CN103776776A - Method and device for researching quick reaction mechanism of energetic material - Google Patents
Method and device for researching quick reaction mechanism of energetic material Download PDFInfo
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Abstract
The invention discloses a method and device for researching the quick reaction mechanism of an energetic material. The method is characterized in that the device for researching the quick reaction mechanism of the energetic material is adopted. The method comprises the following steps: positioning a monochromator in the position of a primary product characteristic spectral line, and recording the intensity time history (namely, time history curve) of the characteristic spectral line through a digital oscilloscope after photoelectric conversion, so as to study the time history of chief constituents of the energetic material decomposed due to impact; simulating the dynamic characteristic curve of the quick reaction of the energetic material with a reaction power calculation program, and correcting the reaction passage of the quick reaction of the energetic material according to the experiment detected occurrence time, inflection point time and maximum peak time of the primary product. A simplified reaction model obtained according to the method focuses on a main path, abandons reaction with poor impact, and can accurately reflect the real processes of the quick reaction of the energetic material under practical experimental conditions.
Description
Technical field
The embodiments of the present invention relate to spectral measurement methods field, relate more specifically to study the method and apparatus of energetic material fast reaction mechanism.
Background technology
Energetic material is that a class itself has higher-energy performance, can discharge the material of large energy, and it is particularly extensive in the application of space flight, military project and other high-tech area, is therefore a focus for the research of energetic material reaction mechanism always.Want to study substance reaction mechanism, just must analyze the chemical dynamics process in course of reaction and decomposition channels, this is mainly to measure in real time according to the transient state of intermediate product.In this respect, various spectral analysis techniques can be used as a kind of means of surveying energetic material atom and molecule level, and the physical property that it is conducive to more in depth to understand more comprehensively material under shock wave changes and corresponding mechanism.
Since the eighties, energetic material being decomposed to microscopic mechanism abroad studies.Experimentally mainly adopt the technology such as molecular beam mass spectrometer, ultraviolet/visible absorption spectra, spontaneous Raman spectrometer, fourier transform infrared spectroscopy, but because energetic material fast-response time is that microsecond magnitude is even shorter, the response time of general instrument does not reach, therefore can not to middle and final product over time process study.External some mechanism adopts the technology such as laser-induced fluorescence (LIF), high power video and high-speed camera, although these methods can be differentiated the physics and chemistry process that material internal occurs in impact compress process, but these instruments are expensive, and some equipment importation is restricted, general unit and mechanism are difficult to buy.Therefore be domesticly mostly limited to thermoanalytical method, and heat analysis method be a kind of under slow temperature program(me) control the transformation of research material and the process of reaction, it can not really simulate the process of energetic material rapid reaction under high-temperature and high-pressure conditions (burning, blast etc.).These reasons have all greatly limited the research work of energetic material rapid reaction microscopic mechanism above.
For the problem that is applicable to impact transient state spectrum test equipment due to the very difficult bulk/volume buying of the reasons such as funds and the external restriction to high-tech technology, the present invention is assembled and is enabled to meet the requirement of impacting spectrum experiment by existing spectral instrument, and proposes a kind of new method and device that combines to study energetic material fast reaction mechanism with theoretical modeling and dynamic experiment.This method not only can greatly reduce experimental amount, and can real simulation state when energetic material rapid reaction, more closing to reality application.
Summary of the invention
Object of the present invention is to overcome existing impact transient state spectrum test equipment price costliness, import difficulty and the problem such as the more difficult research of reaction mechanism that energetic material is occurred within the utmost point short time, the impact transient state spectrum test device being mainly made up of monochromatic spectrometer, photomultiplier and oscillograph is provided, and proposes a kind of new method and device that combines to study ammonium nitrate class energetic material fast reaction mechanism with theoretical modeling and dynamic experiment.
The technical scheme that the present invention takes for technical solution problem is:
Theoretical combining with experiment is to study the effective method of energetic material reaction mechanism, is also energetic material research and development trend.Therefore the research of this project is carried out from experimental study and two aspects of theoretical research:
Experimentally: utilize take shock tube as loading tool, the transient state spectrum testing system being formed by many monochromatic spectrometers, energetic material rapid-action intermediate product signal is carried out to synchronous acquisition, utilize the signal data that obtains to carry out the dynamic characteristic of the reaction that corrected Calculation goes out.
