CN117030775A - Broadband dual-laser excitation-based solid engine spray pipe adhesive curing viscosity photo-thermal characterization device and characterization method thereof - Google Patents
Broadband dual-laser excitation-based solid engine spray pipe adhesive curing viscosity photo-thermal characterization device and characterization method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 description 6
- 239000003822 epoxy resin Substances 0.000 description 5
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- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 3
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- 229920005989 resin Polymers 0.000 description 2
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- 238000001328 terahertz time-domain spectroscopy Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
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- 101100163901 Rattus norvegicus Asic2 gene Proteins 0.000 description 1
- -1 alloy/modified acrylic ester Chemical class 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
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- 239000003795 chemical substances by application Substances 0.000 description 1
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- 239000011152 fibreglass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
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Abstract
A broadband dual-laser excitation-based solid engine spray pipe adhesive curing viscosity photo-thermal characterization device and a characterization method thereof. The computer (1) is sequentially connected with the first function generator (4) and the high-power semiconductor laser power supply (6), the high-power semiconductor laser power supply (6) is respectively connected with the high-power semiconductor laser (9) and the TEC refrigerator power supply (11), the TEC refrigerator power supply (11) is provided with the TEC semiconductor refrigerator (10), and the high-power semiconductor laser (9) is sequentially connected with the first collimating mirror (20), the first engineering diffuser (21) and the second polaroid (22); the computer (1) is also connected with a phase-locked detection amplifier (39), and the phase-locked detection amplifier (39) is sequentially connected with a preamplifier (15), an HCT heat detector (17), a first polaroid (18) and a band-pass filter (19). The invention solves the problem that the curing time of the solid engine spray pipe adhesive can not be quantified in the practical application process.
Description
Technical Field
The invention belongs to the technical fields of photothermal science, detection and signal processing, and particularly relates to a solid engine spray pipe adhesive curing viscosity photothermal characterization device based on broadband dual-laser excitation and a characterization method thereof.
Background
The bonding of the solid engine spray pipe comprises the bonding of the resin-based carbon fiber composite material lining and the metal shell, and the bonding effect is mainly determined by the surface state of an adherend, the adhesive property and the interface layer property. As the epoxy resin has activity on a plurality of materials, the curing reaction belongs to nucleophilic addition reaction, high pressure is not needed during curing, and the bonding molding process is simple. The formula on the basis is easy to select, and the corresponding curing agent is selected according to the curing temperature used, and meanwhile, the pot life and the performance of the adhesive after curing are both considered. In the practical application process, the adhesive of the E-51 epoxy resin and the 2-ethyl-4-methylimidazole formula system belongs to a medium-temperature cured epoxy resin structural adhesive, and long-term batch production type use shows that the adhesive can meet the adhesion between a long tail nozzle metal shell and a glass fiber reinforced plastic lining in a tactical missile solid rocket engine. The performance index, the molding process, the quality stability, the reliability and the like of the adhesive completely meet the use requirements of products. The complete curing time of the E-51 epoxy resin and the adhesive of the 2-ethyl-4-methylimidazole formula system at the specified temperature can be roughly calculated based on an apparent kinetic equation. Setting the ambient temperature at 80 c, a complete cure time of 4.44 hours was obtained. Considering the influence of heat conduction and radiation between the material and the environment, the total curing time is generally 6-8 hours under the environment of 80 ℃. In order to ensure effective bonding of the solid engine composite liner to the metal shell, bonding is generally required at a point in time prior to complete curing of the material, at which time no empirical or theoretical formula is currently available for calculation reference. After full investigation, the actual engineering experience of bonding workers is mainly relied on to judge the moment at the production workshop, fingers are adopted to touch the adhesive in the curing process, and the optimal bonding time is obtained when the adhesive has the effect of wire drawing and non-adhesion.
In the prior art, a terahertz time-domain spectrometer is used for collecting terahertz time-domain signals of an organic adhesive sample piece after curing for T1 time at normal temperature, so as to obtain a terahertz data set. Carrying out mathematical statistics on variance values and flight time of each point in the variance imaging diagram and the flight time imaging diagram to form a histogram; carrying out Gaussian curve fitting on the histogram, and carrying out statistics on the characteristic value mu of the Gaussian curve after fitting; repeating the steps until the characteristic value of the Gaussian curve is obtained after normal-temperature curing is completed; and carrying out statistical analysis on the characteristic values of the normal-temperature cured Gaussian curve of each period of the organic adhesive sample piece to obtain a graph. According to the invention, the characteristic change in the curing process is obtained by adopting a terahertz time-domain spectroscopy, so that the curing of the adhesive can be evaluated to a certain extent, but quantitative indexes are lacking, and therefore, the quantitative judgment cannot be carried out. Another prior art does not mention a method of detecting or quantifying the extent of cure. The prior art also discloses that magnesium aluminum alloy is used as a bonded material, a nonlinear ultrasonic testing system is utilized to excite and receive longitudinal wave ultrasonic signals, fourier transformation is carried out on the received ultrasonic signals, fundamental frequency amplitude and frequency multiplication amplitude of ultrasonic signals passing through a bonding structure are obtained, corresponding nonlinear coefficients are obtained, and finally, the relationship between the nonlinear coefficients and the curing time of the adhesive is established. In the paper, the curing degree of the material is evaluated by using a self-defined nonlinear coefficient, so that the method has no interpretability, is used for contact measurement, and is not suitable for a non-contact detection scene. When the prior art takes 6061 aluminum alloy/modified acrylic ester glue/6061 aluminum alloy bonding test piece as a research object, the collinear transverse wave and longitudinal wave mixing detection technology is adopted, and the change condition of the resonance wave amplitude along with the curing time of the bonding interface is experimentally researched. The results show that: there is an inherent relationship between the amplitude of the resonant wave and the number of randomly distributed cracks in the bond line, and the curing time of the bond test piece. However, the method is still a real-time monitoring method, and lacks an effective measurement quantification index for the curing degree of the material.
