CN115041825B - Tar strain sensing array applied to road health detection - Google Patents

Tar strain sensing array applied to road health detection Download PDF

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CN115041825B
CN115041825B CN202210626141.9A CN202210626141A CN115041825B CN 115041825 B CN115041825 B CN 115041825B CN 202210626141 A CN202210626141 A CN 202210626141A CN 115041825 B CN115041825 B CN 115041825B
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tar
film
laser
carbonized
sensing array
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CN115041825A (en
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臧浠凝
张曼
黄金财
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Tsinghua University
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Tsinghua University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/36—Removing material
    • B23K26/362—Laser etching
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/60—Preliminary treatment
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
    • G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge

Abstract

The invention discloses a tar oil sensor applied to road health detectionA variable sensing array and a method for manufacturing the same. Road health detection is an important means for immediately eliminating major accident potential by detecting road surface conditions on bridges or roads and vehicle passing conditions. By using tar, a by-product of petroleum production, produced by spraying equipment, a heating tank and CO 2 The roll-to-roll processing equipment formed by the laser cutting machine upgrades coal tar and ethylene tar into a functional carbon material with low resistance and sensitive response to tiny strain in an environment-friendly mode, and encapsulates the functional carbon material by utilizing a flexible material. The strain sensing array can respond to micro cracks and damages on a road and real-time electric signals through abnormal conditions of vehicles, such as overload and overspeed, and contributes to intelligent road construction.

