CN102445419A - Grating monitoring method for glass transition temperature of polymer-based composite material - Google Patents

Grating monitoring method for glass transition temperature of polymer-based composite material Download PDF

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Publication number
CN102445419A
CN102445419A CN2011102846887A CN201110284688A CN102445419A CN 102445419 A CN102445419 A CN 102445419A CN 2011102846887 A CN2011102846887 A CN 2011102846887A CN 201110284688 A CN201110284688 A CN 201110284688A CN 102445419 A CN102445419 A CN 102445419A
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grating
temperature
polymer matrix
matrix composite
sensor
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CN2011102846887A
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卢少微
高禹
王柏臣
王继杰
王赫男
张海军
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Shenyang Aerospace University
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Shenyang Aerospace University
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Abstract

The invention discloses a grating monitoring method for the glass transition temperature of a polymer-based composite material. The method comprises the following steps of: 1, manufacturing a dual-grating sensor; 2, calibrating the temperature transduction factor KT of a grating temperature sensor with a mercury thermometer by adopting a bath oiling method; 3, burying an optical fiber provided with the dual-grating sensor into the space between reinforced materials of the polymer-based composite material in the layering process of the reinforced materials of the polymer-based composite material; 4, preparing the polymer-based composite material with a wet/dry molding process; 5, in the molding process of curing engineering, monitoring the central wavelength change of the grating temperature sensor, computing the temperature change according to the temperature transduction factor KT, and monitoring the peak light intensity change value of a reflection spectrum peak light intensity sensor; and 6, drawing a relation curve between the reflection spectrum peak light intensity and the temperature in the curing process of the polymer-based composite material, wherein the turning point of the slope of a fitting straight line occurs, and a temperature value which corresponds to the intersection point between two fitting straight lines is the glass transition temperature Tg of the polymer-based composite material.

