KR20190065585A - Apparatus and method for analyzing properties of matter in real-time in reaction process of polymer material - Google Patents

Abstract

The present invention relates to a device and a method for real-time property analysis. The device comprises: a measurement sample having a harden polymer sample; a light source part for irradiating light; an interferometer which divides the light into two paths and recombines the branched light to cause an interference phenomenon; an image acquiring part for acquiring an interference pattern image by photographing the outgoing light from the interferometer; and an image processing part for calculating a refractive index by analyzing the interference pattern image.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus and a method for real-time physical property analysis in a reaction process of a polymer material,

The present invention relates to an apparatus and method for analyzing physical properties, and more particularly, to an apparatus and a method for analyzing a process of a curable polymer material in real time when the material is cured.

Thermosetting polymers such as phenol, urea, melamine, epoxy, unsaturated polyester, silicone, urethane, and polyamide are substances that are cured when heated and have a desired shape. These polymers are often formed by adding a catalyst or initiator to the base and then forming the formed foam through a curing process. However, depending on the composition ratio of each material, the material characteristics, for example, the curing point, are different. In the initial development, it is very important to set the curing point to a desired temperature in the development of the thermosetting polymer material.

When developing a polymer material, it is necessary to check the refractive index so that the composition of the polymer base, the catalyst and the initiator are changed, and the hardening point can be grasped. However, until now, there has been no apparatus that can confirm the refractive index in real time during the curing process. At most, after the curing process has been completed, the cured polymer sample is taken out of the chamber and the refractive index is measured afterwards to confirm the result.

Therefore, there is a need for a physical property analyzer capable of calculating the refractive index of the polymer material in real time during the curing process so that the composition ratio can be adjusted so that the curing process of the curable polymer material is cured at a desired curing point.

Published Patent Application No. 10-1998-063067

SUMMARY OF THE INVENTION The present invention provides a physical property analyzing apparatus and method capable of real-time analysis of the process when the curable polymer material is cured.

It is another object of the present invention to provide a measurement specimen used in a physical property analyzer to analyze a process of the curable polymer material in real time.

In order to solve these problems, an apparatus for real-time property analysis according to an embodiment of the present invention includes a metal plate having a through hole into which a curable polymer sample is injected, and an upper cover glass and a lower cover glass sandwiching the metal plate therebetween A light source section for irradiating light; a light source section for dividing the light into a first light path and a second light path, the through hole being disposed on the second light path, An image acquiring unit for acquiring at least three interference fringe images by photographing the outgoing light from the interferometer, and an image processor for analyzing the at least three fringe images to calculate a refractive index.

A specimen holder including a heater for fixing the measurement specimen and for providing heat to the curable polymer specimen.

The specimen holder may be disposed on the second optical path.

The specimen holder may further include a slide glass at upper and lower portions of the through hole.

The specimen holder may include a metal cover that surrounds the heater and forms a chamber together with the slide glass.

The specimen holder includes a metal cover that forms a chamber with the slide glass, the heater is disposed outside the chamber, and the polymer sample can be cured to the entire atmosphere temperature inside the chamber.

The specimen holder may further include temperature measurement means capable of measuring the temperature of the measurement specimen.

And the refractive index of the curable polymer sample can be calculated in real time in the course of heat transfer to the curable polymer sample by the heater.

A specimen holder for fixing the measurement specimen, and a curing light source for providing curing light to the curable polymer specimen.

The real-time property analyzing method according to another embodiment of the present invention includes the steps of preparing a measurement specimen provided with a curable polymer sample, disposing the measurement specimen in the optical path of the interferometer, applying heat to the measurement specimen, A step of curing the polymer sample, and a step of calculating the refractive index of the curable polymer sample in real time by analyzing the light obtained in the curing step.

The measurement specimen may include a metal plate having a through hole into which the curable polymer sample is injected, and an upper cover glass and a lower cover glass with the metal plate interposed therebetween.

And analyzing a refractive index graph generated by repeatedly calculating the refractive index of the curable polymer sample while curing the curable polymer sample to derive a curing point.

