CN105548237B - A kind of energetic material carefully sees the modeling method of hot spot physical model - Google Patents
A kind of energetic material carefully sees the modeling method of hot spot physical model Download PDFInfo
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Abstract
The invention belongs to the thermally safe technical field of energetic material, it is related to the modeling method that a kind of energetic material carefully sees ermal physics model.Including：The determination of Thermal Decomposition Mechanism function and parameter；Research to energetic material Microstructures Topography Evolution；Research to energetic material microstructure portion Morphology Evolution rule；To four parts of measurement of energetic material component thermal constant.The present invention is compared with the existing technology advantageous in that：This method has fully considered characteristic specific to energetic material self-inflicted injury, for the providing convenience property of selection and versatility of the INTERFACE MODEL parameter that energetic material microscopic damage numerical simulation uses, actual feature and process are predicted with comprehensive simulated, it establishes the physical analogy hierarchy of criteria and meets the thin sight ermal physics model of criterion, it is full-featured, be easily achieved.
Description
Technical field
The invention belongs to the thermally safe technical field of energetic material, it is related to the modeling that a kind of energetic material carefully sees ermal physics model
Method.
Background technique
Energetic material is thermally decomposed, the release of heat is usually accompanied by.If thermally decomposing discharged heat cannot expand
It is scattered to ambient enviroment, it would be possible to cause spontaneous combustion even explosion accident.
Chemical reaction-heat transfer model that macroscopical homogeneous is assumed is mainly based upon for thermally safe physical model at present, this
Model is well used during the roasting combustion of emulation macroscopic view, but cannot be disclosed using the simulation model that macroscopic view homogenizes containing energy
The thermally safe profound mechanism of material, formula design thermally safe for energetic material and risk do not have prediction effect.
The meso-scale of energetic material determines its thermally safe and thermal explosion mechanism, and energetic material is non-equal on meso-scale
Matter, it can be regarded as the three-phase as composed by oxidizing agent pellets, adhesive substrate and bonding interface band between the two
Inhomogeneous composite materials.Interface and each component are in warm between the inconsistent heat transfer property of each component and decomposition caused heat release performance, component
The inconsistent chemical reaction mechanism followed in decomposable process, and in thermal decomposition process inside each component and component boundary
The complicated structure evolution that face is occurred, these are all the complexity for determining that energetic material is thermally safe.
In order to disclose the mechanism of the thermally safe profound level of energetic material, the comprehensive a variety of macro mesoscale experiments methods of the present invention, from containing
Can the Thermal Decomposition Kinetic Parameters and mechanism function of material and its component, the Microstructures Topography of energetic material and its component drill
The microstructure portion Morphology Evolution rule of law, energetic material and its component, the survey to energetic material component thermal constant
Fixed four aspects expansion, carefully sees hot spot physical model to establish correct energetic material.
Have in the pervious document in the prior art, retrieved of the present invention：[1] temperature such as Liu Libin are to propellant powder safety
[D] trajectory journal .2004 is calculated with the numerical value of energy affect：2；[2] inscription on pottery files numerical heat transfer [M] Xi'an Communications University
Publishing house, 2001；[3] in the bright confined space of Du Zhi chemical reacting flow the Beijing thermal ignition [D]：Beijing Institute of Technology,
1993；[4] the roasting combustion mechanism study of Jing Song Ji condensed explosive and the Changsha Two-dimensional numerical simulation [D]：The National University of Defense technology, 2004；
Above-mentioned document is generic technology relevant to the technology of the present invention theme, still, in terms of disclosure of that, it is not yet found that closing
Energetic material carefully sees the report of ermal physics model building method.
Summary of the invention
According to above-mentioned background technique, it is an object of the present invention to be the research thermally safe mechanism of energetic material and thermally safe
Critical-temperature and the prediction for delay time of exploding provide foundation, and providing one kind for improvement energetic material thermal stability formula being capable of structure
The energetic material for building high quality and high efficiency carefully sees the modeling method of hot spot physical model.
