CN112595677A - Monitoring method, system, storage medium and device for polymer photocuring process - Google Patents
Monitoring method, system, storage medium and device for polymer photocuring process Download PDFInfo
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- CN112595677A CN112595677A CN202011331046.3A CN202011331046A CN112595677A CN 112595677 A CN112595677 A CN 112595677A CN 202011331046 A CN202011331046 A CN 202011331046A CN 112595677 A CN112595677 A CN 112595677A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/16—Measuring arrangements characterised by the use of optical techniques for measuring the deformation in a solid, e.g. optical strain gauge
- G01B11/161—Measuring arrangements characterised by the use of optical techniques for measuring the deformation in a solid, e.g. optical strain gauge by interferometric means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
- G01N21/45—Refractivity; Phase-affecting properties, e.g. optical path length using interferometric methods; using Schlieren methods
Abstract
The invention provides a monitoring method, a system, a storage medium and a device of a polymer photocuring process, aiming at the technical problem that the prior art can not carry out non-contact on-line real-time monitoring on the polymer photocuring process, wherein the method comprises the following steps: s01, performing spectral domain optical coherence tomography on the polymer to be detected through preset optical equipment, and acquiring an interference spectral signal generated by the polymer to be detected in real time; the interference spectrum signal comprises information of phase and optical depth; s02, calculating the phase variation caused by the curing process by extracting the phase and the optical depth in the interference spectrum signal; calculating the respective optical depth variation of the upper surface and the lower surface of the measured polymer according to the phase variation; and S03, calculating the refractive index variation and the shrinkage strain of the measured polymer according to the optical depth variation of the upper surface and the lower surface of the measured polymer.
Description
Technical Field
The invention relates to the technical field of polymer photocuring, in particular to a non-contact monitoring technology in a polymer photocuring process, and more particularly relates to a monitoring method, a monitoring system, a storage medium and a monitoring device in the polymer photocuring process.
Background
The photocuring technology of polymer materials is a novel energy-saving and environment-friendly technology, and has attracted more and more attention in the fields of coating preparation, electronic packaging, surface bonding, tooth restoration and the like. Photocuring of polymeric materials undergoes a physical state change, typically from a liquid to a gel, and then from the gel to a solid.
The currently popular curing monitoring methods mainly include differential scanning calorimetry, dynamic thermomechanical analysis, dielectric analysis, etc., which can also be used for monitoring the photo-curing of polymers. For example, chinese patent application publication No. CN 109312019 a, published at 2019.02.05: the reactive polymer, the photocurable resin composition and the laminate were measured for the progress of photocuring by using a differential scanning calorimeter and detecting the temperature of the polymer. However, these prior methods have various problems in practical applications, such as that differential scanning calorimetry and dynamic thermomechanical analysis cannot achieve on-line measurement, and thus are not suitable for industrial production and manufacturing; the dielectric analysis method is a contact measurement method, and the operation process is complex and cannot be applied to some practical application scenes.
Disclosure of Invention
Aiming at the limitation of the prior art, the invention provides a monitoring method, a monitoring system, a monitoring storage medium and a monitoring device for a polymer photocuring process, wherein the technical scheme adopted by the invention is as follows:
a method of monitoring the photocuring of a polymer comprising the steps of:
performing spectral domain optical coherence tomography on the polymer to be detected through preset optical equipment, and acquiring an interference spectrum signal generated by the polymer to be detected in real time; the interference spectrum signal comprises information of phase and optical depth;
calculating the phase variation caused by the curing process by extracting the phase and the optical depth in the interference spectrum signal; calculating the respective optical depth variation of the upper surface and the lower surface of the measured polymer according to the phase variation;
and calculating the refractive index variation and the shrinkage strain of the measured polymer according to the optical depth variation of the upper surface and the lower surface of the measured polymer.
Compared with the prior art, the monitoring method of the polymer photocuring process combines the phase contrast method and the spectral domain optical coherence tomography technology, overcomes the defects of the prior art, can perform non-contact real-time online monitoring, realizes simultaneous measurement of shrinkage strain and refractive index variation in the photocuring process, is very suitable for practical application of industrial production and manufacturing, and has good application prospect.
Further, the interference spectrum signal is expressed by the following formula:
wherein, I represents light intensity, k represents wave number, t represents time, DC represents direct current component, AC represents self-coherent component, M represents the number of the measured polymer surface, and j represents the measured polymer surface; i isRRepresenting the intensity of the reflected light of a reference surface in said optical device, IjRepresenting the intensity of the reflected light of the j surface of the measured polymer;
φj(t) represents the phase, phi, of the interference spectral signalj(t)=φj0+2kΛj(t);φj0Representing the initial phase, Λ, of the interference spectral signalj(t) represents an optical depth.