According to another embodiment of the present invention, there is provided an optical system including a light source for irradiating light, an interferometer for splitting the light into a first optical path and a second optical path and recombining the split light to cause an interference phenomenon, And an image processing unit for calculating the refractive index by analyzing the at least three interference fringe images, wherein the measurement specimen of the real-time physical property analyzing apparatus comprises: And an upper cover glass and a lower cover glass sandwiching the metal plate, wherein the through hole is disposed on the second optical path of the interferometer.

The real-time property analyzing apparatus may further include a specimen holder including a heater for fixing the upper and lower cover glasses and providing heat to the curable polymer sample.

The specimen holder may further include a slide glass at upper and lower portions of the through hole.

The specimen holder may include a metal cover that surrounds the heater and forms a chamber together with the slide glass.

As described above, according to the real-time property analyzing apparatus and method according to the embodiment of the present invention, when the curable polymer material is cured in the curing process, the refractive index can be calculated in real time.

Therefore, according to the apparatus and method for real-time physical property analysis according to the embodiment of the present invention, when the polymer material is developed, the curing point can be grasped in real time while changing the composition ratio of the polymer base, the catalyst and the initiator.

1 is a schematic diagram of a real-time property analyzer according to an embodiment of the present invention.
2 is a schematic view of the measuring specimen shown in Fig.
3 is a front view showing the measurement specimen and the specimen holder shown in Fig.
4 is a cross-sectional view of AA 'shown in FIG.
5 is a graph showing the refractive indexes calculated according to the real-time property analyzer according to the embodiment of the present invention.
6 is a front view showing a measurement specimen and a specimen holder according to another embodiment of the present invention.
7 is a cross-sectional view of BB 'shown in FIG.
8 is a front view showing a measurement specimen and a specimen holder according to another embodiment of the present invention.
9 is a cross-sectional view of CC 'shown in FIG.
10 is a flowchart illustrating an operation of the real time physical property analyzing apparatus according to an embodiment of the present invention.

The terms and words used in the present specification and claims should not be construed as limited to ordinary or dictionary terms and the inventor may appropriately define the concept of the term in order to best describe its invention It should be construed as meaning and concept consistent with the technical idea of the present invention.

Therefore, the embodiments described in the present specification and the configurations shown in the drawings are merely the most preferred embodiments of the present invention and are not intended to represent all of the technical ideas of the present invention. Therefore, various equivalents And variations are possible.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings so that those skilled in the art can easily carry out the present invention.

FIG. 1 is a block diagram of a real time physical property analyzing apparatus according to an embodiment of the present invention, and FIG. 2 is a schematic diagram of a specimen shown in FIG. FIG. 3 is a front view showing the measurement specimen and the specimen holder shown in FIG. 2, FIG. 4 is a cross-sectional view of the specimen holder and the measurement specimen shown in FIG. 3, And Fig.

1 to 4, the real-time property analyzing apparatus according to an embodiment of the present invention includes a light source 110, an interferometer 120, an image acquiring unit 130, a measurement specimen 140, a specimen holder 150, a control unit 160, and an image processing unit 190.

The light source unit 110 includes a laser light source and a collimating lens that converts light emitted from the laser light source into parallel light.

The interferometer 120 is a measuring device using interference phenomenon of light. The interferometer 120 generates interference fringes by using interference of two light beams, and analyzes it to calculate the refractive index of a sample located on one optical path. That is, the interferometer 120 divides the light from the light source unit 110 into two light paths, places a sample on one light path to make a difference in the two light paths, ≪ / RTI >

As shown in FIG. 1, a Mach-Zehnder interferometer 120 includes a beam splitter 121, a first prism 122, a second prism 123, and a beam combiner 124, But not limited to, a Mach-Zehnder interferometer, a Michelson interferometer, a Fabry-Perot interferometer, a Toowayman interferometer, a Jamann interferometer, and the like.

The beam splitter 121 transmits 50% of the light incident from the light source unit 110, reflects 50% thereof, and branches to two mutually orthogonal optical paths. The first optical path is a path of light which is distributed to the right side of the beam splitter 121 and directed to the first prism 122. The second optical path is distributed to the lower end of the beam splitter 121 and passes through the measurement specimen 140, 2 prism 123 as shown in FIG. The beam combiner 124 combines the two lights reflected from the first prism 122 and the second prism 123 along the first and second optical paths, respectively. As a result, the two lights combine to cause interference and interference fringes.