Now present inventive concept and technical solution are described below：
Basic conception of the invention is to consider microscopical structure formation and developing the thermal physical characteristic with temperature to component material
Can influence, the influence factor comprehensive and reasonable of consideration, and form it is simple, it is easy to use under the premise of, thin hot spot physics is seen to it
The method for building up of model is described, and this method includes：The determination of Thermal Decomposition Mechanism function and parameter；To energetic material micro-structure
The research of surface topography Evolution；Research to energetic material microstructure portion Morphology Evolution rule；To energetic material component
Four parts of measurement of thermal constant, specifically include following steps：
Step 1：The thermal capacitance and thermal conductivity of component material are determined by DSC method and the thermally conductive method of laser；
Step 2：It is tested based on DSC-TG and determines Thermal Decomposition Mechanism function and parameter；
Step 3：It is tested by scanning electron microscope and obtains energetic material surface topography with the Evolution of temperature, quantitatively divided
Analysis obtains surface topography with Temperature Evolution rule；
Step 4：It is tested by μ CT and obtains energetic material internal morphology with the Evolution of temperature, and carry out quantitative analysis,
Compared with surface topography Evolution, basis is provided for the foundation of numerical model；
Step 5：That summarizes the above four steps contains energy material as a result, obtaining based on thermal conduction study equation (3) and structure evolution rule
The ermal physics model of material：
Wherein ρ is density, C is specific heat capacity, T is temperature, t is the time, λ is thermal coefficient, S is chemical heat release item；
There is following General expression for chemical heat release item S
Wherein Q is the chemical heat release of unit quality, α is mass percent that energetic material has reacted away.
The present invention further provides the modeling methods that a kind of energetic material carefully sees ermal physics model, it is characterised in that：Step 1
Described in the specific method of " thermal capacitance and thermal conductivity of component material are determined by DSC method and the thermally conductive method of laser " be：
Step 1.1 obtains the thermal capacitance containing energy particle and adhesive substrate using differential scanning calorimetry DSC method.
High pure nitrogen atmosphere, flow velocity 30-50ml/min；Adhesive substrate sample is pre-machined into a thickness of 0.5-
1.5mm, diameter are the smooth wafer type test specimen of 5-7mm；The granulated powder sample containing energy is directly loadable into sample disc, when filling sample
Sample disc is gently shaken, it is good to be contacted between sample room, sample and disk.From 25 degrees Celsius of room temperature, according to certain heating speed
Rate (general 1~10 degree Celsius/min) heating sample obtains the DSC curve of sample until sample volatilizees completely.According to curve meter
Calculation obtains the thermal capacitance of sample；
Step 1.2：Thermal conductivity containing energy particle and adhesive substrate is obtained using the thermally conductive method of laser.
Energy particle will be contained and diameter is pre-machined into as 10-14mm in adhesive substrate, error is less than 1.5mm；Thickness 0.5-
1.5mm, error are less than the smooth wafer type test specimen of 0.5mm.The test specimen made is put into conductometer, according to certain heating
Rate (general 1~10 degree Celsius/min) heats test specimen, until 400 degrees Celsius, every 50 degrees Celsius of heating obtains it by probe and leads
Hot coefficient, every test specimen obtain 5 values, by being averaged, obtain its thermal conductivity.
The present invention further provides the modeling methods that a kind of energetic material carefully sees ermal physics model, it is characterised in that：Step 2
Described in the specific method of " tested based on DSC-TG and determine Thermal Decomposition Mechanism function and parameter " be：
Step 2.1 obtains DSC of the component material (particle containing energy and adhesive) of energetic material under four kinds of heating rates
Curve, four kinds of temperature are respectively 1 DEG C/min, 5 DEG C/min, 10 DEG C/min, 15 DEG C/min, for calculating the Arrhenius of component
Parameter, including reaction activity, pre-exponential factor, mechanism function, calculation method are as follows：
The material containing energy is determined using non-isothermal Kinetics Kissinger equation (1) and Coats-Redfern equation (2) jointly
Expect the chemical reaction kinetic parameters and mechanism function of component：It is obtained first from the TG curve of four kinds of heating rates of institute's test specimens
The mild reaction depth value in the peak DTG, obtains reaction activity and pre-exponential factor with Kissinger equation, then pass through Coats-
Redfern equation determines g (α) function.
It is wherein β heating rate, TpFor peak temperature, T is any temperature, E in thermal decomposition processaFor apparent activation energy, A is
Pre-exponential factor, R are gas 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 (particle containing energy and adhesive) in the case where heating rate is 5 DEG C/min
TG curve, for comparing calculation material with the evolution of temperature geometrical morphology.
The present invention further provides the modeling methods that a kind of energetic material carefully sees ermal physics model, it is characterised in that：Step 3
Described in " by scanning electron microscope test obtain energetic material surface topography with temperature Evolution, carry out quantitative analysis, obtain
Out surface topography with Temperature Evolution rule " specific method be：
Step 3.1 obtains the thin sight surface topography picture of the particle containing energy at different temperatures, to calculate the granule-morphology containing energy
Basis is provided with Temperature Evolution curve；
Step 3.2 obtains the thin sight surface topography picture of adhesive film at different temperatures, to study adhesive film
Pattern provides foundation with Temperature Evolution rule.
