CN112557336B - Method for measuring humidity of cable by using double-path infrared spectrum analysis method - Google Patents
Method for measuring humidity of cable by using double-path infrared spectrum analysis method Download PDFInfo
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- CN112557336B CN112557336B CN202011437230.6A CN202011437230A CN112557336B CN 112557336 B CN112557336 B CN 112557336B CN 202011437230 A CN202011437230 A CN 202011437230A CN 112557336 B CN112557336 B CN 112557336B
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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
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3554—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for determining moisture content
-
- 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
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- 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
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
- G01N2021/3572—Preparation of samples, e.g. salt matrices
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention relates to a method for measuring the internal humidity of a cable by a two-way infrared spectrum analysis method, which comprises the following steps: and irradiating the same position of the test material by adopting double paths of infrared light, testing the reflected light intensity, calculating the absorbance, and calculating the internal humidity of the cable according to a linear relation formula of an absorbance-humidity standard curve, wherein the test material is formed by coating a water absorption material on a hydrophobic base material. The invention adopts infrared light with double light paths to detect the humidity, has sensitive reaction, adopts high water absorption material to realize rapid water vapor balance, adopts optical cables to calculate the absorbance, is convenient and rapid, and is convenient for monitoring the water content condition in the cable in real time. The linear relation between the humidity and the absorbance established by the invention is excellent, the sensitivity is good, and when the graphene oxide is adopted as the water absorbing material, the corresponding sensitivity to the change of the humidity is 0.0065 percent‑1。
Description
Technical Field
The invention belongs to the technical field of humidity sensors, and particularly relates to a method for measuring the internal humidity of a cable by using a two-way infrared spectrum analysis method.
Background
China is a power country, and a cable is made of one or more mutually insulated conductors, an insulating layer and a protective layer, and is used for transmitting power or information from one place to a lead at another place. Typically an aerial cable or an underground cable. The cable has high requirements on water resistance and moisture resistance, and once the cable is wetted after water enters, water branch discharge is gradually formed under the action of a high-voltage electromagnetic field, so that the main insulation is damaged until breakdown discharge. Therefore, quality assurance of cable construction and laying is very important for the reliable operation of the cable in the future; the power cable has great water inlet harm, may cause serious short circuit and even fire, and brings serious loss and potential safety hazard to national economic construction. In the weather of over-temperature and high humidity in the south, or because the underground cable is buried underground, the moisture is heavy, the cable is stored for too long time, and the water vapor can permeate into the end of the cable due to improper storage; particularly, power cables and high-voltage cables for large-scale engineering in modern cities are laid underground mostly and need to pass through roads, bridges, culverts and the like frequently; due to weather or other reasons, a lot of water is often accumulated in the cable trench, and the situation that the cable head is immersed in the water for construction is inevitable in the laying process; the water inflow of the cable end is caused sometimes under natural disaster conditions, such as rainstorm, flood or the damage of the pipe needed by buried construction due to the water and human factors in the pipe; water enters the cable due to improper protection, untight bundling or damage of the cable head; in addition, the outer sheath and even the steel armor are scraped when the pipe is pulled and penetrated, and the phenomenon is particularly remarkable when mechanical pulling is used. The whole section of circuit is detected after the general outage of traditional operating mode, and can only detect the change of whole cable resistance and judge whether the cable intakes, can't accomplish real-time detection and moisture content numerical value to equipment cable joint. Meanwhile, the traditional resistance method cannot determine the water inlet position, and great difficulty is caused to cable maintenance construction.