Disclosure of Invention
The invention provides a broadband dual-laser excitation-based solid engine spray pipe adhesive curing viscosity photo-thermal characterization device and a characterization method thereof, which are used for solving the problem that the curing time of the solid engine spray pipe adhesive cannot be quantified in the practical application process. The detection method and the detection system are suitable for the field of accurate quantitative evaluation of the curing viscosity and the optimal curing time of the solid engine spray pipe adhesive.
The invention is realized by the following technical scheme:
the solid engine spray pipe adhesive curing viscosity photo-thermal characterization device based on broadband dual laser excitation comprises a computer 1, a first function generator 4, a high-power semiconductor laser power supply 6, a high-power semiconductor laser 9, a TEC semiconductor refrigerator 10, a TEC refrigerator power supply 11, a first mounting support 13, a large off-axis parabolic mirror 14, a preamplifier 15, an HCT heat detector 17, a first polaroid 18, a band-pass filter 19, a first collimating mirror 20, a first engineering diffuser 21, a second polaroid 22, a second collimating mirror 23, a second engineering diffuser 24, a third polaroid 25, a focusing plate 26, a small off-axis parabolic mirror 27, a test piece 28 to be tested, an incubator 29, a two-dimensional micro-displacement moving table 30, a second mounting support 32, a two-axis driver 33, a low-power semiconductor laser 35, a second function generator 37, a phase-locking amplifier 39 and a driving control line 41;
the computer 1 is sequentially connected with a first function generator 4 and a high-power semiconductor laser power supply 6, the high-power semiconductor laser power supply 6 is respectively connected with a high-power semiconductor laser 9 and a TEC refrigerator power supply 11, a TEC semiconductor refrigerator 10 is arranged on the TEC refrigerator power supply 11, and the high-power semiconductor laser 9 is sequentially connected with a first collimating mirror 20, a first engineering diffuser 21 and a second polaroid 22;
the computer 1 is also connected with a phase-locked detection amplifier 39, and the phase-locked detection amplifier 39 is sequentially connected with a preamplifier 15, an HCT heat detector 17, a first polaroid 18 and a band-pass filter 19; the band-pass filter 19 is matched with the large off-axis parabolic mirror 14 for use, and the large off-axis parabolic mirror 14 is arranged on the first mounting support 13;
the phase-locked detection amplifier 39 is further connected to a second function generator 37, the second function generator 37 is sequentially connected to the low-power semiconductor laser 35, the second collimating mirror 23, the second engineering diffuser 24, the third polarizing plate 25 and the focusing plate 26 are embedded in a designated installation position of the small off-axis parabolic mirror 27, and the small off-axis parabolic mirror 27 is arranged on the second installation support 32;
the computer 1 is also connected with a two-axis driver 33, the two-axis driver 33 is connected with a two-dimensional micro-displacement moving table 30, an incubator 29 is arranged on the two-dimensional micro-displacement moving table 30, and a test piece 28 to be tested is placed in the incubator 29.
Further, the computer 1 is provided with 2 output signal ends and 1 input/output signal end, the computer 1 is connected with the phase-locked detection amplifier 39 through the input/output signal end Ethernet line 40, and the computer 1 is connected with the input signal end of the first function generator 4 through the first output signal end first B-type USB data line 3; the computer 1 is connected with the two-axis driver 33 through a second output signal end driving control line 41; the output signal end of the phase-locked detection amplifier 39 is connected with the second function generator 37 through a second BNC data line 38; the input signal end of the phase-locked detection amplifier 39 is connected with the preamplifier 15 through the high-performance radio-frequency coaxial cable 2; the second function generator 37 is connected with the low-power semiconductor laser 35 through a second B-type USB data line 36, and the laser emitted by the low-power semiconductor laser 35 is transmitted to the second collimating mirror 23 through a second laser fiber 34;
the second engineered diffuser 24, the third polarizer 25, and the focusing plate 26 are embedded in the small off-axis parabolic mirror 27 at designated mounting locations; the test piece 28 to be tested is placed in the incubator 29, the incubator 29 is placed on the two-dimensional micro-displacement moving table 30, and the position scanning detection of the test piece 28 to be tested is realized; the small off-axis parabolic mirror 27 is arranged on the second mounting support 32, and the large off-axis parabolic mirror 14 is arranged on the first mounting support 13; the HCT heat detector 17 is connected with an input signal end of the preamplifier 15 through a coaxial cable 16, so that amplification of the obtained photo-thermal signal is realized; the band-pass filter 19 and the first polaroid 18 are fixed in front of the HCT heat detector 17 through threaded connection, and the band-pass filter 19 is used for effectively filtering near infrared excitation light; the output signal end of the first function generator 4 is connected with a high-power semiconductor laser power supply 6 through a first BNC data line 5; the high-power semiconductor laser power supply 6 is connected with the high-power semiconductor laser 9 and the TEC refrigerator power supply 11 through the semiconductor laser power supply line 7 and the TEC refrigerator power supply line 8 respectively, and the TEC semiconductor refrigerator 10 is positioned between the high-power semiconductor laser 9 and the TEC refrigerator power supply 11; the high power semiconductor laser 9 transmits laser light to the first collimating mirror 20 through the first laser fiber 12, and a first engineering diffuser 21 and a second polarizer 22 are respectively installed in front of the first collimating mirror 20.