Description

Tar strain sensing array applied to road health detection
Technical Field
The invention belongs to the technical field of tar treatment, and particularly relates to a preparation method of a tar-based film strain sensing array and application of the tar-based film strain sensing array to road health detection.
Background
Road health detection is an important ring of intelligent road construction, and the sensing array is used for immediately responding to damages, cracks and vehicles caused by influences of environmental erosion, material aging, fatigue and the like, converting the damages, cracks and vehicles into electrical signals, and timely early warning and eliminating accident potential. Meanwhile, coal tar and ethylene tar are used as byproducts in the production process of coke and ethylene, and annual yield is huge. The globalization carbon negative target needs to upgrade the polycyclic aromatic hydrocarbon into the functional carbon material, so as to improve the added value of the tar secondary chemical product. Therefore, the tar processing product is used for road health detection, which is beneficial to intelligent road construction and can realize secondary high-efficiency utilization of carbon materials.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the related art to some extent. Therefore, the invention aims to provide a tar-based film strain sensing array and a preparation method thereof, which take coal tar and ethylene tar as raw materials, and utilize roll-to-roll equipment to continuously process the tar-based film strain sensing array into a strain sensor, so that the tar-based film strain sensing array can be directly used for road health detection. The invention greatly improves the added value of tar products by a green production flow, and the prepared sensing array can produce sensitive response to micro strain and assist intelligent road construction.
In one aspect of the invention, a method of making a tar-based thin film strain sensing array is provided. According to an embodiment of the invention, the method comprises:
(1) Dispersing tar with organic solvent dichloromethane, spraying tar solution on quartz substrate to form uniform film;
(2) Carrying out sectional heating oxidation on the tar film to fully volatilize organic solvent molecules and small organic molecules;
(3) Designing an array pattern, and printing the pattern on the heated film by laser;
(4) Washing the area which is not carbonized by the laser by using an organic solvent, and naturally airing;
(5) The strain sensor is obtained by transferring the sensor array to ecoflex and encapsulating the array with such flexible material.
According to the method for preparing the tar-based strain sensing array, disclosed by the embodiment of the invention, coal tar and ethylene tar are mixed with organic solvent dichloromethane and sprayed on the surface of a quartz substrate at a certain speed, so that a uniform tar film is formed. And then carrying out sectional heating oxidation to fully volatilize the organic solvent molecules and the aromatic small organic molecules in the film. Further utilize CO 2 The laser processes the film by first pre-carbonizing at a lower power to avoid cracking of the film at high energy densities. And then the film is fully carbonized by high power, and the tar-based film sensing array is obtained according to the designed printing pattern, so that the tar-based film sensing array has good electrical property. For convenience in road detection, the film is subjected to substrate transfer. The processed film was first washed with NMP organic solvent to remove the non-carbonized areas. And (3) sticking conductive adhesive tapes on two sides of the film after natural air drying, reinforcing connection of contact parts by using conductive silver paste, coating the contact parts on the surface of the film by using ecoflex, cleaning by using absolute ethanol solution after air drying and molding, enabling the film to fall off from a quartz substrate, and continuously coating ecoflex packaging devices on the reverse side to obtain the tar-based strain sensing array. The roll-to-roll preparation process meets the green production requirement, and realizes the development of high-additional products of tar.
In addition, the method for preparing the tar-based strain sensing array according to the embodiment of the invention can also have the following additional technical features:
in some embodiments of the invention, in step (1), the tar solution has a concentration of 70wt% coal tar and a concentration of 50wt% ethylene tar.
In some embodiments of the present invention, in step (1), the spraying rate of the coal tar solution is 5mL/min, and the spraying rate of the ethylene tar solution is 10mL/min, and the surface of the quartz substrate after spraying has a flat transparent film.
In some embodiments of the present invention, in step (2), the staged heating process is specifically heating at 100 ℃ and 150 ℃ for 15min,200 ℃ for 1h,250 ℃ and 300 ℃ for 15min, respectively.
In some embodiments of the invention, in step (3), CO is used 2 And the laser prints the tar film subjected to oxidation treatment, the array is printed according to the designed pattern, and the interval of laser scanning lines of each area is 0.5mm.
In some embodiments of the invention, the laser machining process is divided into pre-carbonization and carbonization, and for coal tar films, the scanning speed is 25mm/s at 5W low power machining, and then 8.5W carbonization is performed, and the scanning speed is still 25mm/s. For ethylene tar films with higher aromatic content, 5W,25mm/s processing parameters were used for pre-carbonization, and then 8.5W,25mm/s laser carbonization was performed 6 times.
In some embodiments of the invention, in step (4), the patterned carbonized layer has a thickness of 20 to 30 μm.
In some embodiments of the invention, in step (4), the organic solvent NMP is used to remove non-carbonized areas of the tar film after laser carbonization in step (3).
In some embodiments of the invention, in step (4), conductive tapes are attached to both ends of the carbonized region, and conductive silver wires are connected according to test requirements, and conductive silver paste is used to connect between the tapes and the tar film.
In some embodiments of the present invention, in step (5), the vacuum defoamed ecoflex slurry is uniformly coated on the surface of the air-dried tar film, after the ecoflex is shaped, the film is washed by absolute ethyl alcohol to separate from the quartz substrate, and the reverse surface is encapsulated again by ecoflex coating.