CN210053192U discloses a flexible fireproof cable terminal with instruction function, which is characterized in that one side of the flexible fireproof cable terminal close to an exposed cable core is fixed to be connected with a transparent box body, and anhydrous copper sulfate powder serving as a water-absorbing color-changing drying agent is placed in the box body. CN105575523A discloses a moisture-proof cable, which is provided with a test paper which is stained with water and changes color. CN207165258U discloses a waterproof motor power line, which is internally provided with anhydrous copper sulfate particles which absorb water and change color, and the inside of the cable is observed through an external transparent external insulating sleeve layer to judge whether water enters the cable. However, the water-absorbing color-changing material adopting the test paper or the reagent has insufficient mechanical strength, is easy to take out for testing, or is damaged under the installation condition, and is inconvenient to install in the cable. And the indicator is greatly affected by the ambient heat and has low resolution. More importantly, inside simply putting into the cable with the test paper that discolours or the reagent that discolours, can take place to discolour promptly under lower humidity environment, the reagent has not reached the super standard value of the inside water content of cable this moment, and the cable detects or changes on the spot this moment, can lead to very big incremental cost. Therefore, simple will absorb water in the color-changing material directly places the cable, and the technology is troublesome, and is not enough to judging whether cable water content exceeds standard reliability, on this basis, need develop one kind can effectively test whether the cable intakes the material, and the comprehensiveness is excellent, and mechanical strength is up to standard, and it is convenient to make, the material of quick reaction.
The applicant's former patent CN202011001219.5 discloses a composite test material for testing whether a cable is flooded, a preparation method and an application thereof, which is a composite test material prepared by using water-absorbent resin, polyurethane acrylic resin, inorganic color-developing agent, plasticizer, filler and flame retardant as raw materials, and when in use, the material is observed to change color to judge whether the cable is flooded, but the method of the patent can only qualitatively analyze whether the cable is flooded, but cannot judge the specific condition of the internal humidity of the cable. CN202011002738.3 proposes a composite material whose transmittance changes with humidity, which can quantitatively pass through standard curves of transmittance and humidity, and the transmittance of the tested material can be calculated to obtain humidity. The linear relationship between transmittance and humidity is good over a wide range of humidity 25-70 RH%. However, the material reaction is not sensitive enough, and the light transmittance test is not sensitive enough due to the instrument precision, so that the humidity inside the cable cannot be accurately reflected.
Therefore, it is necessary to develop a method for measuring the humidity inside the cable, which can be rapidly balanced, has sensitive response and excellent linear relationship. The material based on the graphene oxide is a novel humidity sensor material and a method, and the graphene oxide is graphene with oxygen-containing functional groups, is a carbon film with special physical and chemical properties, and has strong hydrophilicity. Graphene oxide is placed in environments with different humidity, the number of adsorbed water molecules is different, the larger the humidity is, the more the adsorbed water molecules are, and due to the unique optical or electrical properties of the graphene oxide, the graphene oxide is often used for manufacturing sensors. At present, the graphene oxide composite material is used as a humidity sensor. The method has sensitive response and can ensure good linear relation in a wide humidity range. Generally, the material is a thin film formed by covering a layer of graphene oxide on the outer surface of an optical fiber, and the change of the properties of the graphene oxide under different humidity is used for expressing electrical signals, such as resistivity, refractive index of an optical waveguide, optical power and the like.
Research on graphene-based optical fiber humidity sensing (showa, journal of optics, stage 4 of 2015) discloses an optical fiber humidity sensor in which graphene oxide is deposited on a Side Polished Fiber (SPF). In the range of a high-humidity area, the change of the optical power and the humidity has good linear relation, and the response is sensitive and quick. This document is based on the random deposition of graphene film layers on the polished surface of SPF by alcoholic suspension of graphene oxide, by natural evaporation of alcohol, with film thickness from 200nm to 1000nm, with non-uniform dispersion, even if claimed to have a very good linear relationship, but must be performed for a fixed point of the material at each test. The linear relationship may be subject to large shifts if the position of the material under test is changed.