As a preferable scheme, the optical depth variation is obtained according to the following formula:
wherein, Delta Lambdaj(t) represents the amount of change in optical depth, λcRepresenting said optical apparatusCentral wavelength of the light source, Δ φj(t) represents the amount of phase change, t0Denotes an initial time of photocuring of the polymer to be measured, unwrap { } denotes phase unwrapping, diff [ ]]Indicating the differential phase.
Preferably, the refractive index change Δ n (t) is obtained according to the following formula:
wherein A is a point where the light beam of the optical equipment passes on the upper surface of the measured polymer, B is a point where the light beam of the optical equipment passes on the lower surface of the measured polymer, and d represents the distance between the point A and the point B; delta ΛA(t) represents the amount of change in optical depth, Δ Λ, of the upper surface of the polymer to be measuredB(t) represents the amount of change in optical depth of the lower surface of the polymer to be measured; n is0The initial refractive index of the polymer tested is indicated.
Further, the shrinkage strain epsilon (t) is obtained according to the following formula:
through the improvement, when the invention is particularly applied to monitoring in the polymer photocuring process, the change of a specific physical quantity in the polymer photocuring process can be focused, and the simultaneous measurement of shrinkage strain and refractive index change in the photocuring process is realized.
The present invention also provides the following:
a system for monitoring the photocuring of a polymer, comprising:
the interference spectrum signal acquisition module is used for carrying out spectral domain optical coherence tomography on the measured polymer through preset optical equipment and acquiring interference spectrum signals generated on the upper surface and the lower surface of the measured polymer in real time; the interference spectrum signal comprises information of phase and optical depth;
the optical depth variation acquisition module is used for calculating the phase variation caused in the curing process by extracting the phase and the optical depth in the interference spectrum signal; calculating the respective optical depth variation of the upper surface and the lower surface of the measured polymer according to the phase variation;
and the curing monitoring index acquisition module is used for calculating the refractive index variation and the shrinkage strain of the measured polymer according to the respective optical depth variation of the upper surface and the lower surface of the measured polymer.
As an alternative, the optical device comprises a broadband light source, a reference surface, a CCD camera, and:
the first convex lens, the cylindrical lens, the beam splitter prism and the second convex lens are sequentially arranged from the broadband light source output end to the measured object along the main optical axis;
the plane reflector, the third convex lens and the neutral optical filter are sequentially arranged from the light splitting prism to the reference surface along the first light splitting axis;
and the diffraction grating and the fourth convex lens are sequentially arranged from the beam splitter prism to the CCD camera along a second beam splitting axis.
Preferably, the optical device further includes a filter disposed between the diffraction grating and the fourth convex lens along the second split axis.
A storage medium having stored thereon a computer program for implementing the steps of the method for monitoring a photocuring process of a polymer as described above when executed by a processor.
A monitoring apparatus comprising an optical device, a storage medium, a processor, and a computer program stored in the storage medium and executable by the processor, the computer program, when executed by the processor, implementing the steps of the aforementioned monitoring method for polymer photocuring process by the optical device.
Drawings
FIG. 1 is a flow chart illustrating steps of a method for monitoring a polymer photocuring process according to an embodiment of the present invention;
FIG. 2 is a schematic cross-sectional profile of a polymer droplet being tested in an embodiment of the invention;
FIG. 3 is a schematic diagram showing the variation of optical depth at points A and B with respect to photocuring time of a polymer to be tested in an embodiment of the present invention;
FIG. 4 is a schematic diagram showing the refractive index change and shrinkage strain change of a polymer to be tested in the photo-curing process according to an embodiment of the present invention;
FIG. 5 is a schematic view of a monitoring system for monitoring the photocuring of a polymer according to an embodiment of the present invention;
FIG. 6 is a schematic diagram of an optical path of an optical apparatus provided in an embodiment of the present invention;
description of reference numerals: 1. an interference spectrum signal acquisition module; 2. an optical device; 21. a broadband light source; 22. a reference surface; 23. a CCD camera; 24. a first convex lens; 25. a cylindrical mirror; 26. a beam splitter prism; 27. a second convex lens; 28. a plane mirror; 29. a third convex lens; 210. a neutral optical filter; 211. a diffraction grating; 212. a filter; 213. a fourth convex lens; 3. an optical depth variation obtaining module; 4. and a curing monitoring index acquisition module.
