CN110487438B - Preparation method of sandwich-shaped flexible temperature sensor - Google Patents
Preparation method of sandwich-shaped flexible temperature sensor Download PDFInfo
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- CN110487438B CN110487438B CN201910780146.5A CN201910780146A CN110487438B CN 110487438 B CN110487438 B CN 110487438B CN 201910780146 A CN201910780146 A CN 201910780146A CN 110487438 B CN110487438 B CN 110487438B
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Abstract
The invention discloses a preparation method of a sandwich-shaped flexible temperature sensor, which is characterized in that a conducting layer is separately prepared by graphene dispersion liquid, and the conducting layer is embedded between an upper substrate and a lower substrate which are prepared by PDMS materials, so that the van der Waals force among graphene particles is reduced, the electrostatic repulsion between particle surfaces is increased, the distance between graphene sheet layers is increased, and further the agglomeration effect is weakened, so that the resistance temperature change rate of the flexible sensor is increased, and the sensitivity of the flexible sensor to temperature change is improved.
Description
Technical Field
The invention relates to the technical field of temperature sensor manufacturing, in particular to a manufacturing method of a sandwich-shaped flexible temperature sensor.
Background
The flexible temperature sensor is more and more widely applied in the fields of daily life, medical treatment and health and the like, such as detection of health indexes, prevention of postoperative complications and the like. Due to excellent mechanical property, thermal property and ultrahigh electron mobility, graphene is widely used for research of flexible sensor materials. In the prior art, when a flexible sensor is prepared by using graphene, a method of doping graphene into an elastomer PDMS matrix and combining the excellent characteristics of graphene with the flexibility and ductility of the elastomer PDMS matrix is generally selected to prepare a high-sensitivity temperature sensor on a flexible template, and for example, in an invention patent with patent publication No. CN109916527A, a technical scheme of doping graphene into a Poly-dimethyl siloxane (PDMS) material to form a high-sensitivity temperature flexible sensor is disclosed.
However, the above-mentioned technical solutions have a certain technical problem that, since the thickness of the multilayer graphene is only a few nanometers, the distance between the nanoparticles is very small, and on the other hand, the van der waals force and the electrostatic attraction between the particles are very large, which means that the nanoparticles are constantly attracted to each other, and the distance between the particles is further reduced, thereby forming a nano-sized particle. Due to the clustering phenomenon (agglomeration), graphene layers cannot be separated from each other and cannot be interwoven with other components, so that the graphene cannot form a cross-linked network with PDMS (polydimethylsiloxane), a conductive path is blocked, the conductivity of the composite material is weakened to a great extent, the resistance temperature change rate of the flexible sensor is small, and the sensitivity to temperature is not high.
Therefore, how to solve the technical problems that the graphene cannot form a cross-linked network with the PDMS to block a conductive path, so that the resistance temperature change rate of the flexible sensor is very small, and the sensitivity to temperature is not high has become a great need for solving by those skilled in the art.
Disclosure of Invention
The invention provides a method for manufacturing a sandwich-shaped flexible temperature sensor, which is characterized in that a conducting layer is prepared by using graphene dispersion liquid independently to reduce van der Waals force among graphene particles and increase electrostatic repulsion among particle surfaces to increase the distance among graphene sheet layers, so that the agglomeration effect is weakened, and the technical problems of small resistance temperature change rate and low temperature sensitivity of the conventional flexible sensor are solved.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a sandwich-shaped flexible temperature sensor comprises an upper substrate and a lower substrate which are vertically attached, a strip-shaped conductive layer arranged in an attaching surface between the upper substrate and the lower substrate, and two conductive adhesive tapes which are respectively connected with two ends of the conductive layer and extend out of the attaching surface;
the upper substrate and the lower substrate are prepared from PDMS monomers and curing agents;
the conducting layer is prepared from graphene dispersion liquid.
Preferably, the dispersant in the graphene dispersion liquid is NMP or glycerol, and the mass ratio of the graphene in the graphene dispersion liquid to the NMP is 1: 1.2-1: 1.5, or the mass ratio of graphene to glycerol in the graphene dispersion liquid is 1: 6-1: 8.
Preferably, in the upper substrate and/or the lower substrate, the mass ratio of the PDMS matrix to the curing agent is 8: 1-12: 1.
preferably, the length of the upper substrate and the lower substrate is 130-260 mm, the width of the upper substrate and the lower substrate is 35-45 mm, and the thickness of the upper substrate and the lower substrate is 1-3 mm. The conducting layer sets up in the central position on the laminating surface of upper and lower base plate, and the length of conducting layer is 9 ~ 12mm, and the width is 4 ~ 7mm, thickness 0.3 ~ 0.6 mm.