In the prior art, the humidity sensor is prepared by means of different properties exhibited by graphene oxide under different humidities. The optical fiber sensor obtained by taking the optical fiber as the base material adopts the principle based on the double-beam interference principle, the thickness of the graphene oxide is used as the cavity length, and based on the water absorption characteristic of the graphene, when the humidity in the environment changes, the graphene oxide material expands or contracts to change the cavity length of the sensor, so that the optical path changes, and the interference curve can deviate along with the humidity change of the environment. Due to the adoption of an interference method, the absorption deformation of the graphene oxide is uncontrollable, the precision requirement on graphene oxide processing equipment is very high, the dependence on the environment of the whole equipment is large, the problem that the data cannot be measured easily and the deviation is very large is solved. Therefore, the key point of the technology is how to prepare the graphene oxide material with a complete interference structure by a transfer method. The chemical vapor deposition method and the magnetron sputtering coating method can also be used, although the uniformity of the graphene oxide is good, the process is complex, the equipment is expensive, the cost is high, and the method has no industrial advantages and convenience when being used for industrial mass production. Moreover, the test using electrical signals is not applicable inside the cable, since the transmission of electrical signals always involves the use of metallic materials, which is not safe for the operation of the cable.
Therefore, it is highly desirable to develop a method for conveniently, accurately and rapidly testing the internal humidity of the cable.
Disclosure of Invention
In order to solve the problem that a method for testing the humidity in the cable in the prior art is not accurate enough or convenient enough, the invention provides a graphene oxide-based test material, which is used for establishing a humidity-absorbance standard curve by using the change of the material on the absorbance of infrared light so as to measure the water content in the cable.
The purpose of the invention is realized by the following technical scheme:
a method for measuring the internal humidity of a cable by a two-way infrared spectrum analysis method comprises the following steps: and irradiating the same position of the test material by adopting double paths of infrared light, testing the reflected light intensity, calculating the absorbance, and calculating the internal humidity of the cable according to a linear relation formula of an absorbance-humidity standard curve, wherein the test material is formed by coating a water absorption material on a hydrophobic base material.
The water absorption material can quickly absorb water vapor in air to achieve balance, and comprises but is not limited to polyvinyl alcohol (PVA), sodium polyacrylate (PAM-Na) and graphene oxide, wherein the graphene oxide is preferably adopted, and the graphene oxide has high water absorption amount and sensitive reaction and can reach water vapor balance in a short time. And the accuracy of detecting the humidity by the graphene oxide material is higher.
The hydrophobic substrate includes, but is not limited to, polytetrafluoroethylene, polyfluoroalkyl acrylate resin, polyimide resin.
The two-way infrared light is transmitted through an optical fiber, the distance between the optical fiber and the test material being 10-50mm, preferably 10-20 mm. The balance between the accuracy and precision of the detection can be guaranteed to the maximum extent at the distance. Preferably, Y-type optical fiber (optical fiber parameter: band 200-. The optical fiber is a Y-shaped optical fiber, and the transmitting optical fiber interface and the receiving optical fiber interface are arranged at an angle of 0-180 degrees, preferably 0-90 degrees, such as 0 degrees, 30 degrees, 45 degrees, 60 degrees and 90 degrees.
The two paths of infrared light are 1210-1490nm infrared light and 1890-2010nm infrared light which are alternately and respectively irradiated by the same light intensity.
Absorbance A of the invention according to the formula
Calculated, A is the absorbance of the material to infrared light, IIntoIs the intensity of incident light, IInverse directionIs the reflected light intensity.
Due to 1210 + 1490nm (I) of water1) Has no absorption to 1890-2010nm (I)2) Has strong absorption of infrared light. Thus, detection can be performed using two-way infrared light, according to the formula
Calculating the absorbance A, wherein I1 toIs the reflection light intensity of 1210-plus 1490nm infrared light, I2 reverseThe reflected light intensity of infrared light at 1890-2010 nm. Since water has substantially no absorption in infrared light of 1890-2010nm, I can be considered to be1 toAnd I1 intoThe difference between them is the loss in the optical path, such as the absorption of the optical path in air, in which case the infrared light of 1890-2010nm with the same intensity illuminates the same position of the material according to the same optical path, and the losses in the optical paths of I1 and I2 can be considered to be substantially the same due to the same optical path, therefore, I1 and I2 are considered to be substantially the same1 toIt can be considered as the light intensity of the incident infrared light of 1890-2010nm after loss through the optical path. The invention uses a circuit to control the delayer to alternatively irradiate 1210-1) And 1890-2010nm (I)2) The time delay is set to 0.1-0.5 s. Therefore, the invention utilizes the infrared light of double light paths, can conveniently, accurately and quickly obtain the absorbance of the material, and further calculates the environment humidity of the material. Compared with other humidity sensors, the method is faster and more accurate, avoids the problem of safety when monitoring the humidity in the cable according to the metal material used by resistivity and other testing methods.