Detailed Description
The drawings are for illustrative purposes only and are not to be construed as limiting the patent;
it should be understood that the embodiments described are only some embodiments of the present application, and not all embodiments. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments in the present application without any creative effort belong to the protection scope of the embodiments in the present application.
The terminology used in the embodiments of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the embodiments of the present application. As used in the examples of this application and the appended claims, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any and all possible combinations of one or more of the associated listed items.
When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present application. Rather, they are merely examples of apparatus and methods consistent with certain aspects of the application, as detailed in the appended claims. In the description of the present application, it is to be understood that the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not necessarily used to describe a particular order or sequence, nor are they to be construed as indicating or implying relative importance. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.
Further, in the description of the present application, "a plurality" means two or more unless otherwise specified. "and/or" describes the association relationship of the associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a exists alone, A and B exist simultaneously, and B exists alone. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship. The invention is further illustrated below with reference to the figures and examples.
In order to solve the limitation of the prior art, the present embodiment provides a technical solution, and the technical solution of the present invention is further described below with reference to the accompanying drawings and embodiments.
Example 1
Referring to fig. 1, a method for monitoring a polymer photocuring process includes the following steps:
s01, performing spectral domain optical coherence tomography on the polymer to be detected through preset optical equipment, and acquiring an interference spectral signal generated by the polymer to be detected in real time; the interference spectrum signal comprises information of phase and optical depth;
s02, calculating the phase variation caused by the curing process by extracting the phase and the optical depth in the interference spectrum signal; calculating the respective optical depth variation of the upper surface and the lower surface of the measured polymer according to the phase variation;
and S03, calculating the refractive index variation and the shrinkage strain of the measured polymer according to the optical depth variation of the upper surface and the lower surface of the measured polymer.
Compared with the prior art, the monitoring method of the polymer photocuring process combines the phase contrast method and the spectral domain optical coherence tomography technology, overcomes the defects of the prior art, can perform non-contact real-time online monitoring, realizes simultaneous measurement of shrinkage strain and refractive index variation in the photocuring process, is very suitable for practical application of industrial production and manufacturing, and has good application prospect.
As a preferred embodiment, the interference spectrum signal is expressed by the following formula:
wherein, I represents light intensity, k represents wave number, t represents time, DC represents direct current component, AC represents self-coherent component, M represents the number of the measured polymer surface, and j represents the measured polymer surface; i isRRepresenting the intensity of the reflected light of a reference surface in said optical device, IjRepresenting the intensity of the reflected light of the j surface of the measured polymer;
φj(t) represents the phase, phi, of the interference spectral signalj(t)=φj0+2kΛj(t);φj0Representing the initial phase, Λ, of the interference spectral signalj(t) represents an optical depth.
In particular, due to the amplitude of the interference signal and the reflected light intensity IjProportional to frequency and optical depth Λj(t) is inversely proportional, so that after the interference signal is subjected to Fourier transform along the k axis, the amplitude-frequency characteristic reflects the internal depth information of the measured polymer; since the phase variation of the interference signal is proportional to the optical depth variation, the phase variation at different times is calculated by using a phase contrast method, so that the optical depth variation of each surface of the polymer to be measured can be obtained.
Therefore, as a preferred embodiment, the optical depth variation is obtained according to the following formula:
wherein, Delta Lambdaj(t) represents the amount of change in optical depth, λcRepresenting the central wavelength, Δ φ, of the light source of the optical devicej(t) represents the amount of phase change, t0Denotes an initial time of photocuring of the polymer to be measured, unwrap { } denotes phase unwrapping, diff [ ]]Indicating the differential phase.
In particular, due to the central wavelength λ of the light sourcecAbout 800nm, the change of the optical depth of 400nm is shown when the phase changes by 2 pi, and the change delta lambda of the optical depth can be realizedj(t) high sensitivity monitoring.
As a preferred embodiment, the refractive index change Δ n (t) is obtained by the following formula:
wherein A is a point where the light beam of the optical equipment passes on the upper surface of the measured polymer, B is a point where the light beam of the optical equipment passes on the lower surface of the measured polymer, and d represents the distance between the point A and the point B; delta ΛA(t) represents the amount of change in optical depth, Δ Λ, of the upper surface of the polymer to be measuredB(t) represents the amount of change in optical depth of the lower surface of the polymer to be measured; n is0The initial refractive index of the polymer tested is indicated.
