CN113075165B - U-shaped humidity-sensitive optical fiber sensor and manufacturing method thereof - Google Patents
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Abstract
The invention discloses a manufacturing method and a manufacturing method of a U-shaped humidity-sensitive optical fiber sensor; a manufacturing method of a U-shaped humidity-sensitive optical fiber sensor is characterized by comprising the following steps: the method comprises the following steps: step A, fiber grating pretreatment: firstly, removing a protective layer of the middle section of one section of optical fiber, then grinding the middle section of the optical fiber to 200-91500 mu m, and bending the ground optical fiber into a U shape; step B, preparing the U-shaped optical fiber with the sensitization film: b1, firstly dissolving a light guide material polysulfone in a dimethyl sulfoxide solution, adding germanium dioxide into the solution, and uniformly stirring to obtain polysulfone germanium dioxide sol; step C, preparing a humidity-sensitive optical fiber sensor; the U-shaped humidity-sensitive optical fiber sensor with the humidity-sensitive film and the sensitivity enhancing film prepared by the invention can be widely applied to the fields of energy, chemical engineering, biochemical detection and the like.
Description
Technical Field
The invention relates to a hydrogen sensor, in particular to a U-shaped humidity-sensitive optical fiber sensor and a manufacturing method thereof.
Background
Humidity is an important parameter affecting the safe operation of an electrical control cabinet, a communication machine room and the like. In order to maintain the humidity of the power distribution room within the normal allowable relative humidity working range of the device (the maximum allowable relative humidity 75% RH), improve the service life of the device and ensure the safe operation of the device, the humidity in the power distribution room must be monitored in real time.
At present, a plurality of sensors for measuring humidity are used, wherein the optical fiber sensor has the advantages of electromagnetic interference resistance, chemical corrosion resistance, long-distance transmission, high response speed, high sensitivity and the like, and is widely applied. In the optical fiber humidity sensor, compared with a quartz optical fiber humidity sensor, the plastic optical fiber humidity sensor has the advantages of low price, large diameter, large numerical aperture, good flexibility, easiness in shaping and the like. Despite the advantages of the plastic optical fiber humidity sensor, the reported plastic optical fiber humidity sensor faces a critical problem: the sensitivity is low.
In order to improve the sensitivity of the optical fiber humidity sensor, plastic optical fiber humidity sensors with different structural types, such as U-shaped, D-shaped and tapered optical fiber sensors, are developed. Although the sensitivity can be improved by optimizing the shape of the sensitive area of the sensor, the optical fiber humidity sensors still select communication plastic optical fibers as the light transmission and sensing media. The optical transmission in the communication plastic optical fiber is based on a fiber core-cladding film, light beams are mainly limited to be transmitted in the optical fiber, the light radiation intensity on the surface of the optical fiber is low, the action intensity of light and measured parameters is low, and the sensitivity of the sensor is low. Therefore, it is necessary to construct a new optical fiber for enhancing the light radiation intensity on the surface of the optical fiber, and to couple with the selective humidity sensitive material, so as to improve the plastic optical fiber humidity sensor.
Disclosure of Invention
The invention aims to solve the technical problem of providing a U-shaped humidity-sensitive optical fiber sensor and a manufacturing method thereof.
The technical scheme of the invention is as follows: a manufacturing method of a U-shaped humidity-sensitive optical fiber sensor is characterized by comprising the following steps: the method comprises the following steps:
step A, fiber grating pretreatment: the protective layer of the middle section of one section of optical fiber is removed, then the middle section of the optical fiber is ground to 200-91500 μm, and the ground optical fiber is bent into a U shape.
Step B, preparing the U-shaped optical fiber with the sensitization film:
and step B1, firstly dissolving the light guide material polysulfone in a dimethyl sulfoxide solution, adding germanium dioxide into the solution, wherein the germanium dioxide plays a role in light scattering and refractive index modulation, and stirring uniformly to obtain the polysulfone germanium dioxide sol.
And B2, dissolving the tackifier Canadian resin in xylene to obtain Canadian resin sol.
And step B3, mixing the polysulfone germanium dioxide sol with the Canadian resin sol to obtain the sensitization sol.