A broadband dual-laser excitation-based photo-thermal characterization method for curing viscosity of a solid engine spray pipe adhesive comprises the following steps of,
step one: defining a test piece 28 to be tested, placing the test piece to be tested in an incubator 29, opening the incubator 29, and setting the temperature to 80 ℃;
step two: starting a solid engine spray pipe adhesive curing viscosity photo-thermal characterization device based on broadband double-laser excitation;
step three: adjusting the position of the two-dimensional micro-displacement moving table 30 to enable the test piece 28 to be tested to be positioned at the focal position of the small off-axis parabolic mirror 27, and simultaneously adjusting the first mounting support 13 to enable the element detected by the HCT heat detector 17 to be positioned at the focal position of the large off-axis parabolic mirror 14;
step four: the computer 1 sends out instructions to enable the low-power semiconductor laser 35 to generate laser with the modulation frequency of 0Hz through the phase-locked detection amplifier 39 and the second function generator 37, and at the moment, whether the laser spot size is normal or not is checked;
meanwhile, the computer 1 sends out an instruction, the high-power semiconductor laser power supply 6 generates laser with the modulation frequency of 0Hz through the first function generator 4, and at the moment, whether the laser emitted by the first collimating mirror 20 completely covers the test piece 28 to be tested is checked;
step five: observing whether the lock-in detector amplifier 39 acquires the signal from the HCT heat detector 17 in the range, if not, adjusting the preamplifier 15, amplifying or reducing the gain;
step six: when the temperature of the test piece 28 to be tested reaches the set temperature, starting timing, and carrying out a broadband dual-laser excited adhesive curing viscosity photo-thermal characterization test in 0 hours and 0 hours, wherein the modulation frequency band range of the low-power semiconductor laser 35 is set as the range, the frequency of the high-power semiconductor laser power supply 6 is 0Hz, and the power is 45W;
step seven: then, carrying out broadband dual-laser excited adhesive curing viscosity photo-thermal characterization test after every 1h, then judging whether the adhesive is the optimal bonding time by combining a worker master hand touch mode, recording photo-thermal response characteristic data, and recording for 0-5 hours;
step eight: after 5 hours of test data are completed, a dual-laser excitation induction heat radiation signal response model is required to be established according to the characteristics of the test piece to be tested so as to realize quantitative evaluation of the curing degree;
step nine: after the test is finished, the broadband scanning result and the fitting result obtained by the test are saved, meanwhile, the computer 1 controls the high-power semiconductor laser power supply 6 and the low-power semiconductor laser 35 to enable the light intensity to be 0, and simultaneously controls the two-axis driver 33 to enable the two-dimensional micro-displacement mobile station 30 to be zeroed, and the heating function of the incubator 29 is closed;
step ten: after the test was completed, the first function generator 4, the high power semiconductor laser power supply 6, the two-axis driver 33, the preamplifier 15, the hct heat detector 17, the second function generator 37, and the lock-in detector amplifier 39 were turned off in this order at intervals of 5 minutes. After the incubator 29 is returned to room temperature, the test piece 28 to be tested is placed in a designated storage container.
Furthermore, the characteristic of the test piece to be tested in the step eight is established into a dual-laser excitation induction heat radiation signal response model which is specifically,
k in the formula 1 The response gain of the HCT heat detector is k, the thermal conductivity of the test piece to be tested is k, h is the convective heat transfer coefficient existing on the surface of the test piece to be tested, and alpha IR (lambda) is the infrared absorption coefficient of the test piece to be tested; l (L) 1 The thickness of the test piece to be tested; sigma is Stefan-Boltzmann constant; beta is the light absorption attenuation coefficient of the test piece to be tested.
Further, the relation between the heat radiation signal and the surface temperature signal of the test piece to be tested is as follows,
wherein K is a system scale factor; p (λ) is the HCT heat detector spectral response band; epsilon is the emissivity of the test piece to be tested; t (T) 0 Is at room temperature; lambda (lambda) 1 ,λ 2 The spectral response ranges of HCT heat detectors, respectively.
