CN110108749A - The measuring system and method for polymer matrix composites pyrolysis Kinetics Parameter - Google Patents
The measuring system and method for polymer matrix composites pyrolysis Kinetics Parameter Download PDFInfo
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- CN110108749A CN110108749A CN201910345297.8A CN201910345297A CN110108749A CN 110108749 A CN110108749 A CN 110108749A CN 201910345297 A CN201910345297 A CN 201910345297A CN 110108749 A CN110108749 A CN 110108749A
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- G—PHYSICS
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- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
- G01N7/16—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference by heating the material
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Abstract
The present invention relates to the measuring systems and method of a kind of polymer matrix composites pyrolysis Kinetics Parameter.The present invention is based on the barometric surveyings of materials pyrolysis gaseous products and material temperature to measure, obtain the temperature and pyrolysis weight loss data in pyrolytic process with strong association in time, materials pyrolysis kinetic parameter is pushed away by the way that identification method is counter, calculating process is simple, and can be suitably used for the measurement under different temperatures.The system includes spherical vacuum tank, baroceptor, laser, thermal imaging system, aspiration pump, vacuum valve, photodetector and data processing unit;Sample to be tested is placed in spherical vacuum tank, pass through laser irradiation sample to be tested, temperature information and barometric information in spherical vacuum tank are obtained using thermal imaging system, baroceptor, then obtains pyrolysis weight loss data, finally calculates the pyrolysis Kinetics Parameter of sample to be tested.
Description
Technical field
The invention belongs to material analysis test method field, it is related to a kind of polymer matrix composites pyrolysis Kinetics Parameter
Measuring system and method.
Background technique
Polymer matrix composites are a kind of very widely used functional materials, usually with epoxy resin, phenolic resin etc.
As matrix, using carbon fiber, glass fibre etc. as performance enhanced material.Resin is organic high molecular polymer, certain
At a temperature of pyrolysis can occur.This characteristic of resin make to study polymer matrix composites pyrolysis kinetics become to have very much must
It wants.
Existing pyrolysis Kinetics Parameter measurement method is based primarily upon the gravitational thermal analysis method of material, by thermogravimetry, shows
The material analysis means such as poor scanning calorimetry obtain the pyrolysis kinetics such as the pyrolysis activation energy, pre-exponential factor, the order of reaction of material
Parameter.
Thermogravimetry temperature rise rate is slower, and usual temperature rise rate is in tens degrees Celsius of level per minute.Such temperature
It is applicable for situations such as rising thermal cracking processing, the resin formula development of velocity on material.But high temperature rise rate is needed certain
In the case where, such as laser ablation polymer matrix composites, such temperature rise rate is then not suitable for the pyrolytic reaction of research material.
In order to provide the thermogravimetric analysis means of high temperature rise rate, existing method uses based on being transformed to thermogravimetric analyzer, such as passes through
Laser carries out crucible the mode such as to heat, but such mode, overall cost are very high.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of measurement systems of polymer matrix composites pyrolysis Kinetics Parameter
System and method, barometric surveying and material temperature based on materials pyrolysis gaseous products measure, when having strong in acquisition pyrolytic process
Between associated temperature and pyrolysis weight loss data, push away materials pyrolysis kinetic parameter by the way that identification method is counter, implementation is simple
And cost is relatively low.
Technical solution of the invention are as follows:
The present invention provides a kind of measuring systems of polymer matrix composites pyrolysis Kinetics Parameter:
Including spherical vacuum tank, baroceptor, laser, thermal imaging system, aspiration pump, vacuum valve, photodetector with
And data processing unit;
Sample to be tested is placed in spherical vacuum tank, the inner wall of spherical vacuum tank uses blackening process;
Transmission direction on spherical vacuum tank along laser offers laser light incident window and laser emitting window;
Laser light incident window described in laser face is placed, and is provided irradiation for the sample to be tested into spherical vacuum tank and is swashed
Light;
Photodetector be aligned laser light incident window place, for judge laser go out light when between, it is gentle as temperature
Buckle line time zero when, convenient for the time Synchronization Analysis of two kinds of experimental datas.