B4, coating the sensitization sol on the surface of the U-shaped area of the optical fiber, drying the sensitization sol in a vacuum drying oven, and forming a sensitization membrane after the sensitization sol is dried to obtain the U-shaped optical fiber with the sensitization membrane, wherein the sensitization membrane is formed by mixing polysulfone, canadian resin and germanium dioxide; the refractive index of the obtained sensitization film is larger than that of the fiber core of the optical fiber, and light which is transmitted in the optical fiber and is scattered on the surface of the fiber core of the optical fiber can be coupled into the sensitization film so as to improve the light intensity transmitted in the sensitization film; while germanium dioxide GeO 2 Will scatter light and increase the surface radiation of the sensitization filmThe emitted light intensity to further provide the sensitivity of the sensor.
Step C, preparation of humidity-sensitive optical fiber sensor
Step C1, adding the N-methylpyrrolidone solution into a container, continuously stirring under the protection of nitrogen, adding 4,4 '-diaminodiphenyl ether powder, adding pyromellitic dianhydride particles after the 4,4' -diaminodiphenyl ether powder is completely dissolved, and reacting for a certain time to obtain a polyamic acid solution; n-methylpyrrolidone is a solvent of 4,4' -diaminodiphenyl ether powder; 4,4' -diaminodiphenyl ether powder is an intermediate for synthesizing polyimide; pyromellitic dianhydride particles are used as raw materials for synthesizing polyimide; the pyridine solution is used for improving the thermal stability, mechanical property and processing property of the polyimide material; the propionic anhydride solution is used as a water removal agent to promote the low-temperature imidization of the polyamic acid; n-butanol is a solvent of polyether copolyamide PEBA 2533; the polyether copolyamide PEBA2533 is used for improving the water absorption performance of the polyimide film and the toughness and the elongation at break after water absorption.
Step C2, standing the prepared polyamic acid solution, adding a pyridine solution into the polyamic acid solution after bubbles in the solution disappear, and mutually dissolving under magnetic stirring; wherein the pyridine solution is used for improving the thermal stability, the mechanical property and the processing property of the polyimide material.
Step C3, adding a propionic anhydride solution into the mixed solution obtained in the step C2, and continuously reacting under the stirring condition to obtain polyimide humidity sensitive sol; the propionic anhydride solution is used as a water remover to promote the low-temperature imidization of the polyamic acid.
Step C4, adding the polyether copolyamide into n-butanol, and continuously stirring by using a magnetic stirrer to obtain polyether copolyamide and n-butanol sol; the polyether copolyamide PEBA2533 is used for improving the water absorption performance of the polyimide film and the toughness and the elongation at break after water absorption.
Step C5, mixing the sol obtained in the step C3 and the step C4 with silicon dioxide to obtain humidity sensitive sol; the silicon dioxide is used for enhancing the transmission of light beams in the humidity-sensitive sol and enhancing the mechanical property of the humidity-sensitive sol.
And C6, coating the surface of the U-shaped area of the U-shaped optical fiber with the sensitization film obtained in the step B4 with the humidity sensitive sol obtained in the step C5, drying in a vacuum drying oven, and forming the humidity sensitive film after drying the humidity sensitive sol to obtain the U-shaped humidity sensitive optical fiber sensor with the humidity sensitive film and the sensitization film. At the interface of the humidity-sensitive film and the sensitivity-sensitive film, light radiated from the surface of the sensitivity-sensitive film is coupled into the humidity-sensitive film, after the humidity-sensitive film absorbs water molecules, the refractive index changes, the more water molecules are absorbed, the larger the refractive index change is, the stronger the light attenuation in the humidity-sensitive film is, finally, the smaller the light intensity output from the optical fiber is, and the measurement of the humidity is realized by detecting the change of the light intensity at the output end of the optical fiber.
The invention aims to improve the luminous intensity of the surface of the optical fiber, thereby improving the response sensitivity of the sensor to relative humidity; firstly removing a partial coating of an optical fiber and bending the optical fiber into a U shape, then coating a layer of polysulfone germanium dioxide sol on the surface of the U-shaped area, and finally coating a layer of selective humidity-sensitive material, namely a humidity-sensitive film, on the surface of the sensitization film, thereby constructing the high-sensitivity humidity-sensitive optical fiber sensor.
In the humidity sensitive film, polyimide is used for selectively absorbing water molecules to realize selective sensitivity in air, polyether copolyamide PEBA2533 can improve the water absorption performance, the toughness and the elongation at break after water absorption of the polyimide film, the service life of the polyimide film is prolonged, silicon dioxide enhances the transmission of light beams in the humidity sensitive sol and enhances the mechanical property of the humidity sensitive sol, the ground optical fiber has a rough surface, the light intensity in the humidity sensitive film can be increased by adopting a U-shaped structure and a sensitivity enhancing film, the higher the light intensity in the humidity sensitive film is, the more the light attenuation is, and the higher the sensitivity of the sensor is. Therefore, the plastic optical fiber humidity sensor has high sensitivity.