Further, since the signal S (ω) is a complex number, the amplitude-frequency and phase-frequency dynamic response of the photothermal radiation of the test piece to be tested by the modulated laser can be directly obtained, that is:
the multi-parameter fitting is to find the optimal parameters, so that the amplitude and phase information calculated by the mathematical model in the optimal parameters and the amplitude and phase information obtained by the test are brought into the objective function G, and the G reaches the minimum value.
Further, the objective function of the multi-parameter fitting is that,
z in 1 ,Z 2 Is a scale factor; g is a coefficient to be fitted; n is the number of acquisition points; f (f) i Is the modulation frequency; ampl T ，Phase T To calculate amplitude and phase; ampl E ，Phase E Amplitude and phase characteristic data obtained for the trial.
The beneficial effects of the invention are as follows:
the invention can effectively identify the optimal curing time of the solid engine spray pipe adhesive, the thickness of the adhesive is covered with 20-200 mu m, the characteristic phase difference between the optimal curing adhesive and the uncured adhesive is more than 30 degrees, and the frequency of the dual-laser excitation luminous heat radiation response signal is covered with 0.01-102 KHz. Meanwhile, the curing time of the adhesive can be quantitatively evaluated according to inversion resin of the thermal conductivity and the thermal diffusion coefficient, and the inversion accuracy of the thermal conductivity and the thermal diffusion coefficient is respectively better than 10 -4 W/mdeg.C and 10 -3 m 2 /s。
The invention can also be applied to the fields of multi-aspect technology such as the fields of high polymer photo-thermal performance evaluation and the real-time monitoring and quantitative evaluation of the curing degree of the aerospace adhesive.
Compared with detection methods such as ultrasonic and terahertz time-domain spectroscopy, the invention can fully utilize the advantages of non-contact photo-thermal radiation, tunable laser, high heat injection efficiency and the like, and simultaneously effectively extract the characteristic information containing the curing degree of the adhesive by utilizing the advantages of double-path detection operation on high-frequency harmonic signals such as noise filtering and the like, can effectively identify the optimal curing time of the adhesive of the solid engine spray pipe, and detects the thickness coverage of the adhesive to be 20-200 mu m, wherein the characteristic phase difference between the optimal curing and uncured adhesive is more than 30 degrees.
Drawings
Fig. 1 is a schematic structural view of the present invention.
FIG. 2 is a schematic diagram of a test piece to be tested according to the present invention.
FIG. 3 shows the results of broadband thermal radiation response for different cure times for solid engine nozzle adhesive samples of the present invention, wherein (a) the results of the amplitude-frequency response and (b) the results of the phase-frequency response.
FIG. 4 is a graph of the characteristic results of the solid engine nozzle adhesive samples of the present invention at specific frequencies for different cure times, where (a) amplitude and (b) phase.
Fig. 5 is a fitting result of the present invention.
FIG. 6 is an inversion of thermal conductivity and thermal diffusivity of a solid engine nozzle adhesive of the present invention, wherein (a) the thermal conductivity is fit and (b) the thermal diffusivity is fit.
1-computer, 2-high performance RF coaxial cable, 3-first B-type USB data line, 4-first function generator, 5-first BNC data line, 6-high power semiconductor laser power supply, 7-semiconductor laser power supply line, 8-TEC refrigerator power supply line, 9-high power semiconductor laser, 10-TEC semiconductor refrigerator, 11-TEC refrigerator power supply, 12-first laser fiber, 13-first mounting support, 14-large off-axis parabolic mirror, 15-preamplifier, 16-coaxial cable, 17-HCT heat detector, 18-first polarizer, 19-band pass filter, 20-first collimating mirror 21-first engineering diffuser, 22-second polarizer, 23-second collimating mirror, 24-second engineering diffuser, 25-third polarizer, 26-focusing plate, 27-small off-axis parabolic mirror, 28-test piece, 29-incubator, 30-two-dimensional micro-displacement mobile station, 31-motion control line, 32-second mounting support, 33-two-axis driver, 34-second laser fiber, 35-low power semiconductor laser, 36-second USB data line, 37-second function generator, 38-second BNC data line, 39-phase lock detection amplifier, 40-Ethernet line, 41-drive control line
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The solid engine spray pipe adhesive curing viscosity photo-thermal characterization device based on broadband dual laser excitation comprises a computer 1, a first function generator 4, a high-power semiconductor laser power supply 6, a high-power semiconductor laser 9, a TEC semiconductor refrigerator 10, a TEC refrigerator power supply 11, a first mounting support 13, a large off-axis parabolic mirror 14, a preamplifier 15, an HCT heat detector 17, a first polaroid 18, a band-pass filter 19, a first collimating mirror 20, a first engineering diffuser 21, a second polaroid 22, a second collimating mirror 23, a second engineering diffuser 24, a third polaroid 25, a focusing plate 26, a small off-axis parabolic mirror 27, a test piece 28 to be tested, an incubator 29, a two-dimensional micro-displacement moving table 30, a second mounting support 32, a two-axis driver 33, a low-power semiconductor laser 35, a second function generator 37, a phase-locking amplifier 39 and a driving control line 41;
the computer 1 is sequentially connected with a first function generator 4 and a high-power semiconductor laser power supply 6, the high-power semiconductor laser power supply 6 is respectively connected with a high-power semiconductor laser 9 and a TEC refrigerator power supply 11, a TEC semiconductor refrigerator 10 is arranged on the TEC refrigerator power supply 11, and the high-power semiconductor laser 9 is sequentially connected with a first collimating mirror 20, a first engineering diffuser 21 and a second polaroid 22;
the computer 1 is also connected with a phase-locked detection amplifier 39, and the phase-locked detection amplifier 39 is sequentially connected with a preamplifier 15, an HCT heat detector 17, a first polaroid 18 and a band-pass filter 19; the band-pass filter 19 is matched with the large off-axis parabolic mirror 14 for use, and the large off-axis parabolic mirror 14 is arranged on the first mounting support 13;
the phase-locked detection amplifier 39 is further connected to a second function generator 37, the second function generator 37 is sequentially connected to the low-power semiconductor laser 35, the second collimating mirror 23, the second engineering diffuser 24, the third polarizing plate 25 and the focusing plate 26 are embedded in a designated installation position of the small off-axis parabolic mirror 27, and the small off-axis parabolic mirror 27 is arranged on the second installation support 32;
the computer 1 is also connected with a two-axis driver 33, the two-axis driver 33 is connected with a two-dimensional micro-displacement moving table 30, an incubator 29 is arranged on the two-dimensional micro-displacement moving table 30, and a test piece 28 to be tested is placed in the incubator 29.