2, the measurement specimen 140 includes an upper cover glass 141, a lower cover glass 143, and a metal plate 145 interposed therebetween. The metal plate 145 has a through hole 147 at a central portion thereof and the through hole 147 is placed on the second optical path so that light passes through the through hole 147. The shape of the through hole 147 may be circular, square, or triangular, but the interference fringe is circular, and the circular through-hole 147 can be more easily observed in the interference fringe. The metal plate 145 may be made of a copper plate, but is not limited thereto.

A metal plate 145 is adhered to the lower cover glass 143 and a liquid sample made of a polymer base and an additive is filled in the through hole 147 of the metal plate 145 with a syringe. At this time, it is preferable that the volume of the sample to be filled in the through hole 147 is equal to the volume of the through hole 147. Then, the upper cover glass 141 is adhered onto the metal plate 145. By doing so, the possibility of bubbles being generated is reduced, and the thickness of the measurement specimen 140 can be made uniform. The thickness of the measurement specimen 140 may be as thin as possible to reduce variations due to the thickness of the measurement specimen 140. The thickness of the metal plate 145 may be about 0.5 to 1.5 mm.

As described above, interference fringes are generated in the outgoing light of the interferometer 120 because the measurement specimen 140 exists in the second optical path. If there is no measurement specimen 140 (same optical path), constructive interference occurs and bright streaks are generated. If the length difference is different by half wavelength of the light wavelength, destructive interference occurs and darkens. The synthesized light has a varying interference magnitude depending on the difference in brightness, thereby drawing a sine wave. However, since the measurement specimen 140 is provided, the output light characteristic is changed. That is, the interference fringe is generated by the path difference in which the thickness d of the measurement specimen 140 and the refractive index n are reflected.

The optical path length is determined by n * d. The thickness d must be kept constant to correctly calculate the refractive index. That is, the upper and lower cover glasses 141 and 143 and the metal plate 145 are bonded to each other so that the thickness of the measurement specimen 140 does not vary due to a change in tilt or a bubble due to air or the like. If the thickness is not uniform, the refractive index can not be calculated correctly.

If there is no metal plate 145 having through-holes 147 in the measurement specimen 140 and the liquid sample is placed directly between the upper and lower cover glasses 141 and 143, it is difficult to keep the thickness of the measurement specimen constant And the refractive index can not be accurately calculated. However, as in the embodiment of the present invention, the metal plate 145 having the through-hole 147 exists in the measurement specimen 140 so that the liquid sample is placed in the through-hole 147 to uniformly measure the thickness of the measurement specimen 140 can do. In addition, the metal plate 145 can be manufactured easily and has a high thermal conductivity, which also helps to cure the liquid sample.

The specimen holder 150 includes an upper slide glass 154 and a lower slide glass 153 for passing light and fixing the measurement specimen 140 and a heater 151 for providing heat to the measurement specimen 140 . The thickness of the upper and lower slide glasses 153 and 154 is 1 mm or less, but the present invention is not limited thereto. The shape of the specimen holder 150 may be other than a square.

The heater 151 may be made of a thermoelectric element (TEC), but is not limited thereto. The heater 151 is disposed at both ends of the specimen holder 150 in the longitudinal direction. However, the present invention is not limited thereto. have. The temperature of the heater 151 is controlled by the controller 160.

Meanwhile, the specimen holder 150 may further include at least one means for measuring the temperature, such as a thermo couple, and the controller 160 may be connected to the measurement specimen 140 or the specimen holder 150, The internal temperature can be measured.

The specimen holder 150 is also disposed on the second optical path so that the light passes through the through hole 147 of the measurement specimen 140. In the actual experiment, a measurement specimen 140 having a polymer liquid sample is placed in a space between the heaters 151 in a state where the heater 151 is attached on the lower slide glass 153, and the upper slide glass (154).