According to the preferable scheme of the manufacturing method of the U-shaped humidity-sensitive optical fiber sensor, germanium dioxide GeO is adopted in the step B1 2 The mass of the polysulfone germanium dioxide sol is 0.5-5 percent of the total mass of the polysulfone germanium dioxide sol.
According to the preferable scheme of the manufacturing method of the U-shaped humidity-sensitive optical fiber sensor, in the step C5, the sol obtained in the steps C3 and C4 is mixed with the silicon dioxide according to the mass ratio of (95-98) to (5-2) to (0.5-10).
According to the preferable scheme of the manufacturing method of the U-shaped humidity-sensitive optical fiber sensor, in the step C1, the mass ratio of N-methylpyrrolidone to 4,4' -diaminodiphenyl ether powder to pyromellitic dianhydride is (40-45) to (1-2).
The U-shaped humidity-sensitive optical fiber sensor is prepared by the manufacturing method of the U-shaped humidity-sensitive optical fiber sensor.
The U-shaped moisture-sensitive optical fiber sensor with the moisture-sensitive film and the sensitization film and the manufacturing method have the advantages that the refraction index of the sensitization film is larger than that of an optical fiber core, light which is transmitted in an optical fiber in a low-order mode and scattered on the surface of the optical fiber core can be coupled into the sensitization film, and light intensity transmitted in the sensitization film is improved; the light radiated on the surface of the sensitivity enhancing film is coupled into the humidity sensitive film, after the humidity sensitive film absorbs water molecules, the refractive index changes, the more water molecules are absorbed, the larger the refractive index variation is, the stronger the light attenuation in the humidity sensitive film is, and finally, the smaller the light intensity output from the optical fiber is, so that the humidity measurement is realized by detecting the light intensity change at the output end of the optical fiber; the invention has the characteristics of high response sensitivity to the relative humidity change in the environment and simple method, and can be widely applied to the fields of energy, chemical engineering, biochemical detection and the like.
Drawings
FIG. 1 is a schematic structural diagram of a U-shaped moisture-sensitive optical fiber sensor according to the present invention.
FIG. 2 is a response curve of the U-shaped moisture-sensitive optical fiber sensor obtained in example 3 with respect to humidity.
Detailed Description
Example 1, referring to fig. 1, a method for manufacturing a U-shaped moisture-sensitive optical fiber sensor, the method comprising the steps of:
step A, fiber grating pretreatment: taking a section of optical fiber, wherein the optical fiber is provided with an optical fiber core 3, an optical fiber cladding 2 and a protective layer 1; firstly, removing the protective layer at the middle section of the optical fiber, and then grinding the middle section of the optical fiber to 200-91500 mu m by using optical fiber grinding paper with the grain diameter of 3-5 mu m to obtain a fiber core with a rough surface; and bending the ground optical fiber into a U shape, putting the optical fiber into an oil bath pan with the temperature of 110-150 ℃, heating for 2-3min, taking out, cooling to normal temperature, and shaping to obtain the U-shaped optical fiber 6 with a fixed shape.
Step B, preparing the U-shaped optical fiber with the sensitization film:
and step B1, firstly dissolving a light guide material polysulfone in a dimethyl sulfoxide solution, wherein the mass ratio of the polysulfone to the dimethyl sulfoxide solution is 1 2 Sol; geO 2 The mass accounts for 0.5-5% of the total mass of the sol.
And B2, dissolving the tackifier Canadian resin in xylene, wherein the mass ratio of the Canadian resin to the xylene is 1.
Step B3, polysulfone GeO 2 The sol and the Canadian resin sol are mixed according to the mass ratio of 9.
Step B4, coating the sensitization sol on the surface of the U-shaped area of the plastic optical fiber, drying for 10-20h at 50-90 ℃ in a vacuum drying oven, and drying the sensitization sol to form a sensitization membrane 5 to obtain the U-shaped optical fiber with the sensitization membrane with the thickness of 2-2000 mu m, wherein the sensitization membrane is made of polysulfone, canadian resin and GeO 2 Mixing to form; the refractive index of the sensitization film is larger than that of the fiber core of the optical fiber, so that the light which is transmitted in the optical fiber in a low-order mode and scattered on the surface of the fiber core of the optical fiber can be coupled into the sensitization film, and the light intensity transmitted in the sensitization film is improved; with GeO 2 The light will be scattered and the intensity of the radiation on the surface of the sensitization film will be increased to further provide the sensitivity of the sensor.