Further, the computer 1 is provided with 2 output signal ends and 1 input/output signal end, the computer 1 is connected with the phase-locked detection amplifier 39 through the input/output signal end Ethernet line 40, and the computer 1 is connected with the input signal end of the first function generator 4 through the first output signal end first B-type USB data line 3; the computer 1 is connected with the two-axis driver 33 through a second output signal end driving control line 41; the output signal end of the phase-locked detection amplifier 39 is connected with the second function generator 37 through a second BNC data line 38; the input signal end of the phase-locked detection amplifier 39 is connected with the preamplifier 15 through the high-performance radio-frequency coaxial cable 2; the second function generator 37 is connected with the low-power semiconductor laser 35 through a second B-type USB data line 36, and the laser emitted by the low-power semiconductor laser 35 is transmitted to the second collimating mirror 23 through a second laser fiber 34;
the second engineered diffuser 24, the third polarizer 25, and the focusing plate 26 are embedded in the small off-axis parabolic mirror 27 at designated mounting locations; the test piece 28 to be tested is placed in the incubator 29, the incubator 29 is placed on the two-dimensional micro-displacement moving table 30, and the position scanning detection of the test piece 28 to be tested is realized; the small off-axis parabolic mirror 27 is arranged on the second mounting support 32, and the large off-axis parabolic mirror 14 is arranged on the first mounting support 13; the HCT heat detector 17 is connected with an input signal end of the preamplifier 15 through a coaxial cable 16, so that amplification of the obtained photo-thermal signal is realized; the band-pass filter 19 and the first polaroid 18 are fixed in front of the HCT heat detector 17 through threaded connection, and the band-pass filter 19 is used for effectively filtering near infrared excitation light; the output signal end of the first function generator 4 is connected with a high-power semiconductor laser power supply 6 through a first BNC data line 5; the high-power semiconductor laser power supply 6 is connected with the high-power semiconductor laser 9 and the TEC refrigerator power supply 11 through the semiconductor laser power supply line 7 and the TEC refrigerator power supply line 8 respectively, and the TEC semiconductor refrigerator 10 is positioned between the high-power semiconductor laser 9 and the TEC refrigerator power supply 11; the high power semiconductor laser 9 transmits laser light to the first collimating mirror 20 through the first laser fiber 12, and a first engineering diffuser 21 and a second polarizer 22 are respectively installed in front of the first collimating mirror 20.
The solid engine nozzle adhesive curing viscosity photo-thermal characterization device based on broadband dual laser excitation as shown in fig. 1 is implemented, in this embodiment, the modulated light adopted in the test is a low-power semiconductor laser 35 (laser power 32mW, spot diameter 600 μm) with 808nm, and the direct-current light is a high-power semiconductor laser 9 (laser power 45W, coverage area 100mm×100 mm) with 808 nm; an HCT heat detector 17 (detection band 2 μm to 12 μm, detection area 100 μm. Times.100 μm); the applicable frequency band of the related detection is 0.01 Hz-102 KHz, and the test scanning frequency range is 100 Hz-100 KHz. The test piece 28 to be tested is an adhesive of a formula system of E-51 epoxy resin and 2-ethyl-4-methylimidazole, and the thickness is 150 mu m.