The standard curve of humidity-absorbance of the present invention is obtained by a method comprising the steps of: in a constant temperature and humidity test box, the absorbance of the material to infrared light is tested under different humidity, and the absorbance is plotted against the humidity set in the constant temperature and humidity test box to obtain a curve with a linear relation and a linear relation formula. When the composite testing material is used, the absorbance of the material is calculated by testing the intensity of reflected light of infrared light, and the humidity of the environment where the composite testing material is located can be calculated according to the linear relation.
The method for coating the hydrophobic base material with the water-absorbing material comprises van der Waals adhesion, electrostatic self-assembly and chemical bonding.
The van der waals force adhesion method is to soak the hydrophobic material in the water absorbing material dispersion liquid, take out and dry to obtain the product. Preferably, the graphene oxide dispersion is a dispersion of graphene oxide dispersed in water, or a mixed solvent of water and a polar organic solvent, wherein the polar organic solvent comprises at least one of ethanol, DMF, THF, and DMSO. Preferably, the concentration of graphene oxide in the graphene oxide dispersion is 0.5-2 wt%, preferably 0.7-1.2 wt%.
When graphene oxide is used as the water absorbing material, the dispersion of graphene oxide is prepared by placing Ni-Fe-based graphene oxide in an etching solution (such as 50-60% FeCl of electronic grade)3Solution), graphene oxide has kept more complete shape and has floated on the surface like this, transfers graphene oxide to the deionized water and forms the dispersion, and then the dispersion of reuse hydrophobic material flooding in graphene oxide is taken out the drying and is obtained, because graphite oxide has kept more complete shape, it is more even at hydrophobic material surface adhesion ground, can promote the accuracy of detection.
The electrostatic self-assembly is characterized in that dispersion liquid of a graphene oxide-polyacrylic acid compound is used as an anion assembly, fluorine-containing polyacrylate copolymer resin is used as a cation assembly, the fluorine-containing polyacrylate copolymer resin is prepared from a fluorine-containing polyacrylate copolymer and an isocyanate curing agent, a monomer of the fluorine-containing polyacrylate copolymer comprises (methyl) tertiary amine acrylate, the fluorine-containing polyacrylate copolymer resin of the cation assembly is soaked in the dispersion liquid of the graphene oxide-polyacrylic acid compound, and the graphene oxide-polyacrylic acid compound is taken out and dried after being fully soaked.
In the coating method of electrostatic self-assembly, the invention has the following preferable technical scheme:
the graphene oxide-polyacrylic acid compound is prepared by the following preparation method: adding monomer (methyl) acrylic acid and isobornyl acrylate into the graphene oxide dispersion liquid, polymerizing in the presence of an initiator, adjusting the pH value of the polymer to 8-10 by using alkali liquor after the reaction is finished, and obtaining the graphene oxide-polyacrylic acid compound. Preferably, the graphene oxide accounts for 0.5 to 3%, preferably 1 to 2%, of the mass of the (meth) acrylic acid. Isobornyl acrylate is added in an amount of 10 to 15wt% based on the mass of (meth) acrylic acid.