In a second aspect of the invention, the invention provides a tar-based strain sensing array. According to the embodiment of the invention, the tar-based strain sensing array is prepared by adopting the method, can respond to micro strain by high-sensitivity electric signals, and can be used for detecting road health and assisting intelligent road construction.
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
FIG. 1 is a schematic flow diagram of a method of making a tar-based thin-film strain sensor roll-to-roll in accordance with an embodiment of the present invention;
FIG. 2 is a Raman image of the sprayed, oxidized and laser carbonized film of coal tar obtained in example 1;
FIG. 3 is a photograph of a coal tar-based strain sensor made in example 1;
FIG. 4 is a photograph of a tensile fixture of a coal tar-based strain sensor made in example 1;
FIG. 5 is a tensile test image of the coal tar-based strain sensor made in example 1;
FIG. 6 is a Raman image of the film of ethylene tar prepared in example 2 after spraying, oxidation and laser carbonization;
FIG. 7 is a tensile test image of the ethylene tar-based strain sensor made in example 2;
Detailed Description
The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not be construed as limiting the invention.
In a first aspect of the invention, a method of making a tar-based strain sensing array is provided. Referring to fig. 1, according to an embodiment of the present invention, the method includes:
1: mixing tar with organic solvent, spraying tar solution on quartz substrate
The tar solution can be prepared by dispersing tar with an organic solvent, methylene chloride. The inventors found that for coal tar with relatively high fluidity, a concentration of 70wt% is suitable. Too high a concentration can cause difficult dispersion of the solution, poor fluidity and difficult spraying; and the too low concentration can lead to too thin carbonization layer formed by subsequent laser processing, and the carbonization layer is extremely easy to break. Whereas for the more viscous ethylene tar, a concentration of 50wt% is preferred. Too high a concentration can lead to subsequent laser machining carbonization difficulties. Therefore, by adopting the tar concentration, the high-efficiency laser carbonization can be ensured, and the strain sensor with excellent electrical property can be obtained.
In this step, a uniform and light-transmitting tar film can be obtained by spraying a tar solution and an ethylene tar solution on a quartz substrate. For the coal tar solution with higher fluidity, the spraying rate was 5mL/min, while the ethylene tar dispersion was sprayed at 10 mL/min. The inventor observes that if the spraying rate is low, the tar dispersion is difficult to continuously spray out, and uneven films are caused; the high spray rates can cause solution build-up on the surface, which can negatively impact subsequent oxidation and laser processing.
2: heating and oxidizing the tar film
In the step, the coal tar film and the ethylene tar film are heated and oxidized in the air, so that organic solvent molecules and aromatic micromolecules are fully volatilized, and aromatic hydrocarbons in aliphatic hydrocarbon and Polycyclic Aromatic Hydrocarbon (PAHs) are crosslinked and bridged at the same time, thereby improving the connectivity and conductivity of the laser annealing tar and improving the laser processing performance of the laser annealing tar. The film was oxidized by stage heating, specifically, 15min at 100℃and 150℃respectively, 1h at 200℃and 15min at 250℃and 300℃respectively. The inventor finds that if the temperature of heating oxidation is too low, oxidation is insufficient, laser carbonization is difficult, and the electric conduction is still not realized after multiple laser treatments; if the temperature of heating oxidation is too high, the condensed ring aromatic molecules volatilize before bridging, so that the mass loss is increased, defect holes are generated after the thin film laser processing, the density is insufficient, and the electrical property is poor. Meanwhile, if the heating and oxidizing time is too short, the oxidation is insufficient, and the obtained oxidized tar film is uneven; if the time for the heating oxidation is too long, the generation of thermal cracks increases. Therefore, the oxidized tar film is uniform and compact and no thermal crack is generated by adopting the sectional heating oxidation condition.
3: laser processing of oxidized tar film
In this step, CO is used 2 The laser carries out laser processing on the oxidized tar film, and a sensing array is formed according to a designed printing pattern, so that the laser has good electrical property. The defocusing amount is-0.5 mm, and the filling line distance is 0.5mm. The inventor finds that the small filling line distance can cause overlarge carbonization degree of the film, the film is extremely easy to break in the substrate transferring process, and the line distance is overlarge and causes mismatching with the laser spot size, so that the film is difficult to effectively carbonize. The pre-carbonization is performed at a lower power to avoid cracking of the film at high energy density, and then the high power carbonized tar film is used. For the coal tar film, the coal tar film is processed at a low power of 5W, the scanning speed is 25mm/s, and then carbonized at 8.5W, and the scanning speed is still 25mm/s. For ethylene tar films with higher aromatic content, 5W,25mm/s processing parameters were used for pre-carbonization, and then 8.5W,25mm/s laser carbonization was performed 6 times. The inventors found that too low a scan rate resulted in excessive carbonization, increased thermal effects, increased film cracking and reduced processing efficiency, while too high a scan rate resulted in incomplete laser carbonization resulting in poor film electrical properties. In addition, too low carbonization power can result in poor electrical properties of the film, and too high carbonization power can exacerbate thermal effects and increase film cracking. The invention shapes the surface of the film by pre-carbonization, and then carries out carbonization treatment, thus obtaining the tar film with good electrical property and less cracks.
4: cleaning uncarbonized areas on tar films