Thermal imaging system measurement window is offered on spherical vacuum tank;
Thermal imaging system face thermal imaging system measurement window is placed;
Baroceptor is mounted on spherical vacuum tank;
Aspiration pump is connected to by vacuum valve with the spherical vacuum tank;
Data processing unit is electrically connected with baroceptor, photodetector and thermal imaging system respectively.
Further, laser damages external environment after projecting spherical vacuum tank in order to prevent, which also wraps
Graphite screen is included, the graphite screen face laser emitting window is placed, for absorbing to the laser for projecting spherical vacuum tank.
Further, above-mentioned thermal imaging system measurement window face sample to be tested setting, laser are injected in spherical vacuum tank
Optical axis and the normal direction angle in sample to be tested irradiation face are less than 10 °.
Further, above-mentioned sample to be tested is suspended in spherical vacuum tank by filament.
Further, the sample rate of above-mentioned baroceptor is not less than 100Hz, and thermal imaging system sample rate is not less than 50Hz.
Based on the description of the above-mentioned measuring system topology layout to polymer matrix composites pyrolysis Kinetics Parameter, now to making
It is described in detail with the method that the system measures:
1) prepare sample to be tested, and weighed, installed to it;
Polymer matrix composites are prepared into laminar sample to be tested, first measure the initial mass m of sample to be tested0, then
The suspension of sample to be tested filament is fixed on to the central part of spherical vacuum tank;
2) vacuumize process is carried out to spherical vacuum tank;
Spherical vacuum tank is sealed, aspiration pump is started, opens vacuum valve, by gas path pipe by spherical vacuum tank
In air extraction, close vacuum valve after so that spherical vacuum tank is in vacuum state, and close aspiration pump;
3) the control program of log-on data processing unit, control thermal imaging system start to work, while acquire baroceptor and
The output voltage data of photodetector;
4) start laser emitting laser, laser irradiation carries out continuous heating on sample to be tested, to sample to be tested;
Thermal imaging system carries out test constantly to the temperature of sample to be tested, and the temperature curve T (t) measured is recorded at data
It manages in unit;
Baroceptor carries out test constantly to the pressure in spherical vacuum tank, and the pressure curve p (t) measured is recorded
In data processing unit;
Photodetector carries out test constantly to the scattering light of laser, and by the curve record measured in data processing unit
In;
5) laser stops irradiation, stops the control program of data processing unit again after a period of time, starts aspiration pump,
Vacuum valve is opened, the experiment gaseous products in spherical vacuum tank are discharged;
6) vacuum valve and aspiration pump are closed, after restoring the air pressure to atmospheric pressure in spherical vacuum tank, opens spherical vacuum
Tank takes out sample, measures its final mass mfinal;
7) to the initial mass m of sample to be tested0With final mass mfinalIt makes the difference, obtains the total mass loss Δ of sample to be tested
mfinal;
8) the pressure curve p (t) obtained according to baroceptor measurement obtains total gas pressure increment Delta pfinal;
9) pass through the total mass loss Δ m of samplefinalWith total gas pressure increment Delta pfinal, obtain the ratio η of air pressure and quality
=Δ mfinal/Δpfinal, mass loss curve Δ m (t)=η p (t) of sample is obtained by The Ideal-Gas Equation;
10) voltage curve measured according to photodetector obtains the Laser output moment, and damages this moment as quality
Lose curve, temperature curve zero when, both make to have strong association in time;
11) temperature obtained according to Arrhenius pyrolytic reaction equation, the mass loss curve of step 9) acquisition, step 4)
Degree information and identification method are fitted to obtain the pyrolysis Kinetics Parameter of sample to be tested;
The pyrolysis Kinetics Parameter includes pre-exponential factor A, activation energy, order of reaction n;
The Arrhenius pyrolytic reaction equation is specifically:
Wherein, R is mol gas constant.
Further, step 6) should carry out cleaning treatment to sample to be tested, go before measuring sample to be tested final mass
Except the product for being adhered to sample to be tested surface after reaction.
The invention has the following advantages:
1, measuring device structure of the invention is simple, and using the principle of laser irradiation, heating speed is fast (temperature rise rate is high),
Expend cheap, test is time-consuming short, and temperature rise rate adjustable range is wide, easy to adjust.
