasp TATB crystal neutron diffraction lattice parameter changing rule, deepen understanding PBX and exist It is defeated to provide experimental data for PBX macro property evaluation criteria for internal stress response pattern under the changes in environmental conditions such as power, heat Enter.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that those skilled in the art Member can be designed that a lot of other modification and implementations, these modifications and implementations will fall in principle disclosed in the present application Within scope and spirit.

Claims (5)

1. characterizing the method for TATB base PBX internal stress under a kind of power-heat effect, it is characterised in that include the following steps:
Mechanical stress in situ/thermal stress load is carried out to PBX, is joined using the lattice dot matrix that neutron diffraction techniques obtain TATB crystal Number obtains mechanical stress, the relationship of temperature and TATB lattice lattice parameter；
Meanwhile the microscopical structure of PBX is obtained using internal microstructure characterization technique；
The performance inflection point of PBX is obtained by mechanical stress, the relationship of temperature and TATB lattice lattice parameter and microscopical structure, most TATB crystal response Behavior law inside the PBX under coupling thermal and mechanical effect is obtained eventually.
2. the method for TATB base PBX internal stress is characterized under power-heat effect according to claim 1, it is characterised in that:
The neutron diffraction techniques, specifically:
Using neutron stress diffraction screen, PBX external environment is controlled are as follows: -55 DEG C to 200 DEG C of temperature, mechanical stress 0MPa~ 40Mpa obtains the inside PBX TATB lattice lattice parameter under composite force, thermal environment.
3. the method for TATB base PBX internal stress is characterized under power-heat effect according to claim 2, it is characterised in that:
The relationship of mechanical stress, temperature and TATB lattice lattice parameter, obtains particular by following method:
The change of stress and temperature will lead to the change of spacing of lattice, and neutron diffraction measures between the lattice between crystallographic plane Away from so that elastic strain is exported, then according to strain calculation stress and thermal expansion coefficient；When crystalline material by with its interplanar When radiation exposure away from close-spaced wavelength, ray will be diffracted to be formed specific bragg peak, the angle that diffracted ray generates by Bragg diffraction law provides:
2dhkl sinθhkl=λ (1)
In formula: λ is beam wavelength；dhklFor the hkl interplanar distance for generating bragg peak；θhklFor Bragg angle；
The observation position of diffraction maximum and incident beam are at 2 θhklAngle, strain measurement are on the direction of Scattering of Vector, it divides incidence equally The angle of beam and diffracted beam；The variation for measuring interplanar distance d from sample can calculate the size of strain stress:
In formula, d0For the interplanar distance value of unstressed standard sample；
To the neutron that stationary reactor generates, the neutron beam of a certain fixed wave length, the change of sample interplanar distance are selected with monochromator Corresponding diffraction maximum peak position shifted by delta θ can be caused by changing Δ d；The diffraction maximum of a certain crystal face of sample is measured in this way, and is used Gauss/Lorentz lorentz's fit procedure determines the peak position of diffraction maximum；Therefore elastic strain are as follows:
In formula, θ0For the peak position at the Bragg diffraction peak of unstressed standard sample；
When known to principal direction, the measurement in 3 directions determines a complete stress tensor enough；
In formula, E is elasticity modulus, and v is Poisson's ratio, εxx、εyyAnd εzzIt is to measure the elasticity in 3 directions in space from sample to answer respectively Become；
It is linear for obtaining TATB explosive crystal mechanical stress/temperature and TATB crystal neutron diffraction lattice parameter under rarefaction Relationship.
4. the method for TATB base PBX internal stress is characterized under power-heat effect according to claim 1, it is characterised in that:
The internal microstructure characterization technique include: Scanning electron microscopy, Microfocus X-ray x-ray tomography technology or in Sub- small-angle scattering technology.
5. the method for TATB base PBX internal stress is characterized under power-heat effect according to claim 1, it is characterised in that:
The performance inflection point is the inflection point of the PBX microscopical structure variation obtained by internal microstructure characterization technique.
CN201811319457.3A 2018-11-07 2018-11-07 Method for representing internal stress of TATB-based PBX under force-heat action Active CN109470577B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811319457.3A CN109470577B (en) 2018-11-07 2018-11-07 Method for representing internal stress of TATB-based PBX under force-heat action

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811319457.3A CN109470577B (en) 2018-11-07 2018-11-07 Method for representing internal stress of TATB-based PBX under force-heat action

Publications (2)

Publication Number Publication Date
CN109470577A true CN109470577A (en) 2019-03-15
CN109470577B CN109470577B (en) 2021-03-16

Family

ID=65666873

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811319457.3A Active CN109470577B (en) 2018-11-07 2018-11-07 Method for representing internal stress of TATB-based PBX under force-heat action

Country Status (1)

Country Link
CN (1) CN109470577B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110793990A (en) * 2019-11-21 2020-02-14 山东建筑大学 Neutron diffraction characterization method for crystallization dynamic characteristics of bulk amorphous alloy
CN110793855A (en) * 2019-11-13 2020-02-14 北京理工大学 Evaluation method for intercrystalline stress of polycrystalline alloy with cubic structure