In this step, the film is substrate transferred for convenience in road detection. The uncarbonated tar film was dissolved with an organic solvent NMP to form a pattern-printed sensor array. And the conductive adhesive tapes are stuck at the two ends of the film, and the silver paste is used for adhesion at the joint, so that the connection between the tar film and the conductive adhesive tapes is enhanced. According to some embodiments of the invention, the thickness of the patterned carbonized layer is 20-30 μm. The inventor finds that if the thickness of the carbonization layer is too small, carbonization defects greatly affect the electrical performance of the carbonization layer, carbon-carbon bonds and a layered structure are easily damaged in the transfer process, and the conductivity of the product is greatly reduced; if the thickness of the carbonization layer is too large, the carbonization mass distribution in the thickness direction is uneven, the comprehensive performance of the product is affected, the outer surface part of the carbonization layer is easy to fall off, and the surface morphology of the carbonization layer is damaged. Therefore, the carbonized layer has uniform mass distribution and good surface morphology, and the prepared product has high conductivity.
5: transferring a sensing array onto a flexible substrate ecoflex
In the step, the ecoflex slurry after vacuum defoamation is uniformly coated on the surface of an air-dried tar film, after the ecoflex is shaped, absolute ethyl alcohol is used for flushing the film to separate from a quartz substrate, and the reverse surface is coated and packaged by ecoflex again, so that the tar-based flexible strain sensing array can be obtained.
The invention utilizes roll-to-roll equipment, as shown in fig. 1, to realize the mass production of tar-based strain sensing arrays in a green efficient production manner. The strain sensor produced by the coal tar and the ethylene tar can respond to tiny strain, and can be applied to road health detection and power-assisted intelligent road construction.
The inventors found that by first mixing coal tar and ethylene tar with the organic solvent methylene chloride, spraying on a quartz substrate, a uniform tar film can be obtained. The film is subjected to sectional heating oxidation to fully volatilize organic solvent molecules and aromatic small molecules, and simultaneously crosslink and bridge aromatic hydrocarbons in aliphatic hydrocarbons and PAHs. And then laser processing is carried out on the tar film, and according to the designed array pattern, the tar film is carbonized by utilizing high-energy-density light beams, so that excellent electrical properties are obtained. And then removing uncorbonized tar by using an organic solvent NMP to obtain a strain sensing array, connecting conductive adhesive tapes at two ends and enhancing the contact strength of the connection part by using conductive silver paste. And finally, transferring and packaging the film by using an ecoflex material subjected to vacuum defoamation to obtain the tar-based strain sensing array. In summary, the method of the application is adopted to directly process coal tar and ethylene tar as raw materials into the film strain sensor with good electrical property in a green and efficient production mode by using roll-to-roll equipment, so that the added value of tar products is improved, and the prepared tar-based strain sensor array can respond to micro strain and has excellent sensing performance.
In a second aspect of the invention, the invention provides a tar-based strain sensing array that can be used for road health detection. According to the embodiment of the invention, the coal tar-based and ethylene tar-based thin film strain sensing array is prepared by adopting the method. The sensing array is used for immediately responding to damages, cracks and vehicles caused by influences of environmental erosion, material aging, fatigue and the like of a highway or a bridge through abnormal conditions (overweight and overspeed), converting the damages, cracks and vehicles into electrical signals, and can timely early warn, eliminate accident hidden trouble and assist intelligent road construction.
The scheme of the present invention will be explained below with reference to examples. It will be appreciated by those skilled in the art that the following examples are illustrative of the present invention and should not be construed as limiting the scope of the invention. The examples are not to be construed as limiting the specific techniques or conditions described in the literature in this field or as per the specifications of the product. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
Step 1: mixing coal tar with dichloromethane to obtain a coal tar solution (the concentration of the coal tar is 70 wt%);
step 2: spraying the coal tar solution on a quartz substrate to form a uniform tar film (spraying speed is 5 mL/min);
step 3: carrying out sectional heating oxidation (15 min at 100 ℃ and 150 ℃ respectively, 1h at 200 ℃ respectively, and 15min at 250 ℃ and 300 ℃ respectively) on the coal tar film;
step 4: by Synrad48-1 CO 2 Laser printing (0 mm defocus, 0.5mm filling line distance. First scanning: power 5W, scanning speed 25mm/s; second scanning: power 8.5W, scanning speed 25 mm/s.) on oxidized coal tar-based film by laser, fully carbonizing the printed area, and comparing the Raman spectra of the laser carbonized coal tar-based film with those of the original and oxidized films in FIG. 2;
step 5: removing an uncarbonated region on the coal tar film after laser processing by using an organic solvent NMP to obtain a carbonized layer (thickness-30 μm) with patterns;
step 6: the patterned carbonized layer was transferred onto ecoflex to yield a coal tar-based strain sensor (fig. 3). The coal tar-based strain sensing device is subjected to a tensile test, a tensile clamp is shown in fig. 4, a test result is shown in fig. 5, and the device has excellent sensing capability.
Example 2
Step 1: mixing ethylene tar with methylene dichloride to obtain a tar solution (ethylene tar concentration is 50 wt%);
step 2: spraying ethylene tar solution on a quartz substrate to form a uniform tar film (spraying speed is 10 mL/min);
step 3: carrying out sectional heating oxidation (15 min at 100deg.C and 150deg.C, 1h at 200deg.C, and 15min at 250deg.C and 300deg.C respectively) on ethylene tar film;
step 4: by Synrad48-1 CO 2 Laser printing (0 mm defocus, 0.5mm fill line distance, first scan: power 5W, scan speed 25mm/s; second to six scans: power 8.5W, scan speed 25 mm/s.) on oxidized ethylene tar film, fully carbonizing the printed area, FIG. 6 is a Raman spectrum comparison of the laser carbonized ethylene tar-based film with the original and oxidized films;
step 5: removing the non-carbonized region on the film after laser processing by using an organic solvent NMP to obtain a carbonized layer (thickness-30 μm) with patterns;
step 6: and transferring the carbonized layer with the pattern onto ecoflex to obtain the ethylene tar-based strain sensor. The coal tar-based strain sensing device is subjected to tensile test, the test result is shown in fig. 7, and the device has obvious electrical signal response to micro strain and can sensitively detect road health conditions.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.