2, it is fitted to obtain resin base composite wood the present invention is based on Arrhenius pyrolytic reaction equation and identification method
Expect pyrolysis Kinetics Parameter, calculating process is simple, and can be suitably used for the measurement under different temperatures, wide adaptation range.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of measuring system of the present invention.
Appended drawing reference is as follows:
1- laser;2- laser light incident window;3- sample to be tested;4- laser emitting window;5- graphite screen;6- gold
Belong to filament;7- spherical vacuum tank;8- baroceptor;9- thermal imaging system measurement window;10- thermal imaging system;11- aspiration pump;
12- vacuum valve;13- gas path pipe;14- photodetector;15- data processing unit.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Following present a kind of specific embodiments of measuring system of the present invention, and referring to Fig. 1, which includes spherical true
Slack tank 7, laser 1, baroceptor 8, thermal imaging system 10, aspiration pump 11, vacuum valve 12, photodetector 14, graphite screen 5,
Filament 6 and data processing unit 15;
Wherein, the sample rate of baroceptor 8 is not less than 100Hz in the present embodiment, and 10 sample rate of thermal imaging system is not less than
50Hz。
The fixation of sample to be tested 3 is suspended in spherical vacuum tank 7 by filament 6, the inner wall of spherical vacuum tank 7 uses
Blackening process;(circular sheet-like structures that sample to be tested makes in the present embodiment for polymer matrix composites)
Transmission direction on spherical vacuum tank 7 along laser offers laser light incident window 2 and laser emitting window 4;Ball
Thermal imaging system measurement window 9 is offered on shape vacuum tank 7;It should be noted is that thermal imaging system measurement window 9 in the present embodiment
Face sample to be tested 3 is arranged, and optical axis and sample to be tested 3 that laser 1 is injected in spherical vacuum tank 7 irradiate the normal direction angle in face
Less than 10 °.
Photodetector 14, thermal imaging system 10 are installed in the outside of spherical vacuum tank 7,1 face laser light incident window 2 of laser
Incidence, for irradiating sample to be tested;5 face laser emitting window 4 of graphite screen is placed, for absorbing the laser of outgoing.Photoelectricity is visited
It surveys device and is then oriented more at the placement of laser light incident window, place judgement so that the higher scattered light signal of signal-to-noise ratio can be received
Foundation, at the time of for judging that laser starts irradiation;
10 face thermal imaging system measurement window 9 of thermal imaging system is placed, the temperature for real-time measurement sample to be tested;
Baroceptor 8 is mounted on spherical vacuum tank 7, for the atmospheric pressure value in real-time measurement spherical vacuum tank 7;
Aspiration pump 11 is connected to by vacuum valve 12 with the spherical vacuum tank 7, true for take out to spherical vacuum tank 7
Vacancy reason and discharge pernicious gas;
Data processing unit 15 is electrically connected with baroceptor 8, photodetector 14 and thermal imaging system 10 respectively, for controlling
The starting of thermal imaging system processed, and the voltage signal of baroceptor, photodetector is acquired, power is pyrolyzed for polymer matrix composites
It learns parameter and analysis offer input is provided.
Herein it should be understood that the data processing unit being previously mentioned in the present embodiment can be acquired and be deposited merely to only have
Store up the data collection system of data, such as measuring system, the Dewtron data of computer and NI c-RIO cabinet and module composition
Acquisition system, it can be achieved that voltage/current signals acquisition and preservation, triggering level signal output etc. functions, need at data
When reason calculates, data can be uploaded to computer and handled.
In addition to this, which, which can also be used, not only has acquisition and storage data function, but also has at data
The computer of function is managed, that is, acquisition, storage and calculation processing carry out on the same device, without what is exported, uploaded
Step;What is actually used in the present embodiment is exactly a computer with acquisition, storage and calculation processing ability.