A preparation method of a sandwich-shaped flexible temperature sensor comprises the following steps:
preparing a PDMS curing solution, injecting the PDMS curing solution into the first groove mold, and curing to obtain a lower substrate;
respectively attaching at least one conductive adhesive tape extending out from the lower substrate to two ends of the lower substrate, and enclosing a second groove die in the middle area of the lower substrate by using an insulating adhesive tape with the thickness of 0.3-0.6 mm, wherein one end of the conductive adhesive tape is positioned in the second groove die;
injecting the prepared graphene dispersion liquid into the second groove die, enabling the graphene dispersion liquid to be uniformly distributed in the second groove die, and curing to form a conducting layer;
and arranging a third groove mold along the outer edge of the lower substrate, injecting the prepared PDMS curing solution into the third groove mold, and curing to obtain the upper substrate attached to the lower substrate.
Preferably, the dispersant is NMP, and preparing the graphene dispersion liquid includes:
mixing graphene and an NMP solvent according to a mass ratio of 1: 1.2-1: 1.5, wherein the concentration of the NMP solvent is 1; mixing graphene and a glycerol solvent according to a mass ratio of 1: 6-1: 8, wherein the concentration of the glycerol solvent is 1. Placing the mixed solution of graphene and NMP on a magnetic heating stirrer for stirring, wherein the temperature is 40-60 ℃ and lasts for 15-30 min; and at room temperature, placing the mixed solution of graphene and glycerol on a magnetic stirrer for stirring for 40-60 min to prepare the graphene dispersion liquid.
Preferably, the length of the first groove and the third groove is 130-260 mm, the width of the first groove and the third groove is 35-45 mm, and the thickness of the first groove and the third groove is 1-3 mm; the length of the second groove is 9-12 mm, the width is 4-7 mm, and the thickness is 0.3-0.6 mm.
Preferably, the PDMS curing solution is prepared by the following steps:
adding a curing agent into the PDMS solution according to the mass ratio of the PDMS matrix to the curing agent of 8: 1-12: 1, mixing, stirring for 10-20 min, and removing bubbles in vacuum to obtain the PDMS curing solution.
The invention has the following beneficial effects:
1. according to the manufacturing method of the sandwich-shaped flexible temperature sensor, the conducting layer is independently prepared through the graphene dispersion liquid, so that the van der Waals force among graphene particles is reduced, the electrostatic repulsion force among particle surfaces is increased to increase the distance among graphene sheet layers, the agglomeration effect is further weakened, the resistance temperature change rate of the flexible sensor is increased, and the sensitivity of the flexible sensor to temperature change is improved.
2. In the preferred scheme of the invention, PDMS curing agents are adopted: matrix 1: the material of 10 proportions is as upper and lower base plate, can increase the dependent variable and the elastic modulus of flexible sensor for flexible sensor can bear the strain form such as tensile, buckling, distortion, it can effectual with human skin laminating, moves along with skin, and the relevant data of measurement can be more accurate than rigid sensor.
3. In the preferred scheme of the invention, NMP is used as a dispersing agent in the graphene dispersion liquid, so that the uniformity among graphene layers can be greatly improved, the resistance of the prepared flexible sensor is in good linearity along with the temperature change, the stability of the resistance along with the temperature change is improved, and the sensitivity to the temperature can be improved.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic diagram of a flexible sensor according to the present invention;
FIG. 2 is a stress-strain curve of PDMS materials with different ratios in the preferred embodiment of the present invention, wherein the insert is an enlarged view of 1:5 and 1:10 ratios;
FIG. 3 is a process for preparing a flexible sensor according to a preferred embodiment of the present invention, wherein (a) a lower substrate is prepared to be recessed (b) a conductive layer is applied (c) an insulating tape is peeled off (d) a upper substrate is prepared (e) a sample preparation is completed;
FIG. 4 is a resistance temperature curve of a flexible sensor made of graphene (mixed glycerol) in a preferred embodiment of the present invention in the range of 30 deg.C-80 deg.C;
FIG. 5 is a resistance temperature curve and a linear fitting curve of the flexible sensor prepared from graphene (mixed with NMP) in the preferred embodiment of the present invention at 30-80 ℃;
fig. 6 is a resistance temperature curve of graphene mixed with different materials in a preferred embodiment of the present invention.
Detailed Description
The embodiments of the invention will be described in detail below with reference to the drawings, but the invention can be implemented in many different ways as defined and covered by the claims.