Description

The grating monitoring method of polymer matrix composite glass transition temperature
Technical field: the present invention relates to a kind of monitoring method, relate in particular to a kind of grating monitoring method of polymer matrix composite glass transition temperature, belong to polymer matrix composite and make the field.
Background technology: glass transition temperature (Tg) is the key character parameter of polymer matrix composite, and rapid variation has taken place near glass transition temperature the numerous characteristics of material.Polymkeric substance when Tg, except mechanical properties such as deformation and modulus change, many physical propertys, all great changes will take place like volume, thermal expansivity, optical refractive index, specific heat, coefficient of heat conductivity.So just can understand the state variation and the serviceability temperature of polymer matrix composite through measuring glass transition temperature; The physically aged of research polymer matrix composite; Confirm to solidify the processing and forming technology parameter; Carry out the polymer cure repercussion study, measure glass transition temperature and select for prepreg, technology is confirmed with quality control significant.
The conventional method of measuring Tg has a lot; As measure the thermal expansivity and the refraction coefficient of volume change; Measure the thermomechanometry and the stress relaxation method of change in mechanics, measure the differential thermal analysis (DTA) of thermal property and the dynamic mechanical analysis method (DMA) of differential scanning calorimetry (DSC) and measurement modulus or in-fighting etc.These methods only are applicable to carries out offline inspection or product is carried out " afterwards " monitoring subsized specimen.Still can't obtain the Tg information of material internal diverse location at present in real time to the polymer matrix composite manufacture process.Utilizing fiber grating that the polymer matrix composite glass transition temperature is carried out real-time online detects very necessary.
Summary of the invention: for realizing real time on-line monitoring to the polymer matrix composite glass transition temperature; The double grating sensor is imbedded in utilization of the present invention; Optical grating reflection spectrum peak intensity variations rule before and after the monitoring composite material solidification process Tg realizes the real-time monitoring to glass transition temperature.
For realizing above-mentioned purpose, the technical scheme that the present invention adopts is: the grating monitoring method of polymer matrix composite glass transition temperature, and its step is following:
1, make the double grating sensor: naked grating is positioned at optical fiber (6) end, is enclosed within the end of optical fiber (6) with stainless steel capillary (3), and the marginal portion of stainless steel capillary (3) encapsulates with silicon rubber (4), processes grating temperature sensor (1); Another naked grating is positioned at the middle part of optical fiber (6), as reflectance spectrum peak value light intensity sensor (2).Optical fiber (6) at first connects coupling mechanism (8), and coupling mechanism (8) connects grating demodulation appearance (9), and grating demodulation appearance (9) connects computing machine (10).
2, adopt bath oiling to utilize the TEMP COEFFICIENT K of mercury thermometer to grating temperature sensor (1) TDemarcate.
3, in the reinforcing material of polymer matrix composite (5) the shop layer process; The optical fiber (6) that has the double grating sensor is imbedded between the reinforcing material of polymer matrix composite (5), position, the preparation mould gateway reserved part quartz sheath (7) of optical fiber (6) and polymer matrix composite (5).
4, the preparation technology of polymer matrix composite (5) is suitable for wet method, dry-press process technology.
5, solidify in the engineering forming process, the center wavelength variation of monitoring grating temperature sensor (1) is according to the TEMP COEFFICIENT K TAccounting temperature changes, the reflectance spectrum peak value light intensity changing value of monitoring reflectance spectrum peak value light intensity sensor (2).
6, make the reflectance spectrum peak value light intensity (monitoring of reflectance spectrum peak value light intensity sensor) and temperature (grating temperature sensor monitoring) relation curve of polymer matrix composite solidification process; Turning point appears in the slope of its fitting a straight line; Article two, the corresponding temperature value of fitting a straight line intersection point is the glass transition temperature Tg of polymer matrix composite.
The double grating sensor is imbedded in utilization of the present invention, and optical grating reflection spectrum peak intensity variations rule before and after the monitoring composite material solidification process Tg realizes the real-time monitoring to glass transition temperature.
Description of drawings
Fig. 1 is a principle of work sketch of the present invention.
Embodiment
In Fig. 1, symbol 1 is represented fiber-optical grating temperature sensor; Symbol 2 is represented reflectance spectrum peak value light intensity sensor; Symbol 3 is represented stainless steel capillary; Symbol 4 is represented the silicon rubber encapsulation; Symbol 5 representation polymer based composites; Meet 6 and represent optical fiber; Symbol 7 is represented quartz sheath; Symbol 8 is represented coupling mechanism; Symbol 9 is represented the grating demodulation appearance; Symbol 10 is represented computing machine.
As shown in Figure 1: the grating monitoring method of polymer matrix composite glass transition temperature, its step is following:
(1) optical fiber 6 can be selected internal diameter 125 μ m for use; The standard fiber of outer polypropylene coating diameter 250 μ m; Inscribe grating temperature sensor 1 and reflectance spectrum peak value light intensity sensor 2 above that, process after grating temperature sensor 1 usefulness the stainless steel capillary 3 that wherein is positioned at optical fiber 6 ends encapsulates naked grating with silicon rubber 4.The centre wavelength of grating temperature sensor 1 and reflectance spectrum peak value light intensity sensor 2 is controlled between 1510-1590mm.
(2) have grating temperature sensor 1 be positioned at the direction parallel as far as possible with fortifying fibre with the optical fiber 6 of reflectance spectrum peak value light intensity sensor 2.
(3) stainless steel capillary 3 diameters that use of grating temperature sensor 1 encapsulation are 0.6-1.0mm.
(4) the optical fiber (FBG) demodulator of grating signal demodulation use is selected the static optical fiber (FBG) demodulator of sm125-500 of MOI company for use, can monitor the full spectral information of grating centre wavelength and optical grating reflection (can obtain reflectance spectrum peak value light intensity).
(5) preparation technology of polymer matrix composite 5 can be autoclave moulding, compression molding and resin transfer molding technology.
(6) optical fiber 6 is protected with quartz sheath 7 through the position, gateway of polymer matrix composite 5 moulds, and optical fiber 6 at first connects coupling mechanism 8, and coupling mechanism 8 connects grating demodulation appearance 9, and grating demodulation appearance 9 connects computing machine 10.
When (7) grating is monitored; Optical fiber (FBG) demodulator 9 inner wideband light sources are through coupling mechanism 8 emission laser; Import grating temperature sensor 1 and reflectance spectrum peak value light intensity sensor 2 then into; The reflected light of grating temperature sensor 1 and reflectance spectrum peak value light intensity sensor 2 is importing grating demodulation appearance 9 into through coupling mechanism 8, through importing computing machine 10 into after the signal demodulation, the center wavelength variation of monitoring grating temperature sensor 1 and the reflectance spectrum peak value intensity variations of reflectance spectrum peak value light intensity sensor 2.
(8) make the reflectance spectrum peak value light intensity (reflectance spectrum peak value light intensity sensor 2 monitoring) and temperature (1 monitoring of grid temperature sensor) relation curve of polymer matrix composite solidification process; Turning point appears in the slope of its fitting a straight line; Article two, the corresponding temperature value of fitting a straight line intersection point is the glass transition temperature Tg of polymer matrix composite.
Principle of work
The present invention adopts the double grating monitoring technology; Wherein stainless steel capillary encapsulation grating is used for monitor temperature; Reflectance spectrum peak value light intensity sensor directly contacts with polymer matrix composite, changes the glass transition temperature of reflection compound substance through optical grating reflection spectrum peak light intensity.
The grating centre wavelength of grating temperature sensor and the relation equation of temperature are:
Δ λ B λ B = k T ΔT
TEMP COEFFICIENT K wherein TCan utilize bath oiling to demarcate, be used for temperature computation with mercury thermometer.
In the polymer matrix composite solidification process, the chemical reaction of a series of complicacies takes place in resin, sees it all is that micromolecule aggregates into the macromolecular process of bodily form reticulate texture through cross-linking reaction from microcosmic.Before and after compound substance is accomplished glass transition, material physical property such as viscosity, thermal expansivity, particularly variation in refractive is obvious.According to before and after the compound substance glass transition temperature, the optical grating reflection spectrum peak light intensity of imbedding and the relation equation of resin refraction coefficient can know that optical grating reflection spectrum peak light intensity is influenced obviously by glass transition temperature thus.
The relation equation of optical grating reflection spectrum peak light intensity and resin refraction coefficient is:
R = | n f - n m n f + n m | 2
n f, n mBe respectively the specific refractivity of fiber and resin, R is an optical grating reflection spectrum peak light intensity.
So pass through the temperature of the catastrophe point correspondence position of optical grating reflection light intensity and temperature relation fitting a straight line slope variation, can confirm glass transition temperature.