Based on the introduction of the above-mentioned topology layout to the measurement, now the detailed process for using the system to measure is made
More description, step include: in detail
Step 1: detected materials being prepared into thin circular sample 3, first measure 3 initial mass m of sample to be tested0, then will be to
Sample 3 is fixed on the central part of spherical vacuum tank 7 with filament 6;
Step 2: spherical vacuum tank 7 being sealed, aspiration pump 11 is started, vacuum valve 12 is opened, passes through gas path pipe
13 extract the air in spherical vacuum tank 7 out, so that spherical vacuum tank is lain substantially in vacuum state, vacuum valve is closed after stablizing
Door 12 and aspiration pump 11;
Step 3: log-on data processing unit 15 controls program, and control thermal imaging system 10 is started to work, while acquiring air pressure transmission
The output voltage data of sensor 8 and photodetector 14;
Step 4: pending data processing unit 15 starts after acquiring data, starts 1 shoot laser of laser, and laser 1 goes out
Irradiating light beam is irradiated on sample to be tested 3 by laser light incident window 2 with the incident angle for being not more than 10 ° after homogenizing, and treats test sample
Product are heated, and the laser of transmission is incident on graphite screen 5 by laser emitting window 4;In the process, thermal imaging system 10 is to be measured
The temperature of sample 3 carries out test constantly, and the temperature information T (t) measured is recorded in data processing unit;Baroceptor
Pressure in 8 pairs of spherical vacuum tanks 7 carries out test constantly, and the pressure curve p (t) measured is recorded in data processing unit
In;Photodetector 14 carries out test constantly to the scattering light of laser, and the voltage curve measured is recorded in data processing list
In member;
Step 5: laser 1 stops irradiation, stops computer 15 again after a period of time and controls program, starts aspiration pump
11, vacuum valve 12 is opened, the gaseous products in spherical vacuum tank 7 are discharged;
Step 6: closing vacuum valve 12 and aspiration pump 11, after restoring the air pressure to atmospheric pressure in spherical vacuum tank 7, open
Spherical vacuum tank 7 takes out sample 3;
Step 7: cleaning treatment being carried out to sample to be tested 3, removes the product for being adhered to sample to be tested surface after reacting, then
To the final mass m of sample to be tested 3finalIt measures;
Step 8: being made the difference by the quality to sample to be tested after predose, obtain the total mass loss Δ of sample to be tested 3
mfinal;
Step 9: gas pressure curve p (t) in obtained tank being measured according to baroceptor 8, obtains total gas pressure increment Delta pfinal;
Step 10: passing through the total mass loss Δ m of samplefinalWith total gas pressure increment Delta pfinal, obtain air pressure and quality
Ratio η=Δ mfinal/Δpfinal, to obtain mass loss curve Δ m (t)=η p (t) of sample;
Step 11: the voltage curve measured according to photodetector obtains the Laser output moment, and using this moment as matter
Amount loss curve, temperature curve zero when, both make to have strong association in time;
Step 12: according to Arrhenius Arrhenius pyrolytic reaction equation, step 10 obtain mass loss curve,
The temperature information and identification method that step 4 obtains are fitted to obtain the pyrolysis Kinetics Parameter of sample to be tested;
Pyrolysis Kinetics Parameter includes pre-exponential factor A, activation energy, order of reaction n;
Arrhenius pyrolytic reaction equation is specifically:
Wherein, R is mol gas constant.
Claims (7)
1. a kind of measuring system of polymer matrix composites pyrolysis Kinetics Parameter, it is characterised in that: including spherical vacuum tank, gas
Pressure sensor, laser, thermal imaging system, aspiration pump, vacuum valve, photodetector and data processing unit;
Sample to be tested is placed in spherical vacuum tank, the inner wall of spherical vacuum tank uses blackening process;
Transmission direction on spherical vacuum tank along laser offers laser light incident window and laser emitting window;
Laser light incident window described in laser face is placed, and provides irradiation laser for the sample to be tested into spherical vacuum tank;
Photodetector be aligned laser light incident window place, for judge laser go out light when between;
Thermal imaging system measurement window is offered on spherical vacuum tank;
Thermal imaging system face thermal imaging system measurement window is placed;
Baroceptor is mounted on spherical vacuum tank;
Aspiration pump is connected to by vacuum valve with the spherical vacuum tank;
Data processing unit is electrically connected with baroceptor, photodetector and thermal imaging system respectively.