The equipment and materials used in the present invention come out as follows:
table 1 materials used in the experiments
TABLE 2 Experimental Equipment
The first embodiment is as follows:
as shown in fig. 1, the present invention discloses a sandwich-shaped flexible temperature sensor, which comprises an upper substrate 1 and a lower substrate 3 which are vertically attached to each other, a strip-shaped conductive layer 2 arranged in an attachment surface between the upper substrate 1 and the lower substrate 3, and two conductive tapes respectively connected with two ends of the conductive layer 2 and extending out of the attachment surface;
the upper substrate 1 and the lower substrate 3 are prepared from PDMS monomers and curing agents;
the conducting layer 2 is prepared from graphene dispersion liquid.
In addition, this embodiment 1 discloses a method for preparing the sandwich-shaped flexible temperature sensor, which specifically includes the following steps:
preparing a PDMS curing solution, injecting the PDMS curing solution into the first groove mold, and curing to obtain a lower substrate 3;
respectively attaching at least one conductive adhesive tape extending from the lower substrate 3 to two ends of the lower substrate 3, and enclosing a second groove mold in the middle area of the lower substrate 3 by using an insulating adhesive tape, wherein one end of the conductive adhesive tape is positioned in the second groove mold;
injecting the prepared graphene dispersion liquid into the second groove mold, uniformly distributing the graphene dispersion liquid in the second groove mold, and curing to form a conductive layer 2;
and arranging a third groove mold around the outer edge of the lower substrate 3, injecting the prepared PDMS curing solution into the third groove mold, and curing to obtain the upper substrate 1 attached to the lower substrate 3.
According to the sandwich-shaped flexible temperature sensor and the manufacturing method thereof, the conducting layer is independently prepared through the graphene dispersion liquid, so that the van der Waals force among graphene particles is reduced, the electrostatic repulsion force among particle surfaces is increased to increase the distance among graphene sheet layers, and further the agglomeration effect is weakened, so that the resistance temperature change rate of the flexible sensor is increased, and the sensitivity of the flexible sensor to temperature change is improved, so that the technical problems that the resistance temperature change rate of the existing flexible sensor is small and the sensitivity to temperature is low are solved.
Example two:
the embodiment is an expanded embodiment of the first embodiment, and is different from the first embodiment in that the preparation of the upper and lower substrates and the preparation of the conductive layer are refined, and the performance of the prepared flexible sensor is tested. The method specifically comprises the following steps:
preparation of Upper and lower substrates
As a flexible temperature sensor applied to the wearable field, a "sandwich structure" requires a substrate thereof to have excellent flexibility. PDMS has the advantages of large temperature resistance range, good biocompatibility, low preparation cost and the like. Therefore, in this experiment, PDMS was selected as the upper and lower substrates of the "sandwich" and a sandwich-like flexible temperature sensor was designed and manufactured. The PDMS is prepared by mixing a monomer and a curing agent according to a certain proportion, and finally preparing the PDMS flexible material under the curing condition of a certain temperature and time. Preparing a PDMS substrate, firstly preparing materials according to the proportion of a PDMS monomer and a curing agent, mixing the PDMS monomer and the curing agent, and then stirring for 10min by using a glass rod; pouring the mixture into an injector, and vacuumizing to remove residual gas in the injector; injecting the sample into the mold (i.e. the first groove and the third groove in the embodiment) by using an injector, and after the electrothermal constant temperature drying oven is cured, removing the mold and taking out the sample, thereby completing the preparation of the PDMS substrate. It should be noted that a level meter is used to ensure the level of the platform before curing, so as to ensure the uniform thickness of the prepared sample.
The characteristics of the PDMS material such as flexibility and rigidity are greatly related to different mass ratios of the PDMS matrix and the curing agent, so that the performance of the PDMS in different proportions is explored, and the proportion of the PDMS monomer and the curing agent suitable for the sandwich flexible substrate is determined. The experiment adopts Sylgard184 type PDMS material of Dow Corning company, the preparation process is marked to distinguish samples, and finally curing is carried out under the same conditions (60 ℃, 2h) to prepare the curing agent: matrix 1:5, 1:10 and 1:15 samples.
The tensile properties of the three samples were tested using a static tensile machine and processed to obtain the curve shown in figure 2.
The elastic material being under external forceDeformation occurs under the action of the elastic material, and an important parameter showing the mechanical property of the elastic material is the elastic modulus (also called Young modulus), which represents the difficulty of deformation of an object. Calculation formula of stress, strain and elastic modulus[31]The following were used:
stress:
strain:
elastic modulus (young's modulus):
wherein F is the external force applied to the test piece, A is the cross-sectional area during stretching, L is the total length of the test piece after stretching, and L is the total length of the test piece after stretching0The original length of the test piece.