Further, the shrinkage strain epsilon (t) is obtained according to the following formula:
specifically, in an alternative embodiment, the depth resolution of the optical device is 7.5 μm, the depth range is 3mm, and the measurement speed is 20 frames/second; the specific polymer to be detected is in a droplet shape; in this embodiment, first, the cross-sectional profile of the polymer to be measured can be obtained according to the collected spectrum of the interference spectrum, as shown in fig. 2, from which the positions of points a and B can be obtained; extracting the variation curve of the phase of the point A and the point B along with the photocuring time, and further calculating the variation of the optical depth, as shown in fig. 3; finally, the shrinkage strain amount and the refractive index variation amount of the measured polymer in the curing process are calculated and obtained, as shown in fig. 4.
Example 2
A system for monitoring the photocuring process of a polymer, referring to fig. 5, comprising:
the interference spectrum signal acquisition module 1 is used for performing spectral domain optical coherence tomography on the polymer to be detected through a preset optical device 2, and acquiring an interference spectrum signal generated by the polymer to be detected in real time; the interference spectrum signal comprises information of phase and optical depth;
the optical depth variation obtaining module 3 is configured to calculate a phase variation caused in a curing process by extracting a phase and an optical depth in the interference spectrum signal; calculating the respective optical depth variation of the upper surface and the lower surface of the measured polymer according to the phase variation;
and the curing monitoring index acquisition module 4 is used for calculating the refractive index variation and the shrinkage strain of the measured polymer according to the respective optical depth variation of the upper surface and the lower surface of the measured polymer.
As an alternative embodiment, referring to fig. 6, the optical device 2 comprises a broadband light source 21, a reference plane 22, a CCD camera 23, and:
a first convex lens 24, a cylindrical lens 25, a beam splitter prism 26 and a second convex lens 27 which are arranged in sequence from the output end of the broadband light source 21 to the measured object along the main optical axis;
a plane mirror 28, a third convex lens 29 and a neutral filter 210 which are arranged in sequence from the beam splitter prism 26 to the reference surface 23 along a first beam splitting axis;
and a diffraction grating 211 and a fourth convex lens 213 arranged in this order from the beam splitter prism 26 to the CCD camera 23 along the second beam splitting axis.
Specifically, referring to the white arrow direction in fig. 6, during the monitoring process, the light emitted from the broadband light source 21 first illuminates a cross section of the polymer to be detected under the collimation and focusing actions of the first convex lens 24, the cylindrical lens 25 and the second convex lens 27; the reflected light of the reference surface 22 and the reflected light of the reference surface are superimposed on each other at the beam splitter prism 26 to form an interference signal, which is received by a spectrometer composed of the diffraction grating 211, the fourth convex lens 213 and the CCD camera 23. The third convex lens 29 is used to focus light on the reference surface 22, the plane mirror 28 is used to reduce the volume of the optical device, and the neutral filter 210 is used to attenuate the light intensity of the reference surface.
As a preferred embodiment, the optical device 2 further comprises a filter 212 disposed between the diffraction grating 211 and the fourth convex lens 213 along the second optical branch axis.
Specifically, the filter 212 is used for filtering light out of the band of the broadband light source 21; thereby, light emitted by the curing light source as well as external ambient light may be filtered out.
Example 3
A storage medium having stored thereon a computer program for implementing the steps of the method for monitoring a polymer photocuring process as described above when executed by a processor.
Example 4
A monitoring apparatus comprising an optical device, a storage medium, a processor, and a computer program stored in the storage medium and executable by the processor, the computer program, when executed by the processor, implementing the steps of the method for monitoring a polymer photocuring process as described above by the optical device.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. A method of monitoring the photocuring of a polymer, comprising the steps of:
s01, performing spectral domain optical coherence tomography on the polymer to be detected through preset optical equipment, and acquiring an interference spectral signal generated by the polymer to be detected in real time; the interference spectrum signal comprises information of phase and optical depth;
s02, calculating the phase variation caused by the curing process by extracting the phase and the optical depth in the interference spectrum signal; calculating the respective optical depth variation of the upper surface and the lower surface of the measured polymer according to the phase variation;
and S03, calculating the refractive index variation and the shrinkage strain of the measured polymer according to the optical depth variation of the upper surface and the lower surface of the measured polymer.
2. The method of claim 1, wherein the interference spectrum signal is expressed by the following formula:
wherein, I represents light intensity, k represents wave number, t represents time, DC represents direct current component, AC represents self-coherent component, M represents the number of the measured polymer surface, and j represents the measured polymer surface; i isRRepresenting the intensity of the reflected light of a reference surface in said optical device, IjRepresenting the intensity of the reflected light of the j surface of the measured polymer;
φj(t) represents the phase, phi, of the interference spectral signalj(t)=φj0+2kΛj(t);φj0Representing the initial phase, Λ, of the interference spectral signalj(t) represents an optical depth.