The control unit 160 controls the temperature of the heater 151 to maintain a constant temperature and measures the refractive index of the liquid sample in real time in order to determine whether the liquid sample is cured while measuring the temperature inside the measurement sample 140 or the sample holder 150 . The temperature for curing is about 100 ° C to 140 ° C and the maximum temperature that can be discharged through the heater 151 is about 200 ° C so that there is no problem with deformation of the metal plate 145 or the upper and lower cover glasses 141 and 143 .

1, only the measurement specimen 140 is shown on the second optical path for the convenience of explanation. However, the measurement specimen 140 may be provided with the specimen holder 150 as shown in FIGS. 3 and 4 And is disposed on the second optical path.

The image obtaining unit 130 includes a camera and measures an outgoing light emitted by the interferometer 120 to generate an image in which an interference fringe appears. The camera may be a 3 CCD camera or a 1 CCD camera.

Since the interference fringe can be represented by an equation of three unknowns, it is necessary to obtain three or more interference fringe images under a certain condition in order to analyze the interference fringe. In the case of 3 CCD cameras, the light enters the camera, but there are two beam splitters inside, one prism exists to separate the incoming light into three, and the phase retarder to change the phase of the separated light by 120 degrees There are three. There are three CCDs at the end of each phase retarder, so that three interference fringe images having a phase difference of 120 degrees with respect to the input light can be simultaneously obtained.

In contrast, in the case of a single CCD camera, a means for delaying the phase of the light on the first optical path is further provided so that three images can be acquired by capturing at three different viewpoints. In the case of a low-speed camera that captures 30 frames per second, there is a time difference in image acquisition, whereas the heat of the heater 151 is constantly flowing into the measurement specimen 140 to change the curing state. It is possible that errors may be involved in interpreting the interference pattern. Therefore, a high-speed camera, preferably a high-speed camera of 100 frames per second or more, may be more accurate in calculating the refractive index.

The image processing unit 190 calculates the refractive index of the measurement specimen 140 with respect to the sample using at least three images generated by the image acquisition unit 130.

The fact that any material is cured means that the density of the material changes, and the refractive index changes on the photometric side. Therefore, when the refractive index is changed in the curing process, the refractive index is increased. At a certain moment or more, the refractive index is decreased. At the completion of curing, the refractive index is fixed. Referring to FIG. 5, as a method for determining the curing point, a straight line largely increasing firstly and a secondarily saturated straight line are connected and the intersection thereof is set as a curing point. When heated to a temperature of 120 占 폚, the measurement temperature at the point A where the inflection point of the refractive index appears is a curing point. Similarly, when the temperature is 100 ° C, the measurement temperature at the point B becomes 80 ° C, and the measurement temperature at the point C becomes the curing point.

3, the control unit 160 controls the temperature of the heater 151 in the specimen holder 150 and not only measures the temperature of the measurement specimen 140, but also controls the light generation timing of the light source unit 110 And controls each component of the real-time property analyzer 100, such as controlling the image acquisition timing of the image acquisition unit 130.

Hereinafter, a real-time property analyzing apparatus according to another embodiment of the present invention will be described in detail with reference to FIGS. 6 and 7. FIG. 6 is a front view of the specimen holder 180 in which the measurement specimen 170 is disposed, and FIG. 7 is a cross-sectional view of BB 'shown in FIG.

Since only the measurement specimen 140 and the specimen holder 150 of the real-time physical property analyzer 100 of the previous embodiment are different from each other and the remaining components are the same, the description of the same parts is omitted The measurement specimen 170 and the specimen holder 180 will be described only in terms of the difference.

The specimen holder 180 includes an upper glass 185 and a lower glass 187 that pass light and fix the measurement specimen 170, a heater 181 that provides heat to the measurement specimen 170, and a measurement specimen 170 And a metal cover 183 which surrounds the heater 181 and forms a chamber together with the upper and lower glasses 185 and 187. According to the specimen holder 180 of this type, since the metal cover 183 surrounds the chamber, the thermal conductivity is high and the curing process can be easily performed.