Three samples with the ratio of the PDMS curing agent to the PDMS matrix being 1:5, 1:10 and 1:15 are obtained by processing the test data, the maximum strain of the three samples is 0.98, 2.21 and 0.95 respectively, and the average elastic modulus of the three samples is E1＝0.27846MPa、E21.04372MPa and E30.26151 MPa. The maximum strain represents the maximum deformation that the material can withstand, and the greater the modulus of elasticity the greater the stiffness of the material. Compared with other two materials in the proportion, the PDMS material prepared from the curing agent and the PDMS matrix in the proportion of 1:10 has the maximum strain and the maximum elastic modulus, and is a flexible material with excellent flexibility. Therefore, the PDMS curing agent was chosen: PDMS matrix ═ 1: the 10-part material served as the flexible substrate for the "sandwich" structure.
Flexible sensor preparation
The preparation flow is shown in figure 3:
(1) 0.2g of graphene was weighed and mixed with 1.28g of glycerol and 0.258g of NMP solvent, respectively. Placing the mixed solution on a magnetic heating stirrer for stirring for 20min to prepare conductive solutions with different ratios of graphene to the solvent;
(2) preparing a PDMS solution (PDMS substrate: curing agent: 1:10), pouring the solution into a groove mold (acrylic material) with length, width, thickness, 150mm, 40mm, 2mm, and after curing, preparing a lower substrate 3;
(3) attaching a conductive tape (used as an electrode) on the surface of the lower substrate, and enclosing a 10mm by 5mm groove mold by using an insulating tape with the thickness of 0.5mm, as shown in fig. 3 (a);
(4) and (3) coating the prepared conductive solution in the groove mould of the previous step, and uniformly coating the conductive solution by using a glass slide. Tearing off the insulating tape to obtain a conductive layer 2 with the thickness of 0.5mm, which is shown in FIG. 3 (c);
(5) a groove mold of 40mm x 20mm is formed by using an EVA sponge tape of 2mm thickness, and the prepared PDMS solution is poured into the groove mold, and after curing at 60 ℃ for 2 hours, a sandwich-like flexible temperature sensor is successfully prepared, as shown in fig. 3 (e).
Performance testing and results analysis
Temperature sensitive Performance test
The experiment mixes graphite alkene among different solvents, and glycerine can adjust the viscosity and the dispersion graphite alkene of conducting solution, and through the above dispersibility contrast, it is a good graphite alkene dispersant to obtain NMP, has prepared graphite alkene respectively: glycerol ═ 1:6.4 and graphene: NMP ═ 1:1.29 two ratio "sandwich" flexible sensors. The sample is placed on a constant temperature heating table, the sample is fixed by an insulating adhesive tape (convenient for heat transfer), and the built test platform is matched with an LCR bridge to test the temperature and sensitivity characteristics of the sample.
Test results and analysis
Since the minimum temperature provided by the constant temperature heating stage is 30 ℃, and the application field of the sample is wearable equipment, the measurement range of the sample is set to be 30-80 ℃. The temperature rise range is 10 ℃ every time, after the temperature is stable, the resistance of the sample is recorded, and 6 groups of resistance data under constant temperature are obtained by measuring each sample. Because interference exists in the measurement process, the obtained data has serious fluctuation, and therefore the data needs to be processed first. Noise reduction processing is carried out on the signals by using ORIGIN software, and the influence of noise on data results is eliminated as much as possible. Specifically, a noise reduction mode of Percentile Filter smoothing (Percentile Filter) is adopted, and parameters are properly adjusted to realize noise filtering and simultaneously keep the trend of a curve. The noise reduction data is statistically analyzed to obtain the average resistance value and the standard deviation of the samples at different temperatures, so as to obtain the resistance temperature curves of different samples as shown in figures 4 and 5,
as shown in fig. 4 and 5, the resistance changes with temperature first showing a positive temperature effect (PTC) tendency and then a negative temperature effect (NTC) tendency. The change can be explained by applying a conductive channel theory and a tunneling effect theory, and the trend that the resistance of the sample is increased and then decreased along with the temperature is the result of the combined action of the two mechanisms. Based on this, when the temperature is just increased, the interlayer spacing of graphene is increased due to the thermal expansion effect, the conductive channel is damaged, and the sample resistivity is increased. However, as the temperature increases, the interlayer distance is saturated, the effect of thermal expansion decreases, and at high temperatures, electrons in the graphene become active, and the tunneling current increases, so that the resistance value of the sample starts to decrease. As the resistance of the sample of the flexible sensor in fig. 6 increases with increasing temperature, the effect of thermal expansion dominates. By performing linear fitting on the data, the resistance value of the sample of the graphene mixed with NMP is basically linearly changed in the temperature range of 30-80 ℃. Meanwhile, by utilizing a linear equation obtained by ORIGIN software fitting, the correlation coefficient (adj. R-Square) reaches 0.97361, and the fitting effect is good.
