CN101105452A - Temperature and solidification rate real-time monitoring device for polymer based composite material forming process - Google Patents

Temperature and solidification rate real-time monitoring device for polymer based composite material forming process Download PDF

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CN101105452A
CN101105452A CNA2007100726140A CN200710072614A CN101105452A CN 101105452 A CN101105452 A CN 101105452A CN A2007100726140 A CNA2007100726140 A CN A2007100726140A CN 200710072614 A CN200710072614 A CN 200710072614A CN 101105452 A CN101105452 A CN 101105452A
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optical fiber
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refractive index
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谢怀勤
陈幸开
刘淼
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Harbin Institute of Technology
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Abstract

The invention relates to a real-time synchronization monitoring device for monitoring the temperature solidification in the formation process of polymer base compound materials. The invention relates to a material formation monitoring device, which solved the problem of the prior technology that only the off-line measuring of the small test sample can be taken and the precision is low and the cost is high, and the real-time synchronous measuring can not be taken. The output terminal of the laser of the invention is connected with the first terminal port of the first coupler through an isolator, the second terminal port of the first coupler is connected with the terminal port of a sensing module, the third terminal port of the first coupler is connected with the first terminal port of the second coupler, and the second terminal port and the third terminal port are separately connected with an optical receiver and two input terminals, the two output terminals of the optical receiver are separately connected with the two input terminals of a signal processing system. One terminal of the optical fiber refractive index sensor in a sensing module is connected with the second terminal port of the first coupler, and the other terminal is connected with the Bragg optical grating. And the sensing module is buried in the material. Online inspecting is adopted, and the heating temperature and the heating time are adjusted according to the solidification; and the product performance and the productivity are enhanced, the production cycle is reduced and the energy is saved and the cost is reduced.

Description

Real-time synchronous monitoring device for temperature and curing degree in forming process of polymer-based composite material
Technical Field
The invention relates to the technical field of real-time monitoring and analysis of process parameters in an industrial production process, in particular to a material forming monitoring device.
Background
The polymer-based composite material has a complex forming process, macroscopically changes from liquid to solid, microscopically linear high molecules form a three-dimensional network structure through polymerization, and the heat transfer process and the polymerization are mutually influenced and coupled. The curing degree directly influences the physical and chemical properties of the composite material, so the curing degree can be used as a characterization index of the composite material properties. In the forming process, if the heating temperature is too high and too fast, the polymerization reaction is violent, the internal stress of the product is large, microcracks are easy to generate, and the strength is reduced. And the heating temperature is too low, the curing degree is not enough, and the strength and the rigidity of the product can not meet the use requirements. The curing reaction rate can be controlled by adjusting the temperature, and further, the curing degree of the product can be controlled. Therefore, the temperature and the curing degree need to be measured synchronously in real time by double parameters so as to effectively control the production process of the composite material.
The existing detection of temperature and curing degree in the production process of polymer matrix composite materials mainly comprises single measurement of temperature and curing degree. The method for monitoring the curing degree is few, including a dynamic spring method, a dynamic Differential Scanning Calorimetry (DSC), an infrared spectrum method, a dielectric method and the like, most of the methods are only suitable for small test pieces or off-line curing degree monitoring, namely, the production can be carried out only according to a curing procedure obtained based on a trial and error experiment, and the curing degree is mostly used for carrying out 'after-the-fact' detection on products. And the method is not widely applied to actual production due to low measurement precision, high cost and the like. At present, the manufacturing process of the polymer-based composite material cannot obtain the information of the internal state of the material in real time, and the real-time monitoring data of the curing degree in the forming process is very little. As one of the important indexes for measuring the performance of thermosetting composite materials, the curing degree needs to be monitored by an effective and reliable means in the production process of polymer matrix composite materials.
With the intensive research on the optical fiber sensing technology and the increasing maturity of the technology, the research on the molding process of the optical fiber sensor monitoring composite material is started abroad at the end of the 80 th 20 th century, and the research contents relate to the influence of the optical fiber on the mechanical property of the composite material, the optical fiber embedding technology, the optical fiber curing monitoring sensor, the extraction and evaluation of curing information and the like.
In the present Chinese patent, the application number is 00123120.0, the publication number is CN1350174, the publication number is 2002.05.22, the name is a composite material optical fiber curing monitoring method and a patent of a special optical fiber, it is mentioned that an embedded special multimode optical fiber is adopted to firstly complete the online real-time detection of the composite material process, then the same optical fiber is applied to the vibration detection measurement of the material service period, the lifelong multifunctional measurement from the material manufacturing to the using process is really realized, and the curing and vibration detection integration is achieved.