The present invention further provides the modeling methods that a kind of energetic material carefully sees ermal physics model, it is characterised in that：Step 4
Described in " tested by μ CT and obtain energetic material internal morphology with the Evolution of temperature, and quantitative analysis is carried out, with table
Face Morphology Evolution rule compares " specific method be：
Step 4.1 obtains the thin sight internal morphology picture of the particle containing energy at different temperatures, is to calculate granule-morphology with temperature
It spends evolution curve and basis is provided；
Step 4.2 obtains the thin sight internal morphology picture of adhesive substrate at different temperatures, to study adhesive substrate
Pattern provides foundation with Temperature Evolution.
The present invention is compared with the existing technology advantageous in that：This method has fully considered that energetic material self-inflicted injury institute is special
Some characteristics, the providing convenience property of selection of INTERFACE MODEL parameter used for the numerical simulation of energetic material microscopic damage and general
Property, actual feature and process are predicted with comprehensive simulated, the physical analogy hierarchy of criteria is established and meets the hot object of carefully sight of criterion
Model is managed, it is full-featured, be easily achieved.
Specific embodiment
For below will be with HTPB propellant (for the particle containing energy for AP particle, adhesive substrate is fourth hydroxyl HTPB), by right
Its thin thin sight ermal physics model modelling approach of building explanation for seeing hot spot physical model.
Step 1：The thermal capacitance and thermal conductivity of component material are determined by DSC method and the thermally conductive method of laser.
Step 1.1 obtains the thermal capacitance containing energy particle and adhesive substrate using differential scanning calorimetry DSC method.
High pure nitrogen atmosphere, flow velocity 40ml/min；Adhesive substrate sample is pre-machined into a thickness of 1mm, and diameter is
The smooth wafer type test specimen of 6mm；The granulated powder sample containing energy is directly loadable into sample disc, gently to shake sample disc when filling sample,
It is good to be contacted between sample room, sample and disk.From 25 degrees Celsius of room temperature, according to certain heating rate, (general 1~10 is taken the photograph
Family name's degree/min) heating sample until sample volatilizees completely obtains the DSC curve of sample.The heat of sample is calculated according to curve
Hold.
Step 1.2 obtains the thermal conductivity containing energy particle and adhesive substrate using the thermally conductive method of laser.
Energy particle will be contained and diameter is pre-machined into as 12mm, error 1mm in adhesive substrate；Thickness 1.5mm, error are
The smooth wafer type test specimen of 0.5mm.The test specimen made is put into conductometer, according to certain heating rate (general 1~10
Degree Celsius/min) heating test specimen, until 400 degrees Celsius, every 50 degrees Celsius of heating obtains its thermal coefficient, every test specimen by probe
5 values are obtained, by being averaged, obtain its thermal conductivity.
Step 2：It is tested based on DSC-TG and determines AP and HTPB Thermal Decomposition Mechanism function and parameter.
AP and HTPB is obtained under four kinds of heating rates (respectively 1 DEG C/min, 5 DEG C/min, 10 DEG C/min, 15 DEG C/min)
DSC curve, for calculating the Arrhenius parameter (including reaction activity, pre-exponential factor, mechanism function) of component.It calculates
Method is as follows：
The material containing energy is determined using non-isothermal Kinetics Kissinger equation (1) and Coats-Redfern equation (2) jointly
Expect the chemical reaction kinetic parameters and mechanism function of component：It is obtained first from the TG curve of four kinds of heating rates of institute's test specimens
The mild reaction depth value in the peak DTG, obtains reaction activity and pre-exponential factor with Kissinger equation, then pass through Coats-
Redfern equation determines g (α) function.
The parameter that test measures test specimen (AP and HTPB) is as shown in Table 1 and Table 2：
The chemical reaction kinetic parameters of 1 film of table
| Activation energy | Pre-exponential factor ln (A) | Mechanism function g (α) | Mechanism |
| 87.5 | 9.93 | -ln(1-α) | Nucleation and growth |
2 AP reactive kinetics parameters of table and mechanism function
| Stage | Activation energy | Pre-exponential factor | Mechanism function g (α) | Mechanism |
| Low-temperature decomposition section | 167.3 | 29.55 | [-ln(1-α)]1/2 | Nucleation and growth equation |
| Changeover portion | 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：It is tested by scanning electron microscope and obtains AP and HTPB surface topography with the Evolution of temperature, quantitatively divided
Analysis obtains surface topography with Temperature Evolution rule.