2. the measuring system of polymer matrix composites pyrolysis Kinetics Parameter according to claim 1, it is characterised in that: also
Including graphite screen, the graphite screen face laser emitting window is placed.
3. the measuring system of polymer matrix composites pyrolysis Kinetics Parameter according to claim 1, it is characterised in that: institute
The setting of thermal imaging system measurement window face sample to be tested is stated, the optical axis and sample to be tested that laser is injected in spherical vacuum tank irradiate face
Normal direction angle less than 10 °.
4. the measuring system of polymer matrix composites pyrolysis Kinetics Parameter according to claim 1, it is characterised in that: institute
Sample to be tested is stated to be suspended in spherical vacuum tank by filament.
5. the measuring system of polymer matrix composites pyrolysis Kinetics Parameter according to claim 1, it is characterised in that: institute
The sample rate of baroceptor is stated not less than 100Hz, thermal imaging system sample rate is not less than 50Hz.
6. a kind of measurement method of polymer matrix composites pyrolysis Kinetics Parameter, which is characterized in that using such as claim 1 institute
The measuring system stated realizes the measurement of sample to be tested pyrolysis Kinetics Parameter by following steps:
1) prepare sample to be tested, and weighed, installed to it;
Polymer matrix composites are prepared into laminar sample to be tested, first measure the initial mass m of sample to be tested0, then will be to be measured
Sample filament suspends the central part for being fixed on spherical vacuum tank;
2) vacuumize process is carried out to spherical vacuum tank;
Spherical vacuum tank is sealed, aspiration pump is started, opens vacuum valve, it will be in spherical vacuum tank by gas path pipe
Air extraction, closes vacuum valve after so that spherical vacuum tank is in vacuum state, and close aspiration pump;
3) the control program of log-on data processing unit, control thermal imaging system is started to work, while acquiring baroceptor and photoelectricity
The output voltage data of detector;
4) start laser emitting laser, laser irradiation carries out continuous heating on sample to be tested, to sample to be tested;
Thermal imaging system carries out test constantly to the temperature of sample to be tested, and the temperature curve T (t) measured is recorded in data processing list
In member;
Baroceptor carries out test constantly to the pressure in spherical vacuum tank, and the pressure curve p (t) measured is recorded in number
According in processing unit;
Photodetector carries out test constantly to the heat dissipation light of laser emitting laser, and the voltage curve measured is recorded in number
According in processing unit;
5) laser stops irradiation, stops the control program of data processing unit again after a period of time, starts aspiration pump, opens
Experiment gaseous products in spherical vacuum tank are discharged vacuum valve;
6) vacuum valve and aspiration pump are closed, after restoring the air pressure to atmospheric pressure in spherical vacuum tank, spherical vacuum tank is opened, takes
Sample out measures its final mass mfinal;
7) to the initial mass m of sample to be tested0With final mass mfinalIt makes the difference, obtains the total mass loss Δ of sample to be tested
mfinal;
8) the pressure curve p (t) obtained according to baroceptor measurement obtains total gas pressure increment Delta pfinal;
9) pass through the total mass loss Δ m of samplefinalWith total gas pressure increment Delta pfinal, obtain ratio η=Δ of air pressure and quality
mfinal/Δpfinal, mass loss curve Δ m (t)=η p (t) of sample is obtained by The Ideal-Gas Equation;
10) voltage curve measured according to photodetector obtains the Laser output moment, and using this moment as mass loss song
Line, temperature curve zero when, both make to have strong association in time;
11) temperature of the mass loss curve, step 4) acquisition that are obtained according to Arrhenius pyrolytic reaction equation, step 9) is believed
Breath and identification method are fitted to obtain the pyrolysis Kinetics Parameter of sample to be tested;
The pyrolysis Kinetics Parameter includes pre-exponential factor A, activation energy, order of reaction n;
The Arrhenius pyrolytic reaction equation is specifically:
Wherein, R is mol gas constant.
7. the measurement method of polymer matrix composites pyrolysis Kinetics Parameter according to claim 6, it is characterised in that: step
It is rapid 6) before measuring sample to be tested final mass, cleaning treatment should be carried out to sample to be tested, be adhered to after removal reaction to be measured
The product of sample surfaces.
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