CN117812985A - Flexible photo-thermal electric detection device based on spraying method and preparation method thereof - Google Patents
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Abstract
The invention belongs to the technical fields of flexible sensor technology, photo-thermal technology and nano material preparation, and discloses a flexible photo-thermal detection device based on a spraying method and a preparation method thereof, wherein the device comprises a substrate layer, a bottom electrode layer, a photo-thermal sensitive layer and a top electrode layer which are sequentially arranged; the material of the photo-thermal electric sensitive layer is Ag 2 The mixture of Se nanowires and PVP is prepared on the bottom electrode layer by a spraying method. The preparation method is simple, efficient and nontoxic, and PVP can protect Ag 2 The Se nano rod is not easy to oxidize, so that the thermoelectric performance of the device can be kept stable for a long time in a dry environment, and the service life of the device is prolonged.
Description
Technical Field
The invention belongs to the technical field of flexible sensors, photo-thermal power and nano material preparation, and particularly relates to a flexible photo-thermal power detection device based on a spraying method and a preparation method thereof.
Background
With the development of fields such as wearable equipment, intelligent medical treatment, intelligent health monitoring and the like, flexible sensors are widely researched and applied as a key technology. The flexible sensor can realize real-time monitoring of human body movement, physiological signals and the like, and has the advantages of comfort, portability, no interference and the like. The photo-thermal electric technology is a technology that converts light energy into heat energy and then converts the heat energy into an electric signal. This technology has important applications in the fields of sensors, detectors and renewable energy. The existing photo-thermoelectric devices generally adopt materials containing antimony and the like as materials of the thermoelectric devices. However, the conventional thermoelectric materials have problems of high cost, complicated preparation, toxicity, and the like. To overcome these problems, researchers have been working to find new thermoelectric materials, where Ag 2 Se is of great interest due to its good thermoelectric properties and relatively low manufacturing costs. Although Ag 2 Se has certain advantages as a thermoelectric material, but the current preparation method still faces some challenges. The traditional preparation method may have the problems of environmental pollution, low material purity, long preparation time and the like, and the wide application of the traditional preparation method is limited.
Therefore, there is a need to study and propose a simple, efficient, nontoxic photo-thermal electric device and a preparation method thereof to meet the requirements of the field of photo-thermal electric devices.
Disclosure of Invention
In order to solve the problems in the materials and preparation of the photo-thermal electric devices in the prior art, the invention provides a flexible photo-thermal electric detection device based on a spraying method and a preparation method thereof, and Ag is adopted 2 Se is used as a thermoelectric device material and is combined with a spraying technology, so that the preparation process is simplified, the preparation efficiency is improved, and the influence on the environment is reduced.
In order to solve the technical problems, the invention adopts the following technical scheme: a flexible photoelectric detector based on a spraying method comprises a substrate layer, a bottom electrode layer, a photoelectric sensitive layer and a top electrode layer which are sequentially arranged; the material of the photo-thermal electric sensitive layer is Ag 2 The mixture of Se nano rod and PVP is prepared on the bottom electrode layer by a spraying method.
The substrate layer is made of PI, the bottom electrode layer is made of Ti, and the top electrode layer is made of Ag.
The thickness of the bottom electrode layer is 800-1500 mu m, the thickness of the top electrode layer is 30-100 mu m, and the thickness of the photo-thermal sensitive layer is 3-8 mu m; ag in the material of the photo-thermal electric sensitive layer 2 The mass ratio of the Se nano rod to PVP is as follows: 1: 0.02-1: 0.05.
in addition, the invention also provides a preparation method of the flexible photo-thermal electric detection device based on the spraying method, which comprises the following steps:
step S1: synthesis of Ag using template method 2 Se nano rod and preparing Ag 2 Se ink specifically comprises the following steps:
step S101: seO is carried out 2 And adding the beta-cyclodextrin into a beaker containing 100 ml deionized water, and magnetically stirring to form a solution A; adding L-ascorbic acid into another beaker containing 100 ml deionized water to form a solution B; slowly dripping the solution A into the solution B, magnetically stirring until the solution is completely reacted, centrifuging to remove supernatant, washing and drying, and collecting Se nanowires;
step S102: adding the obtained Se nanowire into 10ml glycol, and performing ultrasonic dispersion to form a solution C; adding AgNO into 10ml absolute ethanol 3 Magnetically stirring to form a solution D; adding L-ascorbic acid into 20 ml deionized water, and magnetically stirring to form a solution E; slowly dripping the solution D and the solution E into the solution C in sequence, continuously stirring to react, centrifuging, washing and drying, and collecting Ag 2 Se nanorods;
step S103: ag with 2 Mixing Se nano rod and PVP, dispersing in ethanol solution, and performing ultrasonic treatment by an ultrasonic dispersing instrument to obtain Ag 2 Se ink;
step S2: depositing a bottom electrode layer on the substrate layer through a first shadow mask;
step S3: transferring the device into a clean room, spraying Ag on the bottom electrode layer through a second shadow mask 2 Se ink is uniformly mixed with the film to obtain a photothermal sensitive layer;
step S4: a top electrode layer is deposited over the photothermographic sensitive layer through a third shadow mask.
In the step S101, 0.5g of SeO is added 2 And 0.5g beta-cyclodextrin was added to a beaker containing 100 ml deionized water and magnetically stirred to form solution a; 2 g L-ascorbic acid was added to another beaker containing 100 ml deionized water to form solution B.
In the step S102, 0.3 g Se nanowire is added into 10ml glycol, and the solution C is formed by ultrasonic dispersion.
In the step S102, 1.3g AgNO is added into 10ml glycol 3 Magnetically stirring to form a solution D; 4g of L-ascorbic acid was added to 20 ml deionized water and magnetically stirred to form solution E.
In the step S103, 0.5g of Ag is added 2 Mixing Se nano rod with 0.017g PVP, dispersing in 10ml absolute ethyl alcohol solution, and performing ultrasonic treatment by an ultrasonic dispersing instrument to obtain Ag 2 Se ink.
In the step S3, the pressure of the sprayer is 1bar, the diameter of an outlet of the sprayer is 0.2mm, the sprayer is dried in a vacuum drying oven at 60 ℃ after spraying, and the thickness range of the sprayed