Step 3.1 obtains the thin sight surface topography picture of AP particle at different temperatures, to calculate granule-morphology with temperature
Evolution curve provides basis；
Step 3.2 obtains the thin sight surface topography picture of HTPB film at different temperatures, to study adhesive film pattern
Foundation is provided with Temperature Evolution rule.
Surface topography Evolution through test measurement test specimen is as shown in table 3.
The variation of 3 different temperatures AP surface voids rate of table
| Temperature/DEG C | 100 | 150 | 200 | 230 | 280 | 330 | 380 |
| Hole rate/% | 0 | 0 | 0 | 2.34 | 6.02 | 19.84 | 70 |
Through observation and analysis as it can be seen that the evolutionary process of surface topography is divided into three phases when HTPB film heats：First stage：
Original uniform shape heat shrinkable；Second stage：Fold after contraction；Phase III：Fold degree is constantly aggravated.
Step 4：It is tested by μ CT and obtains AP and HTPB internal morphology with the Evolution of temperature, and carry out quantitative analysis,
Compared with surface topography Evolution, basis is provided for the foundation of numerical model.
The thin sight internal morphology picture of AP particle at different temperatures is obtained, to calculate granule-morphology with Temperature Evolution curve
Basis is provided, AP inner cavity rate varies with temperature as shown in table 4.
The variation of 4 different temperatures AP inner cavity rate of table
| Temperature/DEG C | 100 | 150 | 200 | 230 | 280 | 330 |
| Hole rate/% | 0 | 0 | 0 | 2.01 | 6.54 | 21.05 |
Step 5：Summarize the above four steps as a result, show that fourth hydroxyl pushes away based on thermal conduction study equation (3) and structure evolution rule
Ermal physics model into agent includes three parts：HTPB thermal decomposition and heat transfer, the thermal decomposition of AP particle and heat transfer, AP-HTPB
Interface develops.Multiple chemical reactions occur for AP particle in by thermal decomposition process, and the heat of generation is transmitted by the interface AP-HTPB
Into HTPB, HTPB thermal coefficient is lower, and performance is relatively stable in thermal histories, is formed about at the interface AP-HTPB larger
Temperature gradient starts micropore occur at the same time inside AP particle, the interface AP also starts to shrink and the interface AP-HTPB is caused to pass
Hot property further declines.
Claims (1)
1. the modeling method that a kind of energetic material carefully sees hot spot physical model, it is characterised in that：Consider microscopical structure formed and
It develops and influence of the temperature to the thermophysical property of component material, method for building up that hot spot physical model is carefully seen to it is retouched
It states, this method includes：The determination of Thermal Decomposition Mechanism function and parameter；Energetic material Microstructures Topography Evolution is ground
Study carefully；Research to energetic material microstructure portion Morphology Evolution rule；To measurement four of energetic material component thermal constant
Part specifically includes following steps：
Step 1：The thermal capacitance and thermal conductivity of component material are determined by DSC method and the thermally conductive method of laser；
Step 1.1 obtains the thermal capacitance containing energy particle and adhesive substrate using differential scanning calorimetry DSC method
High pure nitrogen atmosphere, flow velocity 30-50ml/min；Adhesive substrate sample is pre-machined into a thickness of 0.5-1.5mm, directly
Diameter is the smooth wafer type test specimen of 5-7mm；The granulated powder sample containing energy is directly loadable into sample disc, gently to shake sample when filling sample
Product disk is good to contact between sample room, sample and disk；From 25 degrees Celsius of room temperature, examination is heated according to certain heating rate
Sample obtains the DSC curve of sample until sample volatilizees completely；The thermal capacitance of sample is calculated according to curve, wherein certain
Heating rate is 1~10 degree Celsius/min；
Step 1.2：Thermal conductivity containing energy particle and adhesive substrate is obtained using the thermally conductive method of laser
Energy particle will be contained and diameter is pre-machined into as 10-14mm in adhesive substrate, error is less than 1.5mm；Thickness 0.5-
1.5mm, error are less than the smooth wafer type test specimen of 0.5mm；The test specimen made is put into conductometer, according to certain heating
Rate heats test specimen, until 400 degrees Celsius, every 50 degrees Celsius of heating obtains its thermal coefficient by probe, and each test specimen obtains 5
A value obtains its thermal conductivity by being averaged, wherein certain heating rate is 1~10 degree Celsius/min；
Step 2：It is tested based on DSC-TG and determines Thermal Decomposition Mechanism function and parameter；