In theory: we utilize Chemical Kinetics software to calculate the polymerization kinetics curves of (temperature and pressure are drawn by experiment) energetic material rapid-action intermediate product under our experiment condition.And to energetic material rapid-action reaction channel speed (K): K=AT
βa, β, E in exp (E/RT) adjust, what make that " 3 points " time of the change curve of adjusting the dynamic characteristic curve of rear reaction power process simulation and the primary product radiation intensity of measuring tries one's best coincide, and the reaction model obtaining after modification like this can reflect the true process of energetic material rapid-action under experiment condition comparatively accurately.
According to a first aspect of the invention, a kind of device of studying energetic material fast reaction mechanism is provided, it is characterized in that: comprise shock tube, sample fixing device and monochromatic spectrum testing system, wherein shock tube comprises portfire, drives section inflation inlet, experimental section inflation inlet, the first pressure transducer, the second pressure transducer, polyethylene film and optical fiber to export; Sample fixing device comprises optical fiber, annulus base and the sample sack of optical fiber observation panel, high-temperature pipe protection; Monochromatic spectrum testing system comprises light-dividing device, monochromatic spectrometer, photomultiplier, charge amplifier, digital oscilloscope and cable.
The further embodiment according to the present invention, sample fixing device be placed on the first pressure transducer under, to guarantee the time synchronized of pressure transducer and fiber optic recording data.
The further embodiment according to the present invention; optical fiber is coupled on sample fixing device by optical fiber observation panel; and end face shock motion direction dorsad; to prevent the false triggering of optical fiber; high-temperature pipe and corrugated tube protection for optical fiber, affect the transmission of light signal in order to avoid optical fiber sustains damage under high-temperature condition.
The further embodiment according to the present invention, shock wave pipe range 6.00m, internal diameter is 10cm; The first pressure transducer and the second pressure transducer interval 55cm, the first pressure transducer is 2.45m apart from shock tube end.
The further embodiment according to the present invention, the digital oscilloscope of selection bandwidth 500MHz, four-way, the photomultiplier of spectral range 300-650nm, reflective monochromatic spectrometer, the common silica fibre of diameter 0.9mm.
According to a second aspect of the invention, a kind of method that combines to study energetic material fast reaction mechanism by theoretical modeling and dynamic experiment is provided, it is characterized in that: use the device based on the blast of the dynamic mixing method research of shock wave ammonium nitrate explosive, this device comprises shock tube, sample fixing device and monochromatic spectrum testing system, and wherein shock tube comprises portfire, drives section inflation inlet, experimental section inflation inlet, the first pressure transducer, the second pressure transducer, polyethylene film and optical fiber to export; Sample fixing device comprises optical fiber, annulus base and the sample sack of optical fiber observation panel, high-temperature pipe protection; Monochromatic spectrum testing system comprises light-dividing device, monochromatic spectrometer, photomultiplier, charge amplifier, digital oscilloscope and cable; The method comprises:
Monochromator is positioned to primary product characteristic spectral line position, and after opto-electronic conversion, by digital oscilloscope recording feature spectral line Strength Changes in time, i.e. time history curve, inquires into energetic material with this and impacts the key component situation over time of decomposing; And
With reaction power calculation procedure simulation energetic material rapid-action dynamic characteristic curve, in conjunction with the time of occurrence of the primary product of measuring, flex point time and maximum peak time, energetic material rapid-action reaction channel is revised, original reaction channel is given suitable interpolation or deleted, and to the A in the speed K:K=AT β exp (E/RT) of reaction channel, β, E adjusts, wherein A is pre-exponential factor, β is humidity index, E is energy of activation, R is gas law constant, T is absolute temperature, make according to amended parameter institute matching curve and the primary product time of occurrence measuring in experiment and the flex point time out, what the maximum peak time tried one's best coincide, the simplification reaction model obtaining is thus considered emphatically predominating path, gives up the weak reaction of impact, can reflect exactly the true process of energetic material rapid-action under actual experiment condition.
The further embodiment according to the present invention, is characterized in that: the pressure signal P 1 receiving take the first pressure transducer in experiment is trigger pip, the zero point using the photosignal time t1 synchronous corresponding with pressure signal P 1 as record.