Step C, preparation of humidity-sensitive optical fiber sensor
Step C1, adding a certain mass of N-methylpyrrolidone solution into a container, continuously stirring for 30-60min at the rotating speed of 60-100rpm/min under the protection of nitrogen, then adding 4,4 '-diaminodiphenyl ether powder, adding pyromellitic dianhydride particles after the 4,4' -diaminodiphenyl ether powder is completely dissolved, and reacting for 6-8h to obtain a transparent light yellow polyamic acid PAA solution; the mass ratio of N-methylpyrrolidone, 4' -diaminodiphenyl ether powder and pyromellitic dianhydride is (40-45) to (1-2), and specifically 40.
And C2, standing the prepared polyamic acid PAA solution for 30-60min, adding a pyridine solution into the polyamic acid PAA solution after bubbles in the solution disappear, wherein the mass ratio of the pyridine solution to the PAA solution is 5, and mutually dissolving under magnetic stirring.
And C3, adding a propionic anhydride solution into the mixed solution obtained in the step C2, wherein the mass ratio of the propionic anhydride to the pyridine solution to the PAA solution is 1.5.
And C4, adding polyether copolyamide PEBA2533 into the n-butanol, wherein the mass ratio of the polyether copolyamide PEBA2533 to the n-butanol is 1.
And step C5, mixing the sol obtained in the step C3 and the step C4 with silicon dioxide with the diameter of 5nm-1000nm according to the mass ratio of (95-98) to (5-2) to (0.5-10) to obtain the humidity sensitive sol. The mass ratio of the three components is selected from 95.
And C6, coating the moisture-sensitive sol obtained in the step C5 on the surface of the U-shaped area of the sensitization film U-shaped optical fiber obtained in the step B4, drying for 20-30h in a vacuum drying oven at the temperature of 40-80 ℃, and forming a moisture-sensitive film 4 with the thickness of 20nm-1000 mu m after the moisture-sensitive sol is dried, so as to obtain the U-shaped moisture-sensitive optical fiber sensor with the moisture-sensitive film and the sensitization film. At the interface of the humidity sensitive film and the sensitivity enhancing film, light radiated from the surface of the sensitivity enhancing film is coupled into the humidity sensitive film, after the humidity sensitive film absorbs water molecules, the refractive index changes, the more the water molecules are absorbed, the larger the refractive index change is, the stronger the light attenuation in the humidity sensitive film is, and finally the smaller the light intensity output from the optical fiber is, so that the measurement of the humidity is realized by detecting the light intensity change of the output end of the optical fiber.
Example 3, in contrast to example 1:
in the step A, the length of the middle section of the optical fiber is 5cm, the middle section is ground to 900 micrometers, and the bending radius of the U area is 2cm.
The thickness of the sensitization film formed in step B4 is 200 μm, and the thickness of the humidity-sensitive film F formed in step C5 is 20 μm.
The U-shaped humidity-sensitive optical fiber sensor obtained in example 3 was subjected to a humidity response test at 40 ℃ to obtain a humidity response characteristic as shown in FIG. 2, wherein in FIG. 2, the sensor output light intensity I out And relative humidity (x) has a linear relationship: I.C. A out ＝-0.9165x+554.05。
(R 2 0.9817), x in the range of 10-80% RH, sensitivity of-0.9 nW/(1% RH), 6.9 times of the 1500 μm optical fiber surface coated with 10 μm moisture-sensitive film due to rough optical fiber surface, U-shaped structure of optical fiber, high refractive index of sensitizing film, geO 2 The light scattering and the water swelling property of polyimide cause the refractive index change, the polyether copolyamide PEBA2533 enhances the water absorption of the moisture-sensitive film, and the silicon dioxide enhances the greater light attenuation caused by the transmission of light on the moisture-sensitive film, so the comprehensive effects enhance the light intensity and the light attenuation in the moisture-sensitive film, and further improve the sensitivity of the sensor.