The fluorine-containing polypropylene ester copolymer is prepared by copolymerizing the following monomers in parts by weight: 20-30 parts of alkyl (meth) acrylate, 12-18 parts of fluoroalkyl (meth) acrylate, 10-17 parts of tertiary amine (meth) acrylate and 5-10 parts of hydroxyalkyl (meth) acrylate. The mass ratio of the fluorine-containing polyacrylate copolymer to the isocyanate curing agent is 100: 7-12. For convenience of calculation, the mass of the fluorine-containing polyacrylate copolymer can be simply regarded as the sum of the masses of the monomers participating in the reaction, i.e., the sum of the masses of the alkyl (meth) acrylate, the fluoroalkyl (meth) acrylate, the tertiary amine (meth) acrylate and the hydroxyalkyl (meth) acrylate. The isocyanate curing agent is selected from at least one of Toluene Diisocyanate (TDI), isophorone diisocyanate (IPDI), diphenylmethane diisocyanate (MDI), dicyclohexylmethane diisocyanate (HMDI), Hexamethylene Diisocyanate (HDI) and Lysine Diisocyanate (LDI).
The conditions of the above-mentioned preparation method of the fluorine-containing polyacrylate copolymer are well known in the art, and the solvent is at least one selected from isopropanol, ethanol, chloroform, acetonitrile, cyclohexanone, cyclohexane and butyl acetate. The initiator is a conventional initiator for initiating polymerization by free radicals, such as at least one of benzoyl peroxide, azodiisobutyronitrile, potassium persulfate and sodium persulfate, and the amount of the initiator is 0.5-1 wt% of the total mass of the monomers.
In the alkyl (meth) acrylate, the alkyl group has 1 to 6 carbon atoms, such as methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, pentyl (meth) acrylate, hexyl (meth) acrylate; and/or the tertiary amine (meth) acrylate is selected from at least one of dimethylaminoethyl (meth) acrylate, dimethylaminopropyl (meth) acrylate, dimethylaminobutyl (meth) acrylate, diethylaminoethyl (meth) acrylate, diethylaminopropyl (meth) acrylate, diethylaminobutyl (meth) acrylate; and/or the fluoroalkyl (meth) acrylate has 2 to 10 carbon atoms in the fluoroalkyl group and 4 or more fluorine atoms, and is at least one of pentafluoroethyl (meth) acrylate, tetrafluoropropyl (meth) acrylate, hexafluorobutyl (meth) acrylate, heptafluorobutyl (meth) acrylate, nonafluorohexyl (meth) acrylate, dodecafluoroheptyl (meth) acrylate, and tridecafluoroctyl (meth) acrylate; the hydroxyalkyl (meth) acrylate is at least one selected from the group consisting of 2-hydroxyethyl acrylate, 3-hydroxypropyl acrylate, and 4-hydroxybutyl acrylate.
Further, the fluorine-containing polyacrylate copolymer resin is prepared by a preparation method comprising the following steps: like adding isocyanate curing agent and optionally other auxiliary agents into the dispersion liquid of the fluorine-containing polyacrylate copolymer, uniformly coating the dispersion liquid on the surface of a base material, and then curing at constant temperature of 60-80 ℃ to obtain the fluorine-containing polyacrylate copolymer. The other auxiliary agents are selected from at least one of wetting agents, leveling agents, defoamers, film formers, the type and amount of which are well known in the art. After curing, the fluorine-containing acrylate resin is uniformly coated on the surface of the base material, and the thickness is about 0.02mm to 0.05 mm.
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts infrared light with double light paths to detect the humidity, has sensitive reaction, adopts high water absorption materials to realize rapid water vapor balance, adopts optical cables to calculate the absorbance, is convenient and rapid, and is convenient for monitoring the water content condition in the cable in real time.
Secondly, the linear relationship between humidity and absorbance established by the invention is excellent, the sensitivity is good, and when the graphene oxide is adopted as the water absorbing material, the corresponding sensitivity to the change of the humidity is 0.0065 percent-1。
And thirdly, the method does not use a metal structure, and has no influence on the operation safety of the cable.
Drawings
FIG. 1 is a schematic view of an embedment of the invention. 10 is a main body, and 20 is an end cover.