3. The method of claim 2, wherein the optical depth variation is obtained according to the following formula:
wherein, Delta Lambdaj(t) represents the amount of change in optical depth, λcRepresenting the central wavelength, Δ φ, of the light source of the optical devicej(t) represents the amount of phase change, t0Denotes an initial time of photocuring of the polymer to be measured, unwrap { } denotes phase unwrapping, diff [ ]]Indicating the differential phase.
4. The method for monitoring the photocuring process of a polymer according to any one of claims 1 to 3, wherein the refractive index change Δ n (t) is obtained by the following formula:
wherein A is a point where the light beam of the optical equipment passes on the upper surface of the measured polymer, B is a point where the light beam of the optical equipment passes on the lower surface of the measured polymer, and d represents the distance between the point A and the point B; delta ΛA(t) represents the amount of change in optical depth, Δ Λ, of the upper surface of the polymer to be measuredB(t) represents the amount of change in optical depth of the lower surface of the polymer to be measured; n is0The initial refractive index of the polymer tested is indicated.
6. a system for monitoring the photocuring of a polymer, comprising:
the interference spectrum signal acquisition module (1) is used for carrying out spectral domain optical coherence tomography on the polymer to be detected through preset optical equipment (2) and acquiring an interference spectrum signal generated by the polymer to be detected in real time; the interference spectrum signal comprises information of phase and optical depth;
the optical depth variation acquisition module (3) is used for calculating the phase variation caused by the curing process by extracting the phase and the optical depth in the interference spectrum signal; calculating the respective optical depth variation of the upper surface and the lower surface of the measured polymer according to the phase variation;
and the curing monitoring index acquisition module (4) is used for calculating the refractive index variation and the shrinkage strain of the measured polymer according to the optical depth variation of the upper surface and the lower surface of the measured polymer.
7. System for monitoring the photocuring process of polymers according to claim 6, characterized in that the optical device (2) comprises a broadband light source (21), a reference surface (22), a CCD camera (23), and:
the first convex lens (24), the cylindrical lens (25), the beam splitter prism (26) and the second convex lens (27) are sequentially arranged from the output end of the broadband light source (21) to the measured object along a main optical axis;
the plane mirror (28), the third convex lens (29) and the neutral filter (210) are sequentially arranged from the light splitting prism (26) to the reference surface (23) along the first light splitting axis;
and the diffraction grating (211) and the fourth convex lens (213) are sequentially arranged from the beam splitter prism (26) to the CCD camera (23) along a second beam splitting axis.
8. The system for monitoring a photocuring process of a polymer according to claim 7, wherein the optical device (2) further comprises a filter (212) disposed between the diffraction grating (211) and a fourth convex lens (213) along a second optical branch axis.
9. A storage medium having a computer program stored thereon, the computer program comprising: the computer program when executed by a processor implements the steps of the method of monitoring a polymer photocuring process as defined in any one of claims 1 to 5.
10. A monitoring device, characterized by: comprising an optical device, a storage medium, a processor, and a computer program stored in the storage medium and executable by the processor, the computer program, when executed by the processor, implementing the steps of the method for monitoring a photocuring process of a polymer as defined in any one of claims 1 to 5 by means of the optical device.
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CN114279984A (en) * | 2021-12-24 | 2022-04-05 | 广东工业大学 | Non-contact measurement system and method for researching polymerization shrinkage dynamics of dental composite material |
CN116559118A (en) * | 2023-07-11 | 2023-08-08 | 广东工业大学 | Polymer curing monitoring method, system and device based on light attenuation coefficient change |
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Cited By (4)
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CN114279984A (en) * | 2021-12-24 | 2022-04-05 | 广东工业大学 | Non-contact measurement system and method for researching polymerization shrinkage dynamics of dental composite material |
CN114279984B (en) * | 2021-12-24 | 2024-02-02 | 广东工业大学 | Non-contact measurement system and method for researching polymerization shrinkage dynamics of dental composite material |
CN116559118A (en) * | 2023-07-11 | 2023-08-08 | 广东工业大学 | Polymer curing monitoring method, system and device based on light attenuation coefficient change |
CN116559118B (en) * | 2023-07-11 | 2023-09-22 | 广东工业大学 | Polymer curing monitoring method, system and device based on light attenuation coefficient change |
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