Claims (6)

1. The preparation method of the tar strain sensing array for road health detection is characterized by comprising the following steps of:
(1) Dispersing tar with organic solvent dichloromethane, spraying tar solution on quartz substrate to form uniform film;
(2) Carrying out sectional heating oxidation on the tar film to fully volatilize organic solvent molecules and small organic molecules; the sectional heating process comprises heating at 100deg.C and 150deg.C for 15min, heating at 200deg.C for 1 hr, and heating at 250deg.C and 300deg.C for 15min respectively;
(3) Designing an array pattern, and printing the pattern on the heated film by laser; by CO 2 The laser performs laser printing on the tar film subjected to oxidation treatment according to the designA pattern printing array of the meter, wherein the interval of laser scanning lines of each area is 0.5mm;
(4) Washing out the area which is not carbonized by the laser by using an organic solvent, and naturally air-drying, wherein the thickness of the carbonized layer with the pattern is 20-30 mu m;
(5) The strain sensor is obtained by transferring the sensor array to ecoflex and encapsulating the array with such flexible material.
2. The method of claim 1, wherein in step (1), the tar solution has a concentration of 70wt% coal tar and a concentration of 50wt% ethylene tar; the spraying rate of the coal tar solution is 5mL/min, the spraying rate of the ethylene tar solution is 10mL/min, and a layer of smooth transparent tar film is arranged on the surface of the quartz substrate after spraying.
3. The method of claim 1, wherein in step (3), the tar film is pre-carbonized at a low laser power and then carbonized at a high power; for the coal tar film, firstly, processing with 5W low power, and then carbonizing with 8.5W at a scanning speed of 25mm/s, wherein the scanning speed is still 25mm/s; for ethylene tar films with higher aromatic content, 5W,25mm/s processing parameters were used for pre-carbonization, and then 8.5, W,25mm/s laser carbonization was performed 6 times.
4. The method according to claim 1, wherein in the step (4), an organic solvent N-methyl pyrrolidone (NMP) is used to remove the non-carbonized region of the tar film after laser carbonization in the step (3), conductive tapes are stuck to both ends of the carbonized region, conductive silver wires are connected according to test requirements, and conductive silver paste is used to connect the tape and the tar film.
5. The method of claim 1, wherein in step (5), the vacuum defoamed ecoflex slurry is uniformly coated on the surface of the air-dried tar film, after the ecoflex is shaped, the film is washed by absolute ethyl alcohol to be separated from the quartz substrate, and the reverse surface is coated and packaged by the ecoflex again.
6. A strain sensing array, characterized in that the material is prepared by the method of any one of claims 1-5.
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CN105413669B (en) * 2015-11-03 2018-08-24 同济大学 A kind of multifunctional graphite vinyl thin-film material and its manufacturing method and application
CN106925885B (en) * 2017-02-17 2018-08-10 中国船舶重工集团公司第七二五研究所 A kind of method that laser prepares different graphene pattern strain transducers
CN108864450B (en) * 2018-04-25 2020-11-24 齐鲁工业大学 Stress change sensing film and preparation method and application thereof
CN109099832B (en) * 2018-08-21 2020-07-03 华东理工大学 Strain sensor and method for manufacturing the same
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CN114309927B (en) * 2021-11-30 2022-11-08 清华大学 Coal tar-based thin film electronic device and preparation method thereof

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