FIG. 2 is a graph showing the relationship between the absorbance and the ambient humidity of the test material obtained in example 1.
FIG. 3 is a graph showing the relationship between the absorbance and the ambient humidity after the test material obtained in example 1 was left for one month.
FIG. 4 is a graph showing the relationship between the absorbance and the ambient humidity of the test material obtained in example 3.
FIG. 5 is a graph showing the relationship between the absorbance and the ambient humidity after the test material obtained in example 3 was left for one month.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the descriptions in the following. Unless otherwise specified, "parts" in the examples of the present invention are parts by weight unless otherwise specified, and% are mass percentages unless otherwise specified. All reagents used are commercially available in the art.
The graphene oxide is purchased from graphene oxide powder sold by Beijing Deke island gold science and technology Limited, the purity is more than 99 percent, and the oxygen content is 47.8 percent. The Ni-Fe-based graphene oxide is purchased from the combined fertilizer and crystal material technology company Limited.
Example 1
1) Putting a clean surface dish into deionized water, putting graphene oxide powder into the deionized water for dissolving, and dispersing for 2 hours by using ultrasonic waves to prepare a 2.5% graphene oxide dispersion liquid;
2) dipping the prepared graphene oxide dispersion liquid by a polytetrafluoroethylene end, vertically hanging the end downwards, and drying the end in a drying oven at 30 ℃ for about half an hour without wind;
3) inspecting the condition of graphene oxide attached to the surface of the matrix resin by using an electron microscope, wherein the matrix resin is qualified when being completely covered, and the operation can be repeated if the matrix resin is not completely covered;
example 2
1) Cutting the Ni-Fe substrate graphene oxide into squares of 2mm-3mm, taking a clean surface dish, and putting 60% FeCl of electronic grade3Putting the square into a corrosive liquid to float on the surface, accelerating corrosion, observing that a Ni-Fe base falls off after 3 hours of corrosion, transferring the graphene oxide into deionized water by using a silicon dioxide substrate, and soaking for more than 12 hours to obtain the graphene oxide material; the concentration of graphene oxide in deionized water was 2%.
2) Transferring the graphene oxide to the matrix resin end from the water by using the end of polytetrafluoroethylene, and placing the matrix resin end into a drying oven at 30 ℃ for drying for about half an hour without wind;
3) and (4) inspecting the condition that the graphene oxide is attached to the surface of the matrix resin by using an electron microscope, and determining that the matrix resin is qualified after being completely covered.
Example 3
1) Preparation of anion assembly: dispersing 85mg of graphene oxide in 50mL of mixed solvent of water and MDF according to the mass ratio of 1:2, uniformly mixing to obtain a dispersion liquid of the graphene oxide, adding 4.5g of methacrylic acid and 0.5g of isobornyl acrylate into the dispersion liquid, slowly dropwise adding 0.1g of 10% ethyl acetate solution of azodiisobutyronitrile in a nitrogen atmosphere, reacting for 4 hours at 60 ℃, after the reaction is finished, adjusting the pH to 9 by using 10% sodium bicarbonate, centrifuging for 3 times, adding deionized water each time, finally diluting with deionized water, and performing ultrasonic treatment to obtain a dispersion liquid of the graphene oxide-polyacrylic acid compound, wherein the concentration of the graphene oxide in the dispersion liquid is about 0.31 wt%.
2) Preparation of cation assembly: adding 10g of butyl acrylate, 7g of hexafluorobutyl acrylate, 6g of dimethylaminoethyl acrylate and 2.7g of 4-hydroxybutyl acrylate into 180mL of mixed solvent with the volume ratio of isopropanol to butyl acetate being 1:1, slowly dropwise adding 2.8g of 10% ethyl acetate solution of azodiisobutyronitrile under the heating condition, keeping the temperature at 60 ℃ for reacting for 6 hours, cooling to 30-40 ℃, and adding dilute hydrochloric acid to adjust the pH to 6.2 to obtain the fluorine-containing polyacrylate copolymer. And adding 2g of hexamethylene diisocyanate, uniformly mixing to obtain a coating liquid, uniformly spraying the coating liquid on a polytetrafluoroethylene sheet with the thickness of 2mm, and curing at the constant temperature of 60 ℃ for 8 hours to obtain the cation assembly.