Many scholars use grating optical fibers to measure the temperature of a composite material in real time in the molding process, and adjust process parameters in the production process according to the temperature change condition inside the composite material. However, the temperature is monitored singly, and the process parameters can only be adjusted according to the determined curing process, but cannot be adjusted according to the product performance indexes in the actual production process.
Disclosure of Invention
The invention provides a real-time synchronous monitoring device for the temperature curing degree in the forming process of a polymer-based composite material, aiming at solving the defects that in the prior art, only small-sized test pieces can be measured off line, the measurement precision is low, the cost is high and the like, and the device is not widely applied in actual production, and the temperature and the curing degree in the production process cannot be synchronously monitored in real time, so that the heating temperature and the heating time cannot be adjusted according to the curing degree.
The invention is composed of a laser 1, an optical transmission line component 2, an optical receiver 3, a sensing module 6 and a signal processing system 7; the optical transmission line component consists of an isolator 2-1, a first coupler 2-2 and a second coupler 2-3, the output end of the laser 1 is connected with the input end of the isolator 2-1, the output end of the isolator 2-1 is connected with the first port 2-2-1 of the first coupler 2-2, the second port 2-2-2 of the first coupler 2-2 is connected with the port of the sensing module 6, the third port 2-2-3 of the first coupler 2-2 is connected with the first port 2-3-1 of the second coupler 2-3, the second port 2-3-2 and the third port 2-3-3 of the second coupler 2-3 are respectively connected with the two input ends of the optical receiver 3, and the two output ends of the optical receiver 3 are respectively connected with the two data input ends of the signal processing system 7; the sensing module 6 consists of an optical fiber refractive index sensor 6-1 and a Bragg grating 6-2; the optical fiber refractive index sensor 6-1 and the Bragg grating 6-2 are connected in series, one end of the optical fiber refractive index sensor 6-1 is connected with the second port 2-2-2 of the first coupler 2-2, the other end of the optical fiber refractive index sensor 6-1 is connected with one end of the Bragg grating 6-2, and the sensing module 6 is embedded in the molding material 8 to be measured.
The core of the invention is to realize real-time synchronous monitoring of the temperature and the curing degree in the forming process (dynamic and static) of the polymer-based composite material. The basic working principle is that the optical modulation technology is utilized to superpose the detected signal on the carrier light wave transmitted by the fiber core in different modes, and after the modulation process is finished, the signal light carrying the detected parameter information is coupled to the optical detector through the receiving fiber, so that the optical signal is converted into an electric signal, and finally the electric signal is processed by the signal analysis system to obtain the measured signal. Specifically, a Bragg grating 6-2 and an optical fiber refractive index sensor 6-1 are connected in series on an optical fiber, the Bragg grating 6-2 is used for measuring the temperature change in the production process of the composite material, and the optical fiber refractive index sensor 6-1 is used for measuring the curing degree change of the polymer. Can be used as an important experimental means and basis for the control and optimization of the composite material forming process. The method has important significance in improving the product performance, shortening the production period, improving the production efficiency, saving energy and reducing the process cost. The temperature and the curing degree in the production process of the composite material can be synchronously monitored in real time, so that the temperature and the curing degree in the composite material at any moment can be known, and the heating temperature and the heating time can be adjusted according to the curing degree. The research results obtained at present show that the optical fiber sensor has good monitoring capability of the curing process, is well combined with the matrix of the composite material, hardly influences the mechanical property of the material, has obvious advantages compared with the traditional curing monitoring sensor, and provides a brand-new method and means for monitoring the process of the resin matrix composite material. The optical fiber sensor is mainly used for monitoring the curing process of the composite material, and is embedded in the prepreg paving layer in advance to measure the process parameters by utilizing the characteristics of small volume and high sensitivity. For the increasingly intense market competition of products, manufacturers seek to find optimal production process parameters in a manner of seeking, and the purpose of the method is to reduce the production cost of the products as much as possible under the condition of ensuring the product performance, so that the market competition capability of the products is improved. The real-time synchronous monitoring method of the temperature and the curing degree can reduce the energy consumption and the curing time as far as possible under the condition of ensuring that the performance of the product meets certain requirements, and has very important significance for controlling the technological parameters in the production process of the polymer-based composite material.
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FIG. 1 is a schematic structural view of the present invention; fig. 2 is a schematic structural view of the optical fiber refractive index sensor 6-1.