A broadband dual-laser excitation-based photo-thermal characterization method for curing viscosity of a solid engine spray pipe adhesive comprises the following steps of,
step one: defining a test piece 28 to be tested, placing the test piece to be tested in an incubator 29, opening the incubator 29, and setting the temperature to 80 ℃;
step two: starting a solid engine spray pipe adhesive curing viscosity photo-thermal characterization device based on broadband double-laser excitation; the process comprises the steps of starting the first function generator 4, the high-power semiconductor laser power supply 6, the preamplifier 15, the HCT heat detector 17, the phase-locked detection amplifier 39, the second function generator 37, the two-axis driver 33 and other devices;
step three: adjusting the position of the two-dimensional micro-displacement moving table 30 to enable the test piece 28 to be tested to be positioned at the focal position of the small off-axis parabolic mirror 27, and simultaneously adjusting the first mounting support 13 to enable the element detected by the HCT heat detector 17 to be positioned at the focal position of the large off-axis parabolic mirror 14;
step four: the computer 1 sends out instructions to enable the low-power semiconductor laser 35 to generate laser with the modulation frequency of 0Hz through the phase-locked detection amplifier 39 and the second function generator 37, and at the moment, whether the laser spot size is normal or not is checked;
meanwhile, the computer 1 sends out an instruction, the high-power semiconductor laser power supply 6 generates laser with the modulation frequency of 0Hz through the first function generator 4, and at the moment, whether the laser emitted by the first collimating mirror 20 completely covers the test piece 28 to be tested is checked;
step five: observing whether the lock-in detector amplifier 39 acquires the signal from the HCT heat detector 17 in the range, if not, adjusting the preamplifier 15, amplifying or reducing the gain;
step six: when the temperature of the test piece 28 to be tested reaches the set temperature, starting timing, and carrying out a broadband dual-laser excited adhesive curing viscosity photo-thermal characterization test in 0 hours and 0 hours, wherein the modulation frequency band range of the low-power semiconductor laser 35 is set as the range, the frequency of the high-power semiconductor laser power supply 6 is 0Hz, and the power is 45W;
step seven: then, carrying out broadband dual-laser excited adhesive curing viscosity photo-thermal characterization test after every 1h, then judging whether the adhesive is the optimal bonding time by combining a worker master hand touch mode, recording photo-thermal response characteristic data, and recording for 0-5 hours;
step eight: after 5 hours of test data are completed, a dual-laser excitation induction heat radiation signal response model is required to be established according to the characteristics of the test piece to be tested so as to realize quantitative evaluation of the curing degree;
step nine: after the test is finished, the broadband scanning result and the fitting result obtained by the test are saved, meanwhile, the computer 1 controls the high-power semiconductor laser power supply 6 and the low-power semiconductor laser 35 to enable the light intensity to be 0, and simultaneously controls the two-axis driver 33 to enable the two-dimensional micro-displacement mobile station 30 to be zeroed, and the heating function of the incubator 29 is closed;
step ten: after the test is finished, after 5 minutes, sequentially turning off the first function generator, the high-power semiconductor laser power supply, the two-axis driver, the preamplifier, the HCT heat detector, the second function generator and the phase-locked detection amplifier; and after the incubator returns to room temperature, placing the test piece to be tested into a specified storage container.
Furthermore, the characteristic of the test piece to be tested in the step eight is established into a dual-laser excitation induction heat radiation signal response model which is specifically,
k in the formula 1 The response gain of the HCT heat detector is k, the thermal conductivity of the test piece to be tested is k, h is the convective heat transfer coefficient existing on the surface of the test piece to be tested, and alpha IR (lambda) is the infrared absorption coefficient of the test piece to be tested; l (L) 1 The thickness of the test piece to be tested; sigma is Stefan-Boltzmann constant; beta is the light absorption attenuation coefficient of the test piece to be tested.
Further, the relation between the heat radiation signal and the surface temperature signal of the test piece to be tested is as follows,
wherein K is a system scale factor; p (λ) is the HCT heat detector spectral response band; epsilon is the emissivity of the test piece to be tested; t (T) 0 Is at room temperature; lambda (lambda) 1 ,λ 2 The spectral response ranges of HCT heat detectors, respectively.
Further, since the signal S (ω) is a complex number, the amplitude-frequency and phase-frequency dynamic response of the photothermal radiation of the test piece to be tested by the modulated laser can be directly obtained, that is:
the multi-parameter fitting is to find the optimal parameters, so that the amplitude and phase information calculated by the mathematical model in the optimal parameters and the amplitude and phase information obtained by the test are brought into the objective function G, and the G reaches the minimum value.
Further, the objective function of the multi-parameter fitting is that,
z in 1 ,Z 2 Is a scale factor; g is the coefficient to be fitted (including thermal conductivity and thermal diffusivity); n is the number of acquisition points; f (f) i Is the modulation frequency; ampl T ，Phase T To calculate amplitude and phase; ampl E ，Phase E Amplitude and phase characteristic data obtained for the trial. FIG. 3 shows the results of a broadband thermal radiation response test for different cure times for solid engine nozzle adhesive samples. FIG. 4 is a graphical representation of results from analysis of the characteristics of different cure times of solid engine nozzle adhesive samples at a particular frequency. It is clear from fig. 4 that the optimum curing time is around 3 hours. The mathematical model is used for solving the range problem of the acquired test data, and the fitting result of the test values is shown in fig. 5. From the fitting result, specific values of thermal conductivity and thermal diffusivity (as shown in fig. 6) can be obtained, which can be used as a standard for quantitatively evaluating the curing time.