3) And (3) soaking the cation assembly obtained by curing in the step 2) in the dispersion liquid of the anion assembly graphene oxide-polyacrylic acid compound in the step 1) for 0.5h, taking out the cation assembly after full soaking, and drying the cation assembly in a vacuum oven under the pressure of 0.1MPa at the temperature of 60 ℃ for 2h and taking out the cation assembly. Quickly placing in a drying box containing a drying agent calcium chloride for storage and later use.
Application example
FIG. 1 shows an embedded part 10 for testing the present invention, which is a main body, 20 is an end cap, the main body is provided with a window for water vapor exchange, one section of the main body is an optical fiber transmission port, the other end cap is provided with an end cap, and a test material is cut into a suitable shape and size and is adhered to the end cap.
The composite materials obtained in the above embodiments and comparative examples are cut into a cuboid with a size of 20mm × 8mm × 8mm, the cuboid is adhered to a cover made of a PC material by using a solid adhesive, the cover is covered at one end of an embedded part, the other end of the embedded part is provided with a hole capable of placing an optical fiber, the tail end of the hole is in a horn mouth shape, and the composite test material adhered to the cover faces the end of the hole. The embedded part is placed in a constant temperature and humidity box for operation, an 1210-plus 1490nm laser emitter (with power of 50mW) and a 1890-plus 2010nm laser emitter (with power of 50mW) are used for irradiating the material through a Y-shaped optical fiber during testing, the angle of incident light and reflected light is 0 degrees, namely the incident light and the reflected light are combined, the distance between the optical fiber and the tested material and the intensity of the reflected light of the tested material are tested, the absorbance of the material is calculated, and a linear relation graph and a formula are obtained by plotting the absorbance against the humidity and listed in table 1.
TABLE 1
Wherein the humidity-absorbance curve of the test material obtained in example 1 is shown in the figure2, in the linear formula, y is the absorbance and x is the humidity (RH%). It can be seen that the composite test material obtained in example 1 can be obtained by simply testing the intensity of the reflected light of the infrared light, i.e. the relative humidity and the linear correlation degree R of the environment where the test material is located can be calculated and obtained by a formula20.9841, the corresponding sensitivity to changes in humidity was 0.0031 (absorbance)%-1. Because the testing precision of the absorbance by the existing optical instrument can reach very high, the sensitivity of the absorbance to the change of the humidity in the invention can completely meet the aims of testing and monitoring the environment humidity. FIG. 3 is a graph showing the linear relationship of the test material obtained in example 1 after leaving for one month, and the linear correlation R is found2A drop 0.9558 indicates that the stability of this material is not good enough. The graphene oxide may be partially peeled off after being left for a long time, and may be caused by a change in irradiation position.
FIGS. 4 and 5 are absorbance-humidity curves of the test material obtained in example 3, initially and after one month of storage, respectively, and it can be seen that the composite test material obtained by the electrostatic self-assembly method reacts more sensitively, and the corresponding sensitivity to a change in humidity is 0.0065 (absorbance)%-1Degree of linear correlation R20.9962, the linear relationship is more excellent and the stability is better, and the linear relationship is not reduced basically after being placed for one month.