Detailed Description
The first embodiment is as follows: the present embodiment is described with reference to fig. 1 and 2, and is composed of a laser 1, an optical transmission line assembly 2, an optical receiver 3, a sensing module 6, and a signal processing system 7;
the optical transmission line component consists of an isolator 2-1, a first coupler 2-2 and a second coupler 2-3, the output end of the laser 1 is connected with the input end of the isolator 2-1, the output end of the isolator 2-1 is connected with the first port 2-2-1 of the first coupler 2-2, the second port 2-2-2 of the first coupler 2-2 is connected with the port of the sensing module 6, the third port 2-2-3 of the first coupler 2-2 is connected with the first port 2-3-1 of the second coupler 2-3, the second port 2-3-2 and the third port 2-3-3 of the second coupler 2-3 are respectively connected with the two input ends of the optical receiver 3, and the two output ends of the optical receiver 3 are respectively connected with the two data input ends of the signal processing system 7; the sensing module 6 consists of an optical fiber refractive index sensor 6-1 and a Bragg grating 6-2; the optical fiber refractive index sensor 6-1 and the Bragg grating 6-2 are connected in series, one end of the optical fiber refractive index sensor 6-1 is connected with the second port 2-2-2 of the first coupler 2-2, the other end of the optical fiber refractive index sensor 6-1 is connected with one end of the Bragg grating 6-2, and the sensing module 6 is embedded in the molding material 8 to be measured. The optical fiber refractive index sensor 6-1 changes the laser power through the change of the resin refractive index, and the Bragg grating 6-2 changes the reflection wavelength of the Bragg grating through the change of the temperature.
The second embodiment is as follows: the embodiment is described with reference to fig. 1, and the difference between the embodiment and the specific embodiment is that the optical receiver 3 is composed of a grating demodulator 4 and a laser power meter 5, an input end of the grating demodulator 4 and an input end of the laser power meter 5 are respectively connected to the second port 2-3-2 and the third port 2-3-3 of the second coupler 2-3, and an output end of the grating demodulator 4 and an output end of the laser power meter 5 are respectively connected to two data input ends of the signal processing system 7. Other components and connection modes are the same as those of the first embodiment.
The third concrete implementation mode: the present embodiment is described with reference to fig. 1 and 2, and is different from the first embodiment in that the pitch of the series connection of the optical fiber refractive index sensor 6-1 and the bragg grating 6-2 is 1 to 2cm, and the other components and connection modes are the same as those of the first embodiment.
The fourth concrete implementation mode: the present embodiment is described with reference to fig. 2, and the difference between the present embodiment and the present embodiment is that the optical fiber refractive index sensor 6-1 is a sensor device using an optical fiber coating layer and a cladding layer having a fiber stripping length L of 1550nm, and the stripped sensor segment is embedded in a molding material 8 to be measured, and is made into a degree-of-cure sensor segment by using light reflection characteristics. Other components and connection modes are the same as those of the first embodiment. The optical fiber is processed by two procedures, wherein the first procedure is to remove a coating layer of the optical fiber, concentrated sulfuric acid for analyzing alcohol is adopted to remove the coating layer, a section of optical fiber is immersed in the concentrated sulfuric acid for about 3 minutes, and the optical fiber is taken out and then washed by distilled water, so that the coating layer can be completely removed; the second step is to remove the cladding of the optical fiber, dip a section of the optical fiber with the coating removed into hydrofluoric acid with a concentration of 40% until the diameter of the dipped section of the optical fiber approaches the diameter of the core, which is considered to be completely removed, and rinse the optical fiber with distilled water after being taken out.
The fifth concrete implementation mode: the present embodiment is described with reference to fig. 2, and the fourth difference between the present embodiment and the present embodiment lies in that the optical fiber refractive index sensor 6-1 has an optical fiber stripping length L of 10 to 20mm. The other components and the connection mode are the same as those of the fourth embodiment.
The sixth specific implementation mode: the difference between the present embodiment and the specific embodiment is that the bragg grating 6-2 is a capillary-encapsulated bragg grating, and the capillary encapsulation plays a role in protecting the bragg grating and also improves the temperature sensitivity of the grating. Since the wavelength drift of the Bragg grating is in a linear relation with the temperature change, the temperature change can be converted by the central wavelength drift as long as the temperature sensitivity coefficient K of the Bragg grating is obtained. Other components and connection modes are the same as those of the first embodiment.
The seventh embodiment: the second difference between the present embodiment and the second embodiment lies in that interfaces are provided between the laser 1, the isolator 2-1, the grating demodulator 4, the laser power meter 5, the signal processing system 7 and the sensing module 6, and are FC fiber connectors, and the interfaces at both ends of the first coupler 2-2 and the second coupler 2-3 are FC-FC fiber connectors. Other components and connection modes are the same as those of the second embodiment mode.