Claims (7)
1. The solid engine spray pipe adhesive curing viscosity photo-thermal characterization device based on broadband dual laser excitation is characterized by comprising a computer (1), a first function generator (4), a high-power semiconductor laser power supply (6), a high-power semiconductor laser (9), a TEC semiconductor refrigerator (10), a TEC refrigerator power supply (11), a first mounting support (13), a large off-axis parabolic mirror (14), a preamplifier (15), an HCT heat detector (17), a first polaroid (18), a band-pass filter (19), a first collimating mirror (20), a first engineering diffuser (21), a second polaroid (22), a second collimating mirror (23), a second engineering diffuser (24), a third polaroid (25), a focusing sheet (26), a small off-axis parabolic mirror (27), a test piece (28) to be tested, a constant temperature box (29), a two-dimensional micro-displacement mobile station (30), a second mounting support (32), a two-axis driver (33), a low-power semiconductor laser (35), a second function generator (37), a detector amplifier (39) and a phase-locked control line (41);
the computer (1) is sequentially connected with a first function generator (4) and a high-power semiconductor laser power supply (6), the high-power semiconductor laser power supply (6) is respectively connected with a high-power semiconductor laser (9) and a TEC refrigerator power supply (11), a TEC semiconductor refrigerator (10) is arranged on the TEC refrigerator power supply (11), and the high-power semiconductor laser (9) is sequentially connected with a first collimating mirror (20), a first engineering diffuser (21) and a second polarizing plate (22);
the computer (1) is also connected with a phase-locked detection amplifier (39), and the phase-locked detection amplifier (39) is sequentially connected with a pre-amplifier (15), an HCT heat detector (17), a first polaroid (18) and a band-pass filter (19); the band-pass filter (19) is matched with a large off-axis parabolic mirror (14) for use, and the large off-axis parabolic mirror (14) is arranged on the first mounting support (13);
the phase-locked detection amplifier (39) is further connected with a second function generator (37), the second function generator (37) is sequentially connected with a low-power semiconductor laser (35), a second collimating mirror (23), a second engineering diffuser (24), a third polarizing plate (25) and a focusing plate (26), the second engineering diffuser (24), the third polarizing plate (25) and the focusing plate (26) are embedded in a designated installation position of a small off-axis parabolic mirror (27), and the small off-axis parabolic mirror (27) is arranged on a second mounting support (32);
the computer (1) is also connected with a two-axis driver (33), the two-axis driver (33) is connected with a two-dimensional micro-displacement mobile station (30), an incubator (29) is arranged on the two-dimensional micro-displacement mobile station (30), and a test piece (28) to be tested is placed in the incubator (29).
2. The solid engine spray pipe adhesive curing viscosity photo-thermal characterization device based on broadband dual laser excitation according to claim 1, wherein the computer (1) is provided with 2 output signal ends and 1 input/output signal end, the computer (1) is connected with the phase-locked detection amplifier (39) through an input/output signal end Ethernet line (40), and the computer (1) is connected with the input signal end of the first function generator (4) through a first output signal end first type-B USB data line (3); the computer (1) is connected with the two-axis driver (33) through a second output signal end driving control line (41); the output signal end of the phase-locked detection amplifier (39) is connected with a second function generator (37) through a second BNC data line (38); an input signal end of the phase-locked detection amplifier (39) is connected with the preamplifier (15) through a high-performance radio-frequency coaxial cable (2); the second function generator (37) is connected with the low-power semiconductor laser (35) through a second B-type USB data line (36), and laser emitted by the low-power semiconductor laser (35) is transmitted to the second collimating mirror (23) through a second laser optical fiber (34);
a second engineering diffuser (24), a third polarizer (25) and a focusing plate (26) are embedded in a designated mounting position of a small off-axis parabolic mirror (27); the test piece (28) to be tested is placed in the incubator (29), the incubator (29) is placed on the two-dimensional micro-displacement moving table (30), and the position scanning detection of the test piece (28) to be tested is realized; the small off-axis parabolic mirror (27) is arranged on the second mounting support (32), and the large off-axis parabolic mirror (14) is arranged on the first mounting support (13); the HCT heat detector (17) is connected with an input signal end of the pre-amplifier (15) through a coaxial cable (16) to realize amplification of the obtained photo-thermal signal; the band-pass filter (19) and the first polaroid (18) are fixed in front of the HCT heat detector (17) through threaded connection, and the band-pass filter (19) can effectively filter near infrared excitation light; the output signal end of the first function generator (4) is connected with a high-power semiconductor laser power supply (6) through a first BNC data line (5); the high-power semiconductor laser power supply (6) is connected with the high-power semiconductor laser (9) and the TEC refrigerator power supply (11) through the semiconductor laser power supply line (7) and the TEC refrigerator power supply line (8), and the TEC semiconductor refrigerator (10) is positioned between the high-power semiconductor laser (9) and the TEC refrigerator power supply (11); the high-power semiconductor laser (9) transmits laser light to the first collimating mirror (20) through the first laser fiber (12), and a first engineering diffuser (21) and a second polarizer (22) are respectively arranged in front of the first collimating mirror (20).