Claims (7)
1. A method for measuring the internal humidity of a cable by a two-way infrared spectrum analysis method comprises the following steps: irradiating the same position of a test material by adopting double paths of infrared light, testing the reflected light intensity, calculating the absorbance, and calculating the internal humidity of the cable according to a linear relation formula of a humidity-absorbance standard curve, wherein the test material is formed by coating a water absorption material on a hydrophobic base material;
the water absorbing material is a graphene oxide material; the hydrophobic base material comprises polytetrafluoroethylene, polyfluoroalkyl acrylate resin or polyimide resin; the method for coating the hydrophobic base material with the water absorbing material is electrostatic self-assembly;
the electrostatic self-assembly is characterized in that dispersion liquid of a graphene oxide-polyacrylic acid compound is used as an anion assembly, fluorine-containing polyacrylate copolymer resin is used as a cation assembly, the fluorine-containing polyacrylate copolymer resin is prepared from fluorine-containing polyacrylate copolymer and an isocyanate curing agent, and the mass ratio of the fluorine-containing polyacrylate copolymer to the isocyanate curing agent is 100: 7-12; the monomer of the fluorine-containing polyacrylate copolymer comprises (methyl) acrylic acid fluoroalkyl ester, (methyl) acrylic acid tertiary amine ester and (methyl) acrylic acid hydroxyalkyl ester, the fluorine-containing polyacrylate copolymer resin of a cation assembly is impregnated in dispersion liquid of a graphene oxide-polyacrylic acid compound, and the dispersion liquid is taken out and dried after being fully impregnated;
the two paths of infrared light are 1210-1490nm infrared light and 1890-2010nm infrared light which are alternately and respectively irradiated by the same light intensity;
the absorbance a is calculated according to the following formula:
2. The method of claim 1, wherein the two-way infrared light is transmitted through an optical fiber, the distance between the optical fiber and the test material being 10-50 mm; the optical fiber is Y-shaped optical fiber, and the transmitting optical fiber interface and the receiving optical fiber interface form an angle of 0-180 degrees.
3. The method of claim 2, wherein the distance between the optical fiber and the test material is 10-20mm, and the transmitting optical fiber interface is at an angle of 0 ° -90 ° to the receiving optical fiber interface.
4. The method of claim 1, wherein the standard humidity-absorbance curve is obtained by a method comprising the steps of: in a constant temperature and humidity test box, the absorbance of the material to infrared light is tested under different humidity, and the absorbance is plotted against the humidity set in the constant temperature and humidity test box to obtain a curve with a linear relation and a linear relation formula.
5. The method of claim 1, wherein the electrostatic self-assembly coating method comprises:
the graphene oxide-polyacrylic acid compound is prepared by the following preparation method: adding monomer (methyl) acrylic acid and isobornyl acrylate into the graphene oxide dispersion liquid, polymerizing in the presence of an initiator, adjusting the pH of the polymer to 8-10 by using alkali liquor after the reaction is finished, and obtaining a graphene oxide-polyacrylic acid compound;
the fluorine-containing polypropylene ester copolymer is prepared by copolymerizing the following monomers in parts by weight: 20-30 parts of alkyl (meth) acrylate, 12-18 parts of fluoroalkyl (meth) acrylate, 10-17 parts of tertiary amine (meth) acrylate and 5-10 parts of hydroxyalkyl (meth) acrylate.
6. The method according to claim 5, wherein the graphene oxide accounts for 0.5 to 3% by mass of the (meth) acrylic acid, and the isobornyl acrylate is added in an amount of 10 to 15wt% by mass of the (meth) acrylic acid.
7. The method according to claim 6, wherein graphene oxide accounts for 1-2% by mass of the (meth) acrylic acid.
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| JP2017161424A (en) * | 2016-03-10 | 2017-09-14 | パナソニックＩｐマネジメント株式会社 | Optical component sensor |
| CN107024453A (en) * | 2017-05-26 | 2017-08-08 | 北京碳世纪科技有限公司 | A kind of quick humidity method for sensing based on graphene/graphene oxide laminated film |
| CN207036687U (en) * | 2017-05-26 | 2018-02-23 | 北京碳世纪科技有限公司 | A kind of humidity sensor based on graphene/graphene oxide laminated film |
| CN211347927U (en) * | 2019-12-06 | 2020-08-25 | 常州京洋半导体材料科技有限公司 | Optical fiber LMR humidity sensor and sensing system |
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