Meanwhile, the specimen holder 180 may include a plurality of thermocouples, and the controller 160 may measure the temperature of the measurement specimen 170 and the inside of the chamber. The heater 181 may be made of a thermoelectric element (TEC) and is disposed at both ends of the specimen holder 180 in the longitudinal direction, but is not limited thereto. The controller 160 controls the temperature of the heater 181 according to a signal from the thermocouple.

Although the measurement specimen 170 is shown to have a through-hole 177 having a rectangular shape, the measurement specimen 170 is not limited thereto. The through hole 177 is placed on the second optical path. The specimen holder 180 is also disposed on the second optical path so that the light passes through the through hole 177 of the measurement specimen 170.

The real-time property analyzing apparatus according to another embodiment of the present invention will now be described in detail with reference to FIGS. 8 and 9. FIG. FIG. 8 is a front view of the specimen holder 280 in which the measurement specimen 140 is disposed, and FIG. 9 is a cross-sectional view of the CC 'shown in FIG.

Since only the specimen holders 150 and 170 of the real-time physical property analyzer 100 of the previous two embodiments differ from each other and the remaining components are the same, the description of the same parts will be omitted, Only the specimen holder 280 will be described.

The specimen holder 280 surrounds the upper glass 285 and the lower glass 287 and the measurement specimen 140 which are disposed above and below the measurement specimen 140 while passing light therethrough and together with the upper and lower glasses 285 and 287, And at least one heater 281 for providing heat to the chamber. Since the specimen holder 280 of this type can harden the polymer sample at the entire atmosphere temperature inside the chamber by the heater 281, the polymer sample can be cured and have a uniform temperature gradient.

Meanwhile, the specimen holder 280 may include a plurality of thermocouples, and the controller 160 may measure the temperature of the measurement specimen 140 and the inside of the chamber. The heater 281 may be made of a thermoelectric element (TEC) and is disposed at both ends of the specimen holder 280 in the longitudinal direction, but is not limited thereto. The controller 160 controls the temperature of the heater 281 according to a signal from the thermocouple.

The measurement specimen 140 is shown to have a circular through-hole 147, but is not limited thereto. The through hole 147 is placed on the second optical path. The specimen holder 280 is also disposed on the second optical path so that the light passes through the through hole 147 of the measurement specimen 140.

In the embodiments of the present invention, the polymer sample is cured by the heat of the heater. However, when the polymer sample is cured by light such as UV or electron beam, the measurement sample and the sample holder are applied in the same manner A hardening point can be calculated. However, a light source such as UV may be employed in place of the heater in the specimen holder.

The operation of the real time physical property analyzing apparatus according to the embodiment of the present invention will now be described with reference to FIG. For convenience of explanation, the real-time property analyzing apparatus 100 of FIG. 1 will be described.

The metal plate 145 provided with the through hole 147 is adhered onto the lower cover glass 143 and the liquid polymer sample is injected into the through hole 147 and the upper cover glass 141 is adhered onto the metal plate 145 Thereby preparing the measurement specimen 140 (S610).

The measurement specimen 140 is placed on the specimen holder 150 disposed on the second optical path of the interferometer 120 and the through hole 147 of the measurement specimen 140 is also disposed on the second optical path, Through hole 147 (S620).

The heater 151 included in the specimen holder 150 is controlled to provide heat to the liquid polymer sample (S630).

The interferometer 120 generates optical interference by combining light through the first optical path and light through the second optical path, and the image acquiring unit 130 acquires at least three interference fringe images at step S640.

The image processing unit 190 calculates the refractive index by analyzing the interference fringes in at least three images obtained in step S640 (S650). The steps S630 to S650 are repeated to finally obtain the refractive index graph over time as shown in FIG. 5, and the refractive index graph is analyzed to derive the curing point.

According to the apparatus and method for real-time physical property analysis according to the embodiment of the present invention, the refractive index can be calculated by analyzing the interference fringes in real time during the curing process for curing the liquid polymer sample. By analyzing the change of the refractive index, Can be derived.

Therefore, when developing a polymer material, it is necessary to perform various curing experiments while changing the composition ratio of the polymer base, the catalyst and the initiator. Therefore, if the cure point can be grasped in real time during the curing experiment, the time for developing the polymer material is shortened, Can also be saved.