The further embodiment according to the present invention, shock wave pipe range 6.00m, internal diameter is 10cm; The first pressure transducer and the second pressure transducer interval 55cm, the first pressure transducer is 2.45m apart from shock tube end.
The further embodiment according to the present invention, the oscillograph of selection bandwidth 500MHz, four-way, the photomultiplier of spectral range 300-650nm, reflective monochromatic spectrometer, the common silica fibre of diameter 0.9mm.
The beneficial effect that the present invention has is:
Simple to operate, cost is lower; 2. transient state spectrum sensitivity will be far above thermoanalysis technology; And theoretical calculate to combine not only greatly reduce experimental amount, but also the kinetic curve of the reaction can corrected Calculation going out; 3. can real simulation state when energetic material explosive combustion, more closing to reality application.The fast reaction mechanism that this new method of the present invention is energetic material researched and proposed new approaches.
Accompanying drawing explanation
In the time reading by reference to the accompanying drawings below to the detailed description of exemplary embodiment, these and other object, feature and advantage will become apparent, in the accompanying drawings:
Fig. 1 be according to research energetic material fast reaction mechanism of the present invention device use status architecture schematic diagram;
Fig. 2 is the variation diagram of the radiation intensity of the monochrome spectrum of oscillograph recording; And
Fig. 3 is the kinetic curve of the product of reaction power process simulation.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further described.
As shown in Figure 1, a kind of device of studying energetic material fast reaction mechanism, comprises shock tube 1, sample fixing device 2 and monochromatic spectrum testing system 3; Wherein optical fiber 2-2, annulus base 2-3, sample sack 2-4, light-dividing device 3-1, monochromatic spectrometer 3-2, photomultiplier 3-3, charge amplifier 3-4, digital oscilloscope 3-5, the cable 3-6 of portfire 1-1, a driving section inflation inlet 1-2, experimental section inflation inlet 1-3, the first pressure transducer 1-4, the second pressure transducer 1-5, polyethylene film 1-6, optical fiber outlet 1-7, optical fiber observation panel 2-1, high-temperature pipe protection.
Whole experiment is carried out in shock tube 1, first shock tube 1 is sealed, and drives section inflation inlet 1-2 and experimental section inflation inlet 1-3 to be evacuated to 0.005MPa with vacuum pump respectively simultaneously.Driving section inflation inlet 1-2 to be filled with stoichiometric proportion is hydrogen and the oxygen of 2: 1, and reserved certain hour fully mixes it.With portfire 1-1 spark ignition, make hydrogen and oxygen gas mixture blast, break through after polyethylene film 1-6, in shock tube experiment section, just form shock wave (Fig. 1).Before experiment, energetic material is contained in sack 2-4, they are contained on sample fixing device 2.Sample fixing device 2 be placed on the first pressure transducer 1-4 under, to guarantee the time synchronized of pressure transducer and signal optical fibre record data.And optical fiber 2-2 is coupled on sample fixing device 2 by optical fiber observation panel 2-1; and end face shock motion direction dorsad; in case the false triggering of stop signal optical fiber, high-temperature pipe and corrugated tube protection for optical fiber, affect the transmission of light signal in order to avoid optical fiber sustains damage under high-temperature condition.Like this under incident blast wave effect, the energetic material in sack under intense shock wave effect rapidly towards periphery space shed and explosive reaction occur.
Record the intensity time changing curve (Fig. 2) of reaction intermediate characteristic spectral line by monochromatic spectrum testing system (monochromatic spectrometer 3-2, photomultiplier 3-3 and oscillograph 3-5).The light signal producing after exploding primer in experiment is through optical fiber 2-2 transmission, light-dividing device 3-1 light splitting, enters respectively three monochromatic spectrometer 3-2 (in advance by regulating the prism of monochromatic spectrometer 3-2 or the position, angle of grating can select the predetermined monochromatic light of outgoing).Light signal, after monochromatic spectrometer 3-2 dispersion, only has the monochromatic light of a certain wavelength can see through monochromator exit slit, completes light signal and is converted into after electric signal, by digital oscilloscope 3-5 recording voltage waveform through photomultiplier 3-3.