The specific implementation mode is eight: the difference between the present embodiment and the specific embodiment is that the laser 1 emits laser light with a wavelength of 1550nm and a power of 20-30 mw; other components and connection modes are the same as those of the first embodiment. The wavelength of the laser light is matched to the wavelength of the bragg grating, which is generally 1550nm, so that a 1550nm light source is used. The power range is to ensure that the optical fiber refractive index sensor has a sufficient dynamic monitoring range (the difference between the optical power read by the power meter before curing and the optical power read by the power meter after curing), as long as the dynamic range can be obviously represented on the power meter, and the laser power is too large, which causes waste or difficulty in ensuring the stability of the output laser power, so that a laser source of 20-30 mw is adopted.
The specific implementation method nine: the present embodiment is different from the present embodiment in that the signal processing system 7 is a computer data processing system. Other components and connection modes are the same as those of the first embodiment.
The basic working principle of the invention is that the optical modulation technology is utilized, the detected signal is transmitted on the carrier light wave through the fiber core, after the modulation process is finished, the signal light carrying the detected parameter information is coupled to the optical detector through the receiving fiber, the optical signal is changed into the electric signal, and finally the measured signal is obtained through the processing of the signal analysis system.
When the laser device works, light with a certain wavelength is emitted by the laser device 1, enters the first coupler 2-2 through the isolator 2-1, the light entering the first coupler 2-2 is divided into two paths, one path enters a sensing section of a material forming area, and the other path is idle. The laser firstly enters an optical fiber refractive index sensor 6-1 to enable the laser to carry curing degree information, then the laser passes through a Bragg grating 6-2 to enable the laser to carry temperature information, the laser carrying the curing degree and the temperature information is reflected by the Bragg grating 6-2, then the laser enters a first coupler 2-2 to be divided into two paths, wherein one path is provided with an isolator 2-1 to intercept the laser, the other path of light is divided into two paths through a second coupler 2-3, the two divided paths are respectively connected with a grating demodulator 4 and a laser power meter 5, the deviation of the laser wavelength is read through the grating demodulator 4, and the power of the laser is read through the laser power meter 5. Finally, the curing degree and the temperature at any moment can be obtained through the conversion relation between the wavelength and the temperature and the conversion relation between the power and the curing degree. The isolator 2-1 plays a role in protecting the laser, and prevents laser light reflected by an original path from returning to the laser; the coupler plays a role of light splitting; the grating demodulator 4 reads the wavelength of the laser light, and the laser power meter 5 reads the power of the laser light. The optical fiber refractive index sensor 6-1 and the Bragg grating 6-2 adopt different modulation methods, the optical fiber refractive index sensor 6-1 adopts light intensity modulation, the Bragg grating 6-2 adopts wavelength modulation, and the two methods are not influenced by each other, so that the same light source can be adopted for monitoring.
1. The principle of Bragg grating optical fiber curing temperature measurement:
the reflection center wavelength of the fiber Bragg grating meets the Bragg condition, namely:
λ=2n eff Λ (1)
the reflection center wavelength lambda is dependent on the refractive index n as shown in formula (1) eff And the grid constant Λ. The external temperature and strain directly affect the refractive index and the grating constant of the fiber grating, so that the fiber grating responds to the change of the temperature and the strain. The effect of strain on the fiber grating is caused by the variation of the grating period and the elasto-optic effect, and the effect of temperature is caused by the thermal expansion effect and the thermo-optic effect.
The differential expression of the expression (1) represents the change of the central wavelength of the fiber grating when external physical quantity acts on the fiber grating.
Figure A20071007261400091
The basic principle of fiber grating sensing is as follows: when the temperature, strain or other physical quantity to be measured around the grating changes, the grating period lambada or the refractive index n of the fiber core is caused eff So as to shift the central wavelength of the fiber grating by delta lambda B By detecting the displacement of the grating wavelength, the physical quantity to be measured can be obtainedOf the cell. Writing equation (2) as follows:
Figure A20071007261400092
in the formula K ε Is the strain sensing sensitivity coefficient, K, of the grating T The temperature sensing sensitivity coefficient of the grating. It can be seen that the grating is responsive to both temperature and strain, i.e. temperature and strain cross-sensitivity. In many tests, the grating is only required to respond to one variable, so that the packaged Bragg grating is adopted to eliminate the temperature strain sensitivity of the grating and only measure the temperature.