3. A method for photo-thermal characterization of cured viscosity of a solid engine nozzle adhesive based on broadband dual laser excitation according to claim 1 or 2, wherein the characterization method comprises the following steps,
step one: defining a test piece (28) to be tested, placing the test piece to be tested in an incubator (29), opening the incubator (29), and setting the temperature to 80 ℃;
step two: starting a solid engine spray pipe adhesive curing viscosity photo-thermal characterization device based on broadband double-laser excitation;
step three: adjusting the position of a two-dimensional micro-displacement moving table (30) to enable a test piece (28) to be tested to be positioned at the focal position of a small off-axis parabolic mirror (27), and simultaneously adjusting a first mounting support (13) to enable an element detected by an HCT heat detector (17) to be positioned at the focal position of a large off-axis parabolic mirror (14);
step four: the computer (1) sends out an instruction, and the low-power semiconductor laser (35) generates laser with the modulation frequency of 0Hz through the phase-locked detection amplifier (39) and the second function generator (37), so that whether the laser spot size is normal is checked;
meanwhile, the computer (1) sends out an instruction, the high-power semiconductor laser power supply (6) generates laser with the modulation frequency of 0Hz through the first function generator (4), and at the moment, whether the laser emitted by the first collimating mirror (20) completely covers a test piece (28) to be tested is checked;
step five: observing whether the phase-locked detection amplifier (39) acquires the signal from the HCT heat detector (17) in the range, and if not, adjusting the preamplifier (15), amplifying or reducing the gain;
step six: when the temperature of a test piece (28) to be tested reaches a set temperature, starting timing, and carrying out broadband dual-laser excited adhesive curing viscosity photo-thermal characterization test in 0 hour (0 h), wherein the modulation frequency band range of a low-power semiconductor laser (35) is set as the range, and the frequency of a high-power semiconductor laser power supply (6) is set as 0Hz, and the power is 45W;
step seven: then, carrying out broadband dual-laser excited adhesive curing viscosity photo-thermal characterization test after every 1h, then judging whether the adhesive is the optimal bonding time by combining a worker master hand touch mode, recording photo-thermal response characteristic data, and recording for 0-5 hours;
step eight: after 5 hours of test data are completed, a dual-laser excitation induction heat radiation signal response model is required to be established according to the characteristics of a test piece (28) to be tested so as to realize quantitative evaluation of the solidification degree;
step nine: after the test is finished, the broadband scanning result and the fitting result obtained by the test are saved, meanwhile, the computer (1) controls the high-power semiconductor laser power supply (6) and the low-power semiconductor laser (35) to enable the light intensity of the high-power semiconductor laser power supply to be 0, and simultaneously controls the two-axis driver (33) to enable the two-dimensional micro-displacement mobile station (30) to be zeroed, and the heating function of the incubator (29) is closed;
step ten: after the test is finished, after 5 minutes of interval, sequentially closing a first function generator (4), a high-power semiconductor laser power supply (6), a two-axis driver (33), a pre-amplifier (15), an HCT heat detector (17), a second function generator (37) and a phase-locked detection amplifier (39); after the incubator (29) returns to room temperature, the test piece (28) to be tested is placed in a designated storage container.
4. The method for photo-thermal characterization of the curing viscosity of the solid engine nozzle adhesive based on broadband dual-laser excitation according to claim 3, wherein the feature of the test piece to be tested in the step eight is specifically that a dual-laser excitation induced thermal radiation signal response model is established,
k in the formula 1 The response gain of the HCT heat detector is k, the thermal conductivity of the test piece to be tested is k, h is the convective heat transfer coefficient existing on the surface of the test piece to be tested, and alpha IR (lambda) is the infrared absorption coefficient of the test piece to be tested; l (L) 1 The thickness of the test piece to be tested; sigma is Stefan-Boltzmann constant; beta is the light absorption attenuation coefficient of the test piece to be tested.
5. The method for photo-thermal characterization of the curing viscosity of the solid engine nozzle adhesive based on broadband dual laser excitation according to claim 4, wherein the relationship between the thermal radiation signal and the surface temperature signal of the test piece to be tested is as follows,
wherein K is a system scale factor; p (λ) is the HCT heat detector spectral response band; epsilon is the emissivity of the test piece to be tested; t (T) 0 Is at room temperature; lambda (lambda) 1 ,λ 2 The spectral response ranges of HCT heat detectors, respectively.
6. The solid engine spray pipe adhesive curing viscosity photo-thermal characterization method based on broadband dual laser excitation according to claim 5 is characterized in that as the signal S (omega) is complex, the amplitude frequency and phase frequency dynamic response of the photo-thermal radiation of the test piece to be tested under the action of the modulated laser can be directly obtained, namely:
the multi-parameter fitting is to find the optimal parameters, so that the amplitude and phase information calculated by the mathematical model in the optimal parameters and the amplitude and phase information obtained by the test are brought into the objective function G, and the G reaches the minimum value.
7. The method for photo-thermal characterization of curing viscosity of solid engine nozzle adhesive based on broadband dual laser excitation according to claim 6, wherein the objective function of the multi-parameter fitting is,
z in 1 ,Z 2 Is a scale factor; g is a coefficient to be fitted; n is the number of acquisition points; f (f) i Is the modulation frequency; ampl T ，Phase T To calculate amplitude and phase; ampl E ，Phase E Amplitude and phase characteristic data obtained for the trial.
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