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5065439B2 (en) * 2009-05-12 2012-10-31 大陽日酸株式会社 Low temperature tensile testing machine
CN103115826A (en) * 2013-01-29 2013-05-22 中国工程物理研究院核物理与化学研究所 In-situ stress-temperature loading device for neutron diffraction technology
CN104236758A (en) * 2014-09-18 2014-12-24 西安近代化学研究所 Measuring device for internal stress and distribution of internal stress in explosive and powder solidifying and forming process
CN206593984U (en) * 2017-03-09 2017-10-27 中国工程物理研究院核物理与化学研究所 A kind of In Situ Heating device for neutron diffraction
CN108490006A (en) * 2018-03-30 2018-09-04 中国石油大学(华东) A method of testing slab residual stress using neutron diffraction techniques

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5065439B2 (en) * 2009-05-12 2012-10-31 大陽日酸株式会社 Low temperature tensile testing machine
CN103115826A (en) * 2013-01-29 2013-05-22 中国工程物理研究院核物理与化学研究所 In-situ stress-temperature loading device for neutron diffraction technology
CN104236758A (en) * 2014-09-18 2014-12-24 西安近代化学研究所 Measuring device for internal stress and distribution of internal stress in explosive and powder solidifying and forming process
CN206593984U (en) * 2017-03-09 2017-10-27 中国工程物理研究院核物理与化学研究所 A kind of In Situ Heating device for neutron diffraction
CN108490006A (en) * 2018-03-30 2018-09-04 中国石油大学(华东) A method of testing slab residual stress using neutron diffraction techniques

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
JOHN D. YEAGER ET AL.: "Neutron Diffraction Measurements and Micromechanical Modelling of Temperature‐Dependent Variations in TATB Lattice Parameters", 《PROPELLANTS，EXPLOSIVES，PYROTECHNICS》 *
徐尧: "中子衍射法测量TATB基PBX单轴压缩的内应力研究", 《含能材料》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110793855A (en) * 2019-11-13 2020-02-14 北京理工大学 Evaluation method for intercrystalline stress of polycrystalline alloy with cubic structure
CN110793855B (en) * 2019-11-13 2021-03-02 北京理工大学 Evaluation method for intercrystalline stress of polycrystalline alloy with cubic structure
CN110793990A (en) * 2019-11-21 2020-02-14 山东建筑大学 Neutron diffraction characterization method for crystallization dynamic characteristics of bulk amorphous alloy
CN110793990B (en) * 2019-11-21 2022-03-18 山东建筑大学 Neutron diffraction characterization method for crystallization dynamic characteristics of bulk amorphous alloy

Also Published As

Publication number Publication date
CN109470577B (en) 2021-03-16

Similar Documents

Publication Publication Date Title
Cadoni Dynamic characterization of orthogneiss rock subjected to intermediate and high strain rates in tension
Hansen et al. Protracted fabric evolution in olivine: Implications for the relationship among strain, crystallographic fabric, and seismic anisotropy
Guha Roy et al. Effect of heat treatment and layer orientation on the tensile strength of a crystalline rock under Brazilian test condition
Hutchings et al. Introduction to the characterization of residual stress by neutron diffraction
Mayr et al. Double shear creep testing of superalloy single crystals at temperatures above 1000 C
Mishra et al. High strain rate response of rocks under dynamic loading using split Hopkinson pressure bar
Datye et al. Extraction of anisotropic mechanical properties from nanoindentation of SiC-6H single crystals
Van Swygenhoven et al. The use of Laue microdiffraction to study small-scale plasticity
CN109470577A (en) The method of TATB base PBX internal stress is characterized under power-heat effect
Yeager et al. Neutron Diffraction Measurements and Micromechanical Modelling of Temperature‐Dependent Variations in TATB Lattice Parameters
Sun et al. Experiment study of physical and mechanical properties of sandstone after variable thermal cycles
Li et al. Thermal shock effects on the mechanical behavior of granite exposed to dynamic loading
Chen et al. Magnetic field-induced magnetostructural transition and huge tensile superelasticity in an oligocrystalline Ni–Cu–Co–Mn–In microwire
Rohbeck et al. Comparison study of silicon carbide coatings produced at different deposition conditions with use of high temperature nanoindentation
Quansah et al. Mechanical and thermophysical properties of energetic crystals: evaluation methods and recent achievements
Wang et al. Influence of freeze-thaw cycles on engineering properties of tonalite: examples from China
Bai et al. A review of small angle scattering, neutron reflection, and neutron diffraction techniques for microstructural characterization of polymer-bonded explosives
Zhai et al. Mechanical properties of pentaerythritol tetranitrate (PETN) single crystals from nano‐indentation: Depth dependent response at the nano meter scale
Katrusiak High-pressure devices
Filippelli et al. Evaluation of intragranular strain and average dislocation density in single grains of a polycrystal using K-map scanning
Yun et al. Noncontact stress measurement from bare UHPC surface using R aman piezospectroscopy
Guo et al. Creep behavior of titanium alloy used in deep-sea pressure shell considering tensile/compressive asymmetry: Experiments and numerical modeling
CN113984496A (en) Method for measuring static elastic constant of single crystal high-temperature alloy
Grosjean et al. Experimental creep behaviour determination of cladding tube materials under multi-axial loadings
Mirsayapov A study of stress concentration zones under cyclic loading by thermal imaging method.

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant