CN105548237A - Method for building energetic material mesoscopic hot spot physical model - Google Patents

Method for building energetic material mesoscopic hot spot physical model Download PDF

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CN105548237A
CN105548237A CN201510941078.8A CN201510941078A CN105548237A CN 105548237 A CN105548237 A CN 105548237A CN 201510941078 A CN201510941078 A CN 201510941078A CN 105548237 A CN105548237 A CN 105548237A
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energetic material
temperature
evolution
sample
surface topography
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CN105548237B (en
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赵玖玲
强洪夫
赵久奋
张文海
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No 2 Artillery Engineering University Of Chinese Pla
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/005—Investigating or analyzing materials by the use of thermal means by investigating specific heat
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity

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Abstract

The invention belongs to the technical field of energetic material thermo-safety and relates to a method for building an energetic material mesoscopic hot spot physical model. The method comprises thermal decomposition mechanism function and parameter determination, energetic material microstructure surface morphology evolution rule research, energetic material microstructure inner morphology evolution rule research and energetic material ingredient thermal physical constant determination. The method fully considers characteristics of energetic material self-damage, provides convenience and versatility for selection of interface model parameters of energetic material microscopic damage numerical simulation, builds a physical simulation rule system and a mesoscopic hot physical model satisfying the rule through complete simulation and prediction of practical characteristics and processes, has complete functions and can be implemented easily.

Description

The modeling method of focus physical model carefully seen by a kind of energetic material
Technical field
The invention belongs to the hot security technology area of energetic material, relate to the modeling method that ermal physics model carefully seen by a kind of energetic material.
Background technology
For energetic material thermal decomposition, be usually attended by the release of heat.If the heat that thermal decomposition discharges can not be diffused into surrounding environment, spontaneous combustion even explosion accident likely will be caused.
At present for hot secured physical model mainly based on chemical reaction-heat transfer model that macroscopical homogeneous is supposed, this model is well used in the roasting combustion process of emulation macroscopic view, but the realistic model adopting macroscopic view to homogenize can not disclose the mechanism of the profound level of energetic material heat safety, does not have prediction effect for the energetic material safe formula Design of heat and danger.
The meso-scale of energetic material determines its hot safety and thermal explosion mechanism, on meso-scale, energetic material right and wrong are homogeneous, can be regarded as the three-phase inhomogeneous composite materials be made up of oxidizing agent pellets, adhesive substrate and bonding interface band between the two.The inconsistent chemical reaction mechanism that between the inconsistent heat transfer property Sum decomposition exothermicity of each component, component, interface and each component are followed in thermal decomposition process, and in thermal decomposition process the structure evolution of the complexity that interface occurs between each component inner and component, these are all the complicacy determining energetic material heat safety.
In order to disclose the profound mechanism of energetic material heat safety, the comprehensive multiple grand mesoscale experiments method of the present invention, from the microstructure portion Morphology Evolution rule of the Microstructures Topography Evolution of the Thermal Decomposition Kinetic Parameters of energetic material and component thereof and mechanism function, energetic material and component thereof, energetic material and component thereof, mensuration four aspects of energetic material component thermal constant are launched, carefully see focus physical model to set up correct energetic material.
In prior art before the present invention, the document retrieved has: the refined equitemperature of [1] Liu Li is to the numerical evaluation [D] of propellant powder safety and energy affect. trajectory journal .2004:2; [2] inscription on pottery file. numerical heat transfer [M]. publishing house of Xi'an Communications University, 2001; [3] Du Zhiming. the thermal ignition [D] of chemical reacting flow in the finite space. Beijing: Beijing Institute of Technology, 1993; [4] Jing Songji. condensed explosive roasting combustion study mechanism and Two-dimensional numerical simulation [D]. Changsha: the National University of Defense technology, 2004; Above-mentioned document is the generic technology relevant to the technology of the present invention theme, but, from disclosed content, not yet find about the report of ermal physics model building method carefully seen by energetic material.
Summary of the invention
According to above-mentioned background technology, the object of the invention is to, for the prediction studying the hot safety mechanism of energetic material and hot safety critical temperature and blast time delay provides foundation, a kind of energetic material that can build high quality and high efficiency is provided carefully to see the modeling method of focus physical model for improving energetic material thermal stability formula.
Now design of the present invention and technical solution are described below:
Basic conception of the present invention is, considering that microscopical structure formation and differentiation and temperature are on the impact of the thermophysical property of component material, the influence factor comprehensive and reasonable considered, and under form prerequisite simple, easy to use, be described the method for building up that it carefully sees focus physical model, the method comprises: the determination of Thermal Decomposition Mechanism function and parameter; To the research of energetic material Microstructures Topography Evolution; To the research of energetic material microstructure portion Morphology Evolution rule; To mensuration four parts of energetic material component thermal constant, specifically comprise the following steps:
Step 1: by thermal capacitance and the temperature conductivity of DSC method and laser heat conduction method determination component material;
Step 2: determine Thermal Decomposition Mechanism function and parameter based on DSC-TG test;
Step 3: obtain energetic material surface topography with the Evolution of temperature by scanning electron microscope test, carry out quantitative test, show that surface topography is with Temperature Evolution rule;
Step 4: tested by μ CT and obtain the Evolution of energetic material internal morphology with temperature, and carry out quantitative test, compared with surface topography Evolution, the foundation for numerical model provides basis;
Step 5: the result summing up above four steps, draws the ermal physics model of energetic material based on thermal conduction study equation (3) and structure evolution rule:
ρ C d T d t = λ ▿ 2 T + S - - - ( 3 )
Wherein ρ is density, C is specific heat capacity, T is temperature, t is the time, λ is coefficient of heat conductivity, S is chemical heat release item;
Following General expression is had for chemical heat release item S
Wherein Q is the chemical heat release of unit quality, α is the mass percent that energetic material has reacted away.
The present invention further provides the modeling method that ermal physics model carefully seen by a kind of energetic material, it is characterized in that: the concrete grammar of " thermal capacitance and the temperature conductivity by DSC method and laser heat conduction method determination component material " described in step 1 is:
Step 1.1 adopts means of differential scanning calorimetry DSC method to obtain the thermal capacitance containing energy particle and adhesive substrate
High pure nitrogen atmosphere, flow velocity is 30-50ml/min; It is 0.5-1.5mm that adhesive substrate sample is processed into thickness in advance, and diameter is the smooth wafer type test specimen of 5-7mm; Containing can directly load in sample disc by granulated powder sample, during dress sample, gently sample disc to be shaken, so that the Contact of sample room, sample and dish is good.From room temperature 25 degrees Celsius, according to certain heating rate (general 1 ~ 10 degree Celsius/min) heating sample, until sample volatilizees completely, obtain the DSC curve of sample.The thermal capacitance of sample is calculated according to curve;
Step 1.2: adopt laser heat conduction method to obtain the temperature conductivity containing energy particle and adhesive substrate.
To be processed into diameter in advance containing energy particle and adhesive substrate is 10-14mm, and error is less than 1.5mm; Thickness 0.5-1.5mm, error is less than the smooth wafer type test specimen of 0.5mm.The test specimen made is put into conductometer, heats test specimen, to 400 degrees Celsius according to certain heating rate (general 1 ~ 10 degree Celsius/min), often heat up 50 degrees Celsius, obtain its coefficient of heat conductivity by probe, every test specimen obtains 5 values, by averaging, obtain its temperature conductivity.
The present invention further provides the modeling method that ermal physics model carefully seen by a kind of energetic material, it is characterized in that: the concrete grammar of " thermal capacitance and the temperature conductivity by DSC method and laser heat conduction method determination component material " described in step 2 is:
Step 2.1 obtains component material (containing energy particle and bonding agent) the DSC curve under four kinds of heating rates of energetic material, four kinds of temperature be respectively 1 DEG C/min, 5 DEG C/min, 10 DEG C/min, 15 DEG C/min, for calculating the Arrhenius parameter of component, comprise reaction activity, pre-exponential factor, mechanism function, computing method are as follows:
Non-isothermal Kinetics Kissinger equation (1) and Coats-Redfern equation (2) is adopted jointly to determine chemical reaction kinetic parameters and the mechanism function of energetic material component: first to obtain the gentle reaction depth value in DTG peak from the TG curve of four kinds of heating rates of institute's test specimens, obtain reaction activity and pre-exponential factor with Kissinger equation, then determine g (α) function by Coats-Redfern equation.
l n ( β T p 2 ) = l n A R E a - E a RT p - - - ( 1 )
l n ( g ( α ) T 2 ) = l n A R βE a [ 1 - 2 R T E a ] - E a R T - - - ( 2 )
Be wherein β heating rate, T pfor peak temperature, T is arbitrary temperature in thermal decomposition process, E afor apparent activation energy, A is pre-exponential factor, and R is gas law constant, and 8.314J/K.mol, g (α) are mechanism function integrated form, and α is reaction depth;
Step 2.2 obtains energetic material component material (containing energy particle and bonding agent) the TG curve under heating rate is 5 DEG C/min, for the evolution of comparing calculation material with temperature geometrical morphology.
The present invention further provides the modeling method that ermal physics model carefully seen by a kind of energetic material, it is characterized in that: the concrete grammar of " the obtaining the Evolution of energetic material surface topography with temperature by scanning electron microscope test; carry out quantitative test, show that surface topography is with Temperature Evolution rule " described in step 3 is:
Step 3.1 obtains containing energy particle thin sight surface topography picture at different temperatures, for calculating containing providing basis with Temperature Evolution curve by granule-morphology;
Step 3.2 obtains adhesive film thin sight surface topography picture at different temperatures, for research adhesive film pattern provides foundation with Temperature Evolution rule.
The present invention further provides the modeling method that ermal physics model carefully seen by a kind of energetic material, it is characterized in that: described in step 3 " tested by μ CT and obtain the energetic material internal morphology Evolution with temperature; and carry out quantitative test, compared with surface topography Evolution " concrete grammar be:
Step 4.1 obtains containing energy particle thin sight internal morphology picture at different temperatures, for count particles pattern provides basis with Temperature Evolution curve;
Step 4.2 obtains energetic material thin sight internal morphology picture at different temperatures, for research energetic material pattern provides foundation with Temperature Evolution.
The present invention's superiority is compared with the existing technology: the method has taken into full account characteristic specific to energetic material self-inflicted injury, for the selection of the INTERFACE MODEL parameter of energetic material microscopic damage numerical simulation employing provides convenience and versatility, with the characteristic sum process that comprehensive simulated prediction is actual, establish the physical simulation hierarchy of criteria and meet the thin sight ermal physics model of criterion, complete function, be easy to realize.
Embodiment
To be below example with HTPB propellant (containing can particle be AP particle, adhesive substrate be fourth hydroxyl HTPB), by seeing ermal physics model modelling approach to structure explanation of its thin sight focus physical model is thin.
Step 1: by thermal capacitance and the temperature conductivity of DSC method and laser heat conduction method determination component material.
Step 1.1 adopts means of differential scanning calorimetry DSC method to obtain the thermal capacitance containing energy particle and adhesive substrate
High pure nitrogen atmosphere, flow velocity is 40ml/min; It is 1mm that adhesive substrate sample is processed into thickness in advance, and diameter is the smooth wafer type test specimen of 6mm; Containing can directly load in sample disc by granulated powder sample, during dress sample, gently sample disc to be shaken, so that the Contact of sample room, sample and dish is good.From room temperature 25 degrees Celsius, according to certain heating rate (general 1 ~ 10 degree Celsius/min) heating sample, until sample volatilizees completely, obtain the DSC curve of sample.The thermal capacitance of sample is calculated according to curve.
Step 1.2 adopts laser heat conduction method to obtain the temperature conductivity containing energy particle and adhesive substrate
To be processed into diameter in advance containing energy particle and adhesive substrate is 12mm, and error is 1mm; Thickness 1.5mm, error is the smooth wafer type test specimen of 0.5mm.The test specimen made is put into conductometer, heats test specimen, to 400 degrees Celsius according to certain heating rate (general 1 ~ 10 degree Celsius/min), often heat up 50 degrees Celsius, obtain its coefficient of heat conductivity by probe, every test specimen obtains 5 values, by averaging, obtain its temperature conductivity.
Step 2: determine AP and HTPB Thermal Decomposition Mechanism function and parameter based on DSC-TG test
Obtain the DSC curve of AP and HTPB under four kinds of heating rates (be respectively 1 DEG C/min, 5 DEG C/min, 10 DEG C/min, 15 DEG C/min), for calculating the Arrhenius parameter (comprising reaction activity, pre-exponential factor, mechanism function) of component.Computing method are as follows:
Non-isothermal Kinetics Kissinger equation (1) and Coats-Redfern equation (2) is adopted jointly to determine chemical reaction kinetic parameters and the mechanism function of energetic material component: first to obtain the gentle reaction depth value in DTG peak from the TG curve of four kinds of heating rates of institute's test specimens, obtain reaction activity and pre-exponential factor with Kissinger equation, then determine g (α) function by Coats-Redfern equation.
Test records the parameter of test specimen (AP and HTPB) as shown in Table 1 and Table 2:
The chemical reaction kinetic parameters of table 1 film
Energy of activation Pre-exponential factor ln (A) Mechanism function g (α) Mechanism
87.5 9.93 -ln(1-α) Coring and increment
Table 2AP reactive kinetics parameters and mechanism function
Stage Energy of activation Pre-exponential factor Mechanism function g (α) Mechanism
Low-temperature decomposition section 167.3 29.55 [-ln(1-α)] 1/2 Coring and increment equation
Transition section 64.5 5.23 [(1+α) 1/3-1] 2 Three-dimensional ore body model
Pyrolytic peak 206.4 34.84 [(1+α) 1/3-1] 2 Three-dimensional ore body model
Step 3: obtain AP and HTPB surface topography with the Evolution of temperature by scanning electron microscope test, carry out quantitative test, show that surface topography is with Temperature Evolution rule
Step 3.1 obtains AP particle thin sight surface topography picture at different temperatures, for count particles pattern provides basis with Temperature Evolution curve;
Step 3.2 obtains HTPB film thin sight surface topography picture at different temperatures, for research adhesive film pattern provides foundation with Temperature Evolution rule.
Surface topography Evolution through test determination test specimen is as shown in table 3.
The change of table 3 different temperatures AP surface voids rate
Temperature/DEG C 100 150 200 230 280 330 380
Hole rate/% 0 0 0 2.34 6.02 19.84 70
Visible through observation and analysis, during the heating of HTPB film, the evolutionary process of surface topography is divided into three phases: the first stage: original uniform shape heat shrinkable; Subordinate phase: fold after shrinking; Phase III: fold degree is constantly aggravated.
Step 4: tested by μ CT and obtain the Evolution of AP and HTPB internal morphology with temperature, and carry out quantitative test, compared with surface topography Evolution, the foundation for numerical model provides basis.
Obtain AP particle thin sight internal morphology picture at different temperatures, for count particles pattern provides basis with Temperature Evolution curve, AP inner cavity rate varies with temperature as shown in table 4.
The change of table 4 different temperatures AP inner cavity rate
Temperature/DEG C 100 150 200 230 280 330
Hole rate/% 0 0 0 2.01 6.54 21.05
Step 5: based on thermal conduction study equation (3) and structure evolution rule, the result summing up above four steps, show that the ermal physics model of HTPB propellant comprises three parts: the thermal decomposition of HTPB thermal decomposition and heat transfer, AP particle and heat transfer, the evolution of AP-HTPB interface.There is multiple chemical reaction in AP particle in decomposes process, the heat produced is delivered in HTPB by AP-HTPB interface, HTPB coefficient of heat conductivity is lower, in thermal histories, performance is comparatively stable, larger thermograde is formed at AP-HTPB near interface, meanwhile AP granule interior starts to occur microporosity, and AP interface also starts to shrink and causes AP-HTPB interface heat transfer performance to decline further.

Claims (5)

1. the modeling method of focus physical model carefully seen by an energetic material, it is characterized in that: considering that microscopical structure formation and differentiation and temperature are on the impact of the thermophysical property of component material, the influence factor comprehensive and reasonable considered, and under form prerequisite simple, easy to use, be described the method for building up that it carefully sees focus physical model, the method comprises: the determination of Thermal Decomposition Mechanism function and parameter; To the research of energetic material Microstructures Topography Evolution; To the research of energetic material microstructure portion Morphology Evolution rule; To mensuration four parts of energetic material component thermal constant, specifically comprise the following steps:
Step 1: by thermal capacitance and the temperature conductivity of DSC method and laser heat conduction method determination component material;
Step 2: determine Thermal Decomposition Mechanism function and parameter based on DSC-TG test;
Step 3: obtain energetic material surface topography with the Evolution of temperature by scanning electron microscope test, carry out quantitative test, show that surface topography is with Temperature Evolution rule;
Step 4: tested by μ CT and obtain the Evolution of energetic material internal morphology with temperature, and carry out quantitative test, compared with surface topography Evolution, the foundation for numerical model provides basis;
Step 5: the result summing up above four steps, draws the ermal physics model of energetic material based on thermal conduction study equation (3) and structure evolution rule:
ρ C d T d t = λ ▿ 2 T + S - - - ( 3 )
Wherein ρ is density, C is specific heat capacity, T is temperature, t is the time, λ is coefficient of heat conductivity, S is chemical heat release item;
Following General expression is had for chemical heat release item S
Wherein Q is the chemical heat release of unit quality, α is the mass percent that energetic material has reacted away.
2. the modeling method of focus physical model carefully seen by a kind of energetic material according to claim 1, it is characterized in that: the concrete grammar of " thermal capacitance and the temperature conductivity by DSC method and laser heat conduction method determination component material " described in step 1 is:
Step 1.1 adopts means of differential scanning calorimetry DSC method to obtain the thermal capacitance containing energy particle and adhesive substrate
High pure nitrogen atmosphere, flow velocity is 30-50ml/min; It is 0.5-1.5mm that adhesive substrate sample is processed into thickness in advance, and diameter is the smooth wafer type test specimen of 5-7mm; Containing can directly load in sample disc by granulated powder sample, during dress sample, gently sample disc to be shaken, so that the Contact of sample room, sample and dish is good.From room temperature 25 degrees Celsius, according to certain heating rate (general 1 ~ 10 degree Celsius/min) heating sample, until sample volatilizees completely, obtain the DSC curve of sample.The thermal capacitance of sample is calculated according to curve;
Step 1.2: adopt laser heat conduction method to obtain the temperature conductivity containing energy particle and adhesive substrate
To be processed into diameter in advance containing energy particle and adhesive substrate is 10-14mm, and error is less than 1.5mm; Thickness 0.5-1.5mm, error is less than the smooth wafer type test specimen of 0.5mm.The test specimen made is put into conductometer, heats test specimen, to 400 degrees Celsius according to certain heating rate (general 1 ~ 10 degree Celsius/min), often heat up 50 degrees Celsius, obtain its coefficient of heat conductivity by probe, every test specimen obtains 5 values, by averaging, obtain its temperature conductivity.
3. the modeling method of focus physical model carefully seen by a kind of energetic material according to claim 1, it is characterized in that: the concrete grammar of " thermal capacitance and the temperature conductivity by DSC method and laser heat conduction method determination component material " described in step 2 is:
Step 2.1: component material (containing energy particle and bonding agent) the DSC curve under four kinds of heating rates obtaining energetic material, four kinds of temperature be respectively 1 DEG C/min, 5 DEG C/min, 10 DEG C/min, 15 DEG C/min, for calculating the Arrhenius parameter of component, comprise reaction activity, pre-exponential factor, mechanism function, computing method are as follows:
Non-isothermal Kinetics Kissinger equation (1) and Coats-Redfern equation (2) is adopted jointly to determine chemical reaction kinetic parameters and the mechanism function of energetic material component: first to obtain the gentle reaction depth value in DTG peak from the TG curve of four kinds of heating rates of institute's test specimens, obtain reaction activity and pre-exponential factor with Kissinger equation, then determine g (α) function by Coats-Redfern equation;
l n ( β T p 2 ) = l n A R E a - E a RT p - - - ( 1 )
l n ( g ( α ) T 2 ) = l n A R βE a [ 1 - 2 R T E a ] - E a R T - - - ( 2 )
Be wherein β heating rate, T pfor peak temperature, T is arbitrary temperature in thermal decomposition process, E afor apparent activation energy, A is pre-exponential factor, and R is gas law constant, and 8.314J/K.mol, g (α) are mechanism function integrated form, and α is reaction depth;
Step 2.2: obtain energetic material component material (containing energy particle and bonding agent) the TG curve under heating rate is 5 DEG C/min, for the evolution of comparing calculation material with temperature geometrical morphology.
4. the modeling method of focus physical model carefully seen by a kind of energetic material according to claim 1, it is characterized in that: the concrete grammar of " the obtaining the Evolution of energetic material surface topography with temperature by scanning electron microscope test; carry out quantitative test, show that surface topography is with Temperature Evolution rule " described in step 3 is:
Step 3.1: obtain containing energy particle thin sight surface topography picture at different temperatures, for calculating containing providing basis with Temperature Evolution curve by granule-morphology;
Step 3.2: obtain adhesive film thin sight surface topography picture at different temperatures, for research adhesive film pattern provides foundation with Temperature Evolution rule.
5. the modeling method of focus physical model carefully seen by a kind of energetic material according to claim 1, it is characterized in that: described in step 3 " tested by μ CT and obtain the energetic material internal morphology Evolution with temperature; and carry out quantitative test, compared with surface topography Evolution " concrete grammar be:
Step 4.1: obtain containing energy particle thin sight internal morphology picture at different temperatures, for count particles pattern provides basis with Temperature Evolution curve;
Step 4.2: obtain energetic material thin sight internal morphology picture at different temperatures, for research energetic material pattern provides foundation with Temperature Evolution.
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CN112129890A (en) * 2020-08-17 2020-12-25 西安近代化学研究所 Method for accurately obtaining kinetic parameters of energetic material synthesis reaction process

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CN111323448A (en) * 2020-04-22 2020-06-23 中国工程物理研究院总体工程研究所 Multi-temperature-zone hot baking test device for energetic material product
CN112129890A (en) * 2020-08-17 2020-12-25 西安近代化学研究所 Method for accurately obtaining kinetic parameters of energetic material synthesis reaction process
CN112129890B (en) * 2020-08-17 2022-10-25 西安近代化学研究所 Method for accurately obtaining kinetic parameters of energetic material synthesis reaction process

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