The foregoing detailed description is illustrative of the present invention. It is also to be understood that the foregoing is illustrative and explanatory of preferred embodiments of the invention only, and that the invention may be used in various other combinations, modifications and environments. That is, it is possible to make changes or modifications within the scope of the concept of the invention disclosed in this specification, the disclosure and the equivalents of the disclosure and / or the scope of the art or knowledge of the present invention. The foregoing embodiments are intended to illustrate the best mode contemplated for carrying out the invention and are not intended to limit the scope of the present invention to other modes of operation known in the art for utilizing other inventions such as the present invention, Various changes are possible. Accordingly, the detailed description of the invention is not intended to limit the invention to the disclosed embodiments. It is also to be understood that the appended claims are intended to cover such other embodiments.

100: Real-time property analyzer,
110: light source part,
120: interferometer,
130: image acquisition unit,
140, 170: measurement specimen,
150, 180: Specimen holder,
160:
190:

Claims (16)

A metal plate having a through hole into which a curable polymer sample is injected, and a measurement specimen including an upper cover glass and a lower cover glass sandwiching the metal plate,
A light source unit for irradiating light,
An interferometer for dividing the light into a first optical path and a second optical path, the through hole being disposed on the second optical path, and causing the branched light to recombine to cause an interference phenomenon,
An image acquiring unit for acquiring at least three interference fringe images by photographing the outgoing light from the interferometer, and
An image processing unit for analyzing the at least three interference fringe images to calculate a refractive index;
Time property analyzer. The method of claim 1,
Further comprising a specimen holder including a heater that fixes the measurement specimen and provides heat to the curable polymer specimen. 3. The method of claim 2,
And the specimen holder is disposed on the second optical path. 3. The method of claim 2,
Wherein the specimen holder further comprises a slide glass at the top and bottom of the through hole. 5. The method of claim 4,
Wherein the specimen holder includes a metal cover that surrounds the heater and forms a chamber together with the slide glass. 5. The method of claim 4,
Wherein the specimen holder includes a metal cover forming a chamber with the slide glass, the heater is disposed outside the chamber, and the polymer sample is cured to a total atmospheric temperature inside the chamber. 3. The method of claim 2,
Wherein the specimen holder further comprises temperature measuring means capable of measuring a temperature of the measurement specimen. 3. The method of claim 2,
Wherein the refractive index of the curable polymer sample is calculated in real time while heat is continuously transferred by the heater to cure the curable polymer sample. The method of claim 1,
And a curing light source for providing curing light to the specimen holder for fixing the specimen to be measured and the curable polymer specimen. Preparing a measurement specimen provided with a curable polymer sample,
Placing the measurement specimen in the optical path of the interferometer,
Applying heat to the measurement specimen to cure the curable polymer sample,
Analyzing the light obtained in the curing step and calculating the refractive index of the curable polymer sample in real time
Time property analysis method. 11. The method of claim 10,
Wherein the measurement specimen includes a metal plate having a through hole through which the curable polymer sample is injected, and an upper cover glass and a lower cover glass sandwiching the metal plate. 11. The method of claim 10,
And analyzing a refractive index graph generated by repeatedly calculating a refractive index of the curable polymer sample while curing the curable polymer sample to derive a curing point. An interferometer for diverting the light into a first optical path and a second optical path and recombining the diverged light to cause an interference phenomenon; an optical system for imaging at least three interference fringe images And an image processing unit for calculating the refractive index by analyzing the at least three interference fringe images,
A metal plate having a through hole through which the curable polymer sample is injected, and
An upper cover glass and a lower cover glass sandwiching the metal plate therebetween,
And the through hole is disposed on the second optical path of the interferometer. The method of claim 13,
Wherein the real time property analyzing apparatus further comprises a specimen holder including a heater for fixing the upper and lower cover glasses and for providing heat to the curable polymer sample. The method of claim 14,
Wherein the specimen holder further comprises a slide glass at the top and bottom of the through hole. 16. The method of claim 15,
The specimen holder including a metal cover surrounding the heater and forming a chamber with the slide glass.

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