The pressure signal P 1 receiving take the first pressure transducer 1-4 in experiment is as trigger pip,
Because pressure signal and photosignal are synchronous recordings, therefore, zero point using at this moment synchronous corresponding with P1 photosignal time t1 as record, test signal ski-jump t2 is representing the time of occurrence of product so, test signal ski-jump t2 with record the Δ T duration of ignition (as shown in Figure 2) that time at zero point t1 interval is exactly this intermediate product.The same flex point that can measure intermediate product signal zero point and time to peak with the method time.
The working method of present embodiment is: the fast chemical reaction process of energetic material, under experiment condition, can regard the gas-phase reaction of chemical kinetics control as, and its reaction rate can represent with Arrhenius law
K＝AT
βexp(-E/RT) (1)
Wherein, A is pre-exponential factor; β is humidity index; E is energy of activation; R is gas law constant; T is absolute temperature.
Intend the kinetic curve by reaction product in the rapid reaction of CHEMKIN program calculating energetic material, according to the time of occurrence of multiple reaction product of measuring and the theoretical result of calculating of the poor contrast of time to peak, can obtain the parameter (Fig. 3) such as important products reaction channel and energy of activation in energetic material rapid reaction process under incident shock incentive condition.
Simulate energetic material rapid-action dynamic characteristic curve (Fig. 3) with reaction power calculation procedure, in conjunction with time of occurrence, flex point time and the maximum peak time (Fig. 2) of the primary product of measuring, energetic material rapid-action reaction channel is revised, original reaction channel is awarded suitable interpolation or deleted, and speed (K) to reaction channel: K=AT
βa, β, the E of exp (E/RT) award adjustment, make according to coincideing of trying one's best of curve out of amended parameter institute matching and the product time of occurrence measuring in experiment and flex point, peak-peak time, the simplification reaction model obtaining after revising is like this considered emphatically predominating path, gives up the weak reaction of impact.Can reflect comparatively accurately the true process of energetic material rapid-action under our experiment condition (High Temperature High Pressure) condition.
The gordian technique that the present invention can the Study of the Realization energetic material decomposes microscopic mechanism is:
Simulate energetic material rapid-action dynamic characteristic curve with reaction power calculation procedure in theory, in conjunction with time of occurrence, flex point time and the maximum peak time of the primary product of measuring, to the speed K=AT of energetic material rapid-action reaction channel
βthe parameter such as A, β, E of exp (E/RT) awards adjustment, makes will use up at utmost coincideing of amount according to curve out of amended parameter institute matching and the product time of occurrence measuring and flex point, peak-peak time in experiment.This is the key that reflects exactly the true process of energetic material rapid-action under experiment condition.
The long 6.00m of shock tube 1 in the present embodiment, internal diameter is 10cm; Two pressure transducer 1-4 of experimental section and 1-5 interval 55cm, the first pressure transducer 1-4 is 2.45m apart from shock tube end 1-7, driving section hydrogen and oxygen stoichiometric proportion is 2: 1, select TDS5054 oscillograph (bandwidth 500MHz, four-way), Phillips XP2262 type photomultiplier (spectral range 300-650nm), the reflective monochromator of WDF, YE5852 charge amplifier, optical fiber is common silica fibre (diameter 0.9mm).
Provided instructions of the present invention for the object illustrating and describe, but it is not intended to be exhaustive or be limited to the invention of disclosed form.It may occur to persons skilled in the art that a lot of modifications and variant.
Therefore; embodiment is for principle of the present invention, practical application being described better and making the other staff in those skilled in the art can understand following content and select and describe;; do not departing under the prerequisite of spirit of the present invention, all modifications of making and replacement all will fall in the protection domain of the present invention of claims definition.
Claims (9)
1. study the device of energetic material fast reaction mechanism for one kind, it is characterized in that: comprise shock tube, sample fixing device and monochromatic spectrum testing system, wherein shock tube comprises portfire, drives section inflation inlet, experimental section inflation inlet, the first pressure transducer, the second pressure transducer, polyethylene film and optical fiber to export; Sample fixing device comprises optical fiber, annulus base and the sample sack of optical fiber observation panel, high-temperature pipe protection; Monochromatic spectrum testing system comprises light-dividing device, monochromatic spectrometer, photomultiplier, charge amplifier, digital oscilloscope and cable.
2. device according to claim 1, is characterized in that: sample fixing device be placed on the first pressure transducer under, to guarantee the time synchronized of pressure transducer and fiber optic recording data.