Thus, the rough surface of the optical fiber increases the scattering of light on the surface of the fiber core of the optical fiber, and polysulfone and GeO 2 The refractive index of the coating sensitization film is higher than that of the fiber core of the optical fiber, and the sensitization film with proper thickness is helpful for coupling the low-order mode transmitted in the fiber core into polysulfone and GeO 2 A coating layer to increase light intensity into the humidity sensitive membrane; finally, the appropriate humidity sensitive film thickness is beneficial to enhancing the light attenuation and improving the sensitivity of the sensor; when the fiber core diameter was 900 μm, the sensitivity enhancing film thickness was 200 μm, and the humidity sensitive film thickness was 20 μm, the sensitivity of the sensor reached-0.9 nW/(1% RH).
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (5)
1. A manufacturing method of a U-shaped humidity-sensitive optical fiber sensor is characterized by comprising the following steps: the method comprises the following steps:
step A, fiber grating pretreatment: firstly, removing a protective layer at the middle section of a section of optical fiber, then grinding the middle section of the optical fiber, and bending the ground optical fiber into a U shape;
step B, preparing the U-shaped optical fiber with the sensitization film:
b1, firstly dissolving a light guide material polysulfone in a dimethyl sulfoxide solution, adding germanium dioxide into the solution, and uniformly stirring to obtain polysulfone germanium dioxide sol;
b2, dissolving the tackifier Canadian resin in xylene to obtain Canadian resin sol;
step B3, mixing the polysulfone germanium dioxide sol with the Canadian resin sol to obtain a sensitization sol;
b4, coating the sensitization sol on the surface of the U-shaped area of the optical fiber, drying the sensitization sol in a vacuum drying oven, and forming a sensitization membrane after drying the sensitization sol to obtain the U-shaped optical fiber with the sensitization membrane, wherein the sensitization membrane is formed by mixing polysulfone, canadian resin and germanium dioxide; the refractive index of the obtained sensitization film is larger than that of the fiber core of the optical fiber, and light which is transmitted in the optical fiber and is scattered on the surface of the fiber core of the optical fiber can be coupled into the sensitization film so as to improve the light intensity transmitted in the sensitization film; meanwhile, the germanium dioxide can scatter light, and the radiation intensity of the surface of the sensitization film is increased, so that the sensitivity of the sensor is further improved;
step C, preparation of humidity-sensitive optical fiber sensor
Step C1, adding an N-methylpyrrolidone solution into a container, continuously stirring under the protection of nitrogen, adding 4,4 '-diaminodiphenyl ether powder, adding pyromellitic dianhydride particles after the 4,4' -diaminodiphenyl ether powder is completely dissolved, and reacting for a certain time to obtain a polyamic acid solution;
step C2, standing the prepared polyamic acid solution, adding a pyridine solution into the polyamic acid solution after bubbles in the solution disappear, and mutually dissolving the pyridine solution and the polyamic acid solution under magnetic stirring;
step C3, adding a propionic anhydride solution into the mixed solution obtained in the step C2, and continuously reacting under the stirring condition to obtain polyimide humidity sensitive sol;
step C4, adding the polyether copolyamide into n-butanol, and continuously stirring by using a magnetic stirrer to obtain polyether copolyamide and n-butanol sol;
step C5, mixing the sol obtained in the step C3 and the step C4 with silicon dioxide to obtain humidity sensitive sol;
and C6, coating the surface of the U-shaped area of the U-shaped optical fiber with the sensitization film obtained in the step B4 with the humidity sensitive sol obtained in the step C5, drying in a vacuum drying oven, and forming the humidity sensitive film after drying the humidity sensitive sol to obtain the U-shaped humidity sensitive optical fiber sensor with the humidity sensitive film and the sensitization film.
2. The method for manufacturing a U-shaped moisture-sensitive optical fiber sensor according to claim 1, wherein: in the step B1, the mass of the germanium dioxide accounts for 0.5-5% of the total mass of the polysulfone germanium dioxide sol.
3. The method for manufacturing a U-shaped moisture-sensitive optical fiber sensor according to claim 1, wherein: in the step C5, the sol obtained in the step C3 and the step C4 is mixed with the silicon dioxide according to the mass ratio of (95-98) to (5-2) to (0.5-10).
4. The method for manufacturing a U-shaped moisture-sensitive optical fiber sensor according to claim 1, wherein: in the step C1, the mass ratio of the N-methyl pyrrolidone, the 4,4' -diaminodiphenyl ether powder and the pyromellitic dianhydride is (40-45) to (1-2).
5. The U-shaped moisture-sensitive optical fiber sensor prepared by the method for manufacturing the U-shaped moisture-sensitive optical fiber sensor according to claim 1, 2, 3 or 4.
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