Claims (4)

1. the grating monitoring method of polymer matrix composite glass transition temperature, its step is following:
(1) make the double grating sensor: naked grating is positioned at optical fiber end, is enclosed within the end of optical fiber with stainless steel capillary, and the marginal portion of stainless steel capillary encapsulates with silicon rubber; Process grating temperature sensor; Another naked grating is positioned at the middle part of optical fiber, and as reflectance spectrum peak value light intensity sensor, optical fiber at first connects coupling mechanism; Coupling mechanism connects the grating demodulation appearance, and the grating demodulation appearance connects computing machine;
(2) adopt bath oiling to utilize the TEMP COEFFICIENT K of mercury thermometer to grating temperature sensor TDemarcate;
(3) in the reinforcing material of the polymer matrix composite shop layer process, the optical fiber that has the double grating sensor is imbedded between the reinforcing material of polymer matrix composite, position, the preparation mould gateway reserved part quartz sheath of optical fiber and polymer matrix composite;
(4) preparation technology of polymer matrix composite is suitable for wet method, dry-press process technology;
(5) solidify in the engineering forming process, the center wavelength variation of monitoring grating temperature sensor is according to the TEMP COEFFICIENT K TAccounting temperature changes, the reflectance spectrum peak value light intensity changing value of monitoring reflectance spectrum peak value light intensity sensor;
(6) make the reflectance spectrum peak value light intensity and the temperature relation curve of polymer matrix composite solidification process, turning point appears in the slope of its fitting a straight line, and two temperature values that the fitting a straight line intersection point is corresponding are the glass transition temperature Tg of polymer matrix composite.
2. the grating monitoring method of polymer matrix composite glass transition temperature as claimed in claim 1 is characterized in that: have grating temperature sensor and be positioned at the direction parallel with fortifying fibre with the optical fiber of reflectance spectrum peak value light intensity sensor as far as possible.
3. the grating monitoring method of polymer matrix composite glass transition temperature as claimed in claim 1 is characterized in that: the stainless steel capillary diameter that the grating temperature sensor encapsulation is used is 0.6-1.0mm.
4. the grating monitoring method of polymer matrix composite glass transition temperature as claimed in claim 1 is characterized in that: the preparation technology of polymer matrix composite is autoclave moulding, compression molding and resin transfer molding technology.
CN2011102846887A 2011-09-22 2011-09-22 Grating monitoring method for glass transition temperature of polymer-based composite material Pending CN102445419A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107941283A (en) * 2017-12-22 2018-04-20 中南大学 The multi-parameter on-line monitoring system and method for composite material hot-press solidifying process
CN108467550A (en) * 2018-04-16 2018-08-31 山东大学 A kind of butyl rubber nanocomposites and its dynamic heat build up detection method of graphene-containing
CN113670471A (en) * 2021-08-30 2021-11-19 武汉理工大学 Glass transition temperature detection method based on fiber drawing tower grating coating

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CN101883978A (en) * 2007-12-06 2010-11-10 三菱电机株式会社 Optical fiber sensor
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107941283A (en) * 2017-12-22 2018-04-20 中南大学 The multi-parameter on-line monitoring system and method for composite material hot-press solidifying process
CN107941283B (en) * 2017-12-22 2024-03-12 中南大学 Multi-parameter on-line monitoring system and method for hot-press curing process of composite material
CN108467550A (en) * 2018-04-16 2018-08-31 山东大学 A kind of butyl rubber nanocomposites and its dynamic heat build up detection method of graphene-containing
CN113670471A (en) * 2021-08-30 2021-11-19 武汉理工大学 Glass transition temperature detection method based on fiber drawing tower grating coating

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Application publication date: 20120509