3. device according to claim 1; it is characterized in that: optical fiber is coupled on sample fixing device by optical fiber observation panel; and end face shock motion direction dorsad; to prevent the false triggering of optical fiber; high-temperature pipe and corrugated tube protection for optical fiber, affect the transmission of light signal in order to avoid optical fiber sustains damage under high-temperature condition.
4. device according to claim 1, is characterized in that: shock wave pipe range 6.00m, and internal diameter is 10cm; The first pressure transducer and the second pressure transducer interval 55cm, the first pressure transducer is 2.45m apart from shock tube end.
5. method according to claim 1, is characterized in that: select the digital oscilloscope of bandwidth 500MHz, four-way, the photomultiplier of spectral range 300-650nm, reflective monochromatic spectrometer, the common silica fibre of diameter 0.9mm.
6. one kind combines to study the method for energetic material fast reaction mechanism by theoretical modeling and dynamic experiment, it is characterized in that: use the device based on the blast of the dynamic mixing method research of shock wave ammonium nitrate explosive, this device comprises shock tube, sample fixing device and monochromatic spectrum testing system, and wherein shock tube comprises portfire, drives section inflation inlet, experimental section inflation inlet, the first pressure transducer, the second pressure transducer, polyethylene film and optical fiber to export; Sample fixing device comprises optical fiber, annulus base and the sample sack of optical fiber observation panel, high-temperature pipe protection; Monochromatic spectrum testing system comprises light-dividing device, monochromatic spectrometer, photomultiplier, charge amplifier, digital oscilloscope and cable; The method comprises:
Monochromator is positioned to primary product characteristic spectral line position, and after opto-electronic conversion, by digital oscilloscope recording feature spectral line Strength Changes in time, i.e. time history curve, inquires into energetic material with this and impacts the key component situation over time of decomposing; And
With reaction power calculation procedure simulation energetic material rapid-action dynamic characteristic curve, in conjunction with time of occurrence, flex point time and the maximum peak time of the primary product of measuring, energetic material rapid-action reaction channel is revised, original reaction channel is given suitable interpolation or deleted, and speed K:K=AT to reaction channel
βa, β, E in exp (E/RT) adjust, wherein A is pre-exponential factor, β is humidity index, E is energy of activation, R is gas law constant, T is absolute temperature, makes according to coincideing of trying one's best of curve out of amended parameter institute matching and the primary product time of occurrence measuring in experiment and flex point time, maximum peak time; The simplification reaction model obtaining is thus considered emphatically predominating path, gives up the weak reaction of impact, can reflect exactly the true process of energetic material rapid-action under actual experiment condition.
7. method according to claim 6, is characterized in that: the pressure signal P 1 receiving take the first pressure transducer in experiment is trigger pip, the zero point using the photosignal time t1 synchronous corresponding with pressure signal P 1 as record.
8. method according to claim 6, is characterized in that: shock wave pipe range 6.00m, and internal diameter is 10cm; The first pressure transducer and the second pressure transducer interval 55cm, the first pressure transducer is 2.45m apart from shock tube end.
9. method according to claim 6, is characterized in that: select the oscillograph of bandwidth 500MHz, four-way, the photomultiplier of spectral range 300-650nm, reflective monochromatic spectrometer, the common silica fibre of diameter 0.9mm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104237205A (en) * | 2014-09-23 | 2014-12-24 | 清华大学 | Spectrum detection method and system for fluorine atom density in plasma etching process |
| CN110646459A (en) * | 2019-10-14 | 2020-01-03 | 中国工程物理研究院化工材料研究所 | Compatibility evaluation method of tetrazole-based energetic material based on gas product |
| CN112102892A (en) * | 2020-08-17 | 2020-12-18 | 西安近代化学研究所 | Method for determining temperature correction coefficient of energetic material chemical combination process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104237205A (en) * | 2014-09-23 | 2014-12-24 | 清华大学 | Spectrum detection method and system for fluorine atom density in plasma etching process |
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| CN110646459B (en) * | 2019-10-14 | 2021-12-17 | 中国工程物理研究院化工材料研究所 | Compatibility evaluation method of tetrazole-based energetic material based on gas product |
| CN112102892A (en) * | 2020-08-17 | 2020-12-18 | 西安近代化学研究所 | Method for determining temperature correction coefficient of energetic material chemical combination process |
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