The Temperature Coefficient of Resistance (TCR) represents the relative amount of change in resistance when the temperature changes by 1 ℃. The calculation formula is as follows:
in the formula, R0Represents the initial resistance of the sample in deg.C-1。
TCR is shown in graph as curveSlope, the rate of change of resistance of the sample, respectively TCR, is obtained by solving the average slope of the two curvesVG＝0.00196℃-1、TCRNMP＝0.01621℃-1. The resistance temperature change rate of the sample of the graphene mixed glycerol is small, and the sensitivity to the temperature is not high. And the sample of the graphene mixed glycerol not only has good linearity of resistance changing along with temperature, but also has high sensitivity to temperature. The difference of the dispersion media determines the uniformity between the graphene layers, and further determines the competition result of the thermal expansion effect and the tunnel effect, and macroscopically shows the stability of the resistance along with the temperature change.
In summary, according to the sandwich-shaped flexible temperature sensor and the manufacturing method thereof, the conducting layer is separately prepared through the graphene dispersion liquid, so that the van der waals force among graphene particles is reduced, the electrostatic repulsion force among particle surfaces is increased to increase the distance among graphene sheet layers, and further the agglomeration effect is weakened, so that the resistance temperature change rate of the flexible sensor is increased, and the sensitivity of the flexible sensor to temperature change is improved, so that the technical problems that the resistance temperature change rate of the existing flexible sensor is small and the sensitivity to temperature is not high are solved.
In the preferred scheme of the invention, PDMS curing agents are adopted: PDMS matrix ═ 1: the material of 10 proportions is as upper and lower base plate, can increase the dependent variable and the elastic modulus of flexible sensor for flexible sensor can bear the strain form such as tensile, buckling, distortion, it can effectual with human skin laminating, moves along with skin, and the relevant data of measurement can be more accurate than rigid sensor.
In the preferred scheme of the invention, NMP is used as a dispersing agent in the graphene dispersion liquid, so that the uniformity among graphene layers can be greatly improved, the resistance of the prepared flexible sensor is in good linearity along with the temperature change, the stability of the resistance along with the temperature change is improved, and the sensitivity to the temperature can be improved.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. A preparation method of a sandwich-shaped flexible temperature sensor is characterized by comprising the following steps:
preparing a PDMS curing solution, injecting the PDMS curing solution into the first groove mold, and curing to obtain a lower substrate;
respectively attaching at least one conductive adhesive tape extending out from the lower substrate to two ends of the lower substrate, and enclosing a second groove die in the middle area of the lower substrate by using an insulating adhesive tape with the thickness of 0.3-0.6 mm, wherein one end of the conductive adhesive tape is positioned in the second groove die;
injecting the prepared graphene dispersion liquid into the second groove die, enabling the graphene dispersion liquid to be uniformly distributed in the second groove die, and curing to form a conducting layer;
arranging a third groove mold around the outer edge of the lower substrate, injecting the prepared PDMS curing solution into the third groove mold, and curing to obtain an upper substrate attached to the lower substrate;
wherein the dispersing agent in the graphene dispersion liquid is NMP or glycerol, and the preparation of the graphene dispersion liquid comprises the following steps:
mixing graphene and an NMP solvent according to a mass ratio of 1: 1.2-1: 1.5, wherein the concentration of the NMP solvent is 1; mixing graphene and a glycerol solvent according to a mass ratio of 1: 6-1: 8, wherein the concentration of the glycerol solvent is 1; placing the mixed solution of graphene and NMP on a magnetic heating stirrer for stirring, wherein the temperature is 40-60 ℃ and lasts for 15-30 min; and at room temperature, placing the mixed solution of graphene and glycerol on a magnetic stirrer for stirring for 40-60 min to prepare the graphene dispersion liquid.
2. The method for preparing a sandwich-like flexible temperature sensor according to claim 1, wherein the first and third grooves have a length of 130 to 260mm, a width of 35 to 45mm, and a thickness of 1 to 3 mm; the length of the second groove is 9-12 mm, the width is 4-7 mm, and the thickness is 0.3-0.6 mm.
3. The method of claim 2, wherein the PDMS curing solution is prepared by the following steps:
mixing the PDMS matrix and the curing agent according to the mass ratio of 8: 1-12: 1, stirring for 10-20 min, and removing bubbles in vacuum to obtain the PDMS curing solution.
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