2. Principle of measuring curing degree of polymer-based composite material molding process by optical fiber:
in the curing process of the composite material, resin generates a series of complex chemical reactions, and microscopically, the reactions are all processes that micromolecules are polymerized into macromolecules with a net-shaped structure through a cross-linking reaction. Each covalent bond in the polymer has a bond refractive index, and during curing of the composite matrix, the molecular bonds undergo recombination, resulting in a change in the refractive index of the material. Research on the change rule of the refractive index of the resin in the curing process finds that the refractive index of the resin is a function of the crosslinking density, and the refractive index of the resin is increased along with the deepening of the curing crosslinking reaction. In addition, variations in material density can also affect the refractive index. The change in density may reflect the transition from a fluid form to a crystalline form during the solidification of the polymer, i.e., the decrease in free space between molecular bonds, i.e., the change in viscosity, and thus may also reflect the solidification state. Therefore, information on the degree of curing of the resin can be obtained by tracking the change in the refractive index of the resin. The transmitted light in the optical fiber does not meet the total reflection condition of light at the sensing interface where the sensor is contacted with the measured resin, but has high enough reflectivity, and can provide a large enough optical power change range for refractive index measurement.

Claims (9)

1. The real-time synchronous monitoring device of the temperature curing degree in the forming process of the polymer matrix composite material consists of a laser (1), an optical transmission line component (2), an optical receiver (3), a sensing module (6) and a signal processing system (7); the optical transmission line component consists of an isolator (2-1), a first coupler (2-2) and a second coupler (2-3), and is characterized in that the output end of the laser (1) is connected with the input end of the isolator (2-1), the output end of the isolator (2-1) is connected with the first port (2-2-1) of the first coupler (2-2), the second port (2-2-2) of the first coupler (2-2) is connected with the port of the sensing module (6), the third port (2-2-3) of the first coupler (2-2) is connected with the first port (2-3-1) of the second coupler (2-3), the second port (2-3-2) and the third port (2-3-3) of the second coupler (2-3) are respectively connected with the two input ends of the optical receiver (3), and the two output ends of the optical receiver (3) are respectively connected with the two input ends of the signal processing system (7); the sensing module (6) consists of an optical fiber refractive index sensor (6-1) and a Bragg grating (6-2); the optical fiber refractive index sensor (6-1) and the Bragg grating (6-2) are connected in series, one end of the optical fiber refractive index sensor (6-1) is connected with the second port (2-2-2) of the first coupler (2-2), the other end of the optical fiber refractive index sensor (6-1) is connected with one end of the Bragg grating (6-2), and the sensing module (6) is embedded in the molding material (8) to be measured.
2. The device for monitoring the temperature solidification degree in the polymer matrix composite material forming process in real time synchronously according to claim 1, wherein the light receiver (3) is composed of a grating demodulator (4) and a laser power meter (5), the input end of the grating demodulator (4) and the input end of the laser power meter (5) are respectively connected with the second port (2-3-2) and the third port (2-3-3) of the second coupler (2-3), and the output end of the grating demodulator (4) and the output end of the laser power meter (5) are respectively connected with two data input ends of the signal processing system (7).
3. The device for synchronously monitoring the temperature curing degree in the polymer matrix composite molding process in real time according to claim 1, wherein the distance between the optical fiber refractive index sensor (6-1) and the Bragg grating (6-2) which are connected in series is 1-2 cm.
4. The device for synchronously monitoring the temperature curing degree in the polymer matrix composite molding process in real time according to claim 1, wherein the optical fiber refractive index sensor (6-1) is a sensing device which adopts an optical fiber coating layer and a cladding layer with the wavelength of 1550nm and the optical fiber stripped L length.
5. The device for monitoring the temperature curing degree in the polymer matrix composite molding process in real time synchronously according to claim 4, characterized in that the optical fiber stripping length L of the optical fiber refractive index sensor (6-1) is 10-20 mm.
6. The device for real-time synchronous monitoring of temperature solidification degree in polymer matrix composite material molding process according to claim 1, characterized in that the Bragg grating (6-2) is a Bragg grating packaged by a fast capillary.
7. The device for monitoring the temperature curing degree in the polymer matrix composite material molding process in real time synchronously according to claim 2, wherein interfaces are arranged among the laser (1), the isolator (2-1), the grating demodulator (4), the laser power meter (5), the signal processing system (7) and the sensing module (6), the interfaces are FC optical fiber connectors, and the interfaces at two ends of the first coupler (2-2) and the second coupler (2-3) are FC-FC optical fiber connectors.
8. The device for monitoring the temperature curing degree in the polymer matrix composite material forming process synchronously in real time according to claim 1, wherein the laser (1) emits laser light with the wavelength of 1550nm and the power of 20-30 mw.
9. The device for monitoring the temperature and the curing degree of the polymer matrix composite material in the forming process in real time synchronously according to the claim 1, characterized in that the signal processing system (7) adopts a computer data processing system.
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