Step 2.1：Obtain the component material of energetic material, the DSC curve under four kinds of heating rates, the wherein group of energetic material
Point material include containing can particle and adhesive substrate, 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 material, including reaction activity, pre-exponential factor, mechanism function, calculating side
Method is as follows：
Energetic material is determined using non-isothermal Kinetics Kissinger equation (1) and Coats-Redfern equation (2) jointly
The chemical reaction kinetic parameters and mechanism function of component material：It is obtained first from the TG curve of four kinds of heating rates of institute's test specimens
The mild reaction depth value in the peak DTG is obtained, obtains reaction activity and pre-exponential factor with Kissinger equation, then pass through Coats-
Redfern equation determines g (α) function；
Wherein β is heating rate, TpFor peak temperature, T is any temperature, E in thermal decomposition processaFor apparent activation energy, A is before referring to
The factor, R are gas constant, and 8.314J/K.mol, g (α) are mechanism function integrated form, and α is reaction depth；
Step 2.2：The component material for obtaining energetic material, the TG curve in the case where heating rate is 5 DEG C/min, wherein energetic material
Component material include containing can particle and adhesive substrate, for comparing calculation material with the evolution of temperature geometrical morphology；
Step 3：It is tested by scanning electron microscope and obtains energetic material surface topography with the Evolution of temperature, carry out quantitative analysis,
Obtain surface topography with Temperature Evolution rule；
Step 3.1：The thin sight surface topography picture of the particle containing energy at different temperatures is obtained, is to calculate the granule-morphology containing energy with temperature
It spends evolution curve and basis is provided；
Step 3.2：The thin sight surface topography picture of adhesive substrate at different temperatures is obtained, to study adhesive substrate pattern
Foundation is provided with Temperature Evolution rule；
Step 4：It is tested by μ CT and obtains energetic material internal morphology with the Evolution of temperature, and carry out quantitative analysis, with table
Face Morphology Evolution rule compares, and provides basis for the foundation of numerical model；
Step 4.1：The thin sight internal morphology picture of the particle containing energy at different temperatures is obtained, is to calculate the granule-morphology containing energy with temperature
It spends evolution curve and basis is provided；
Step 4.2：The thin sight internal morphology picture of adhesive substrate at different temperatures is obtained, to study adhesive substrate pattern
Foundation is provided with Temperature Evolution；
Step 5：Summarize the above four steps as a result, obtain energetic material based on thermal conduction study equation (3) and structure evolution rule
Ermal physics model：
Wherein ρ is density, C is specific heat capacity, T is temperature, t is the time, λ is thermal coefficient, S is chemical heat release item；It is described
Ermal physics model include three parts：Adhesive substrate thermal decomposition and heat transfer, the thermal decomposition of the particle containing energy and heat transfer contain energy
Particle/basal body interface develops；
There is following General expression for chemical heat release item S
Wherein Q is the chemical heat release of unit quality, α is mass percent that energetic material has reacted away.
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| CN1873411A (en) * | 2005-06-03 | 2006-12-06 | 中国科学院力学研究所 | Device for testing deflagrability of condensed fire detonator under condition of high termerature and high pressure |
| CN103018276A (en) * | 2011-09-28 | 2013-04-03 | 南京理工大学 | Method for evaluating thermal inductance of liquid energetic material |
| CN103353463A (en) * | 2013-06-14 | 2013-10-16 | 西安近代化学研究所 | Energetic material thermal stability and thermal safety test device and method |
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| US6406918B1 (en) * | 1999-01-25 | 2002-06-18 | University Of Massachusetts | Thermal analysis for detection and identification of explosives and other controlled substances |
| ES2909667T3 (en) * | 2013-03-15 | 2022-05-09 | Charles Stark Draper Laboratory Inc | System and method for a microfluidic calorimeter |
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| CN1873411A (en) * | 2005-06-03 | 2006-12-06 | 中国科学院力学研究所 | Device for testing deflagrability of condensed fire detonator under condition of high termerature and high pressure |
| CN103018276A (en) * | 2011-09-28 | 2013-04-03 | 南京理工大学 | Method for evaluating thermal inductance of liquid energetic material |
| CN103353463A (en) * | 2013-06-14 | 2013-10-16 | 西安近代化学研究所 | Energetic material thermal stability and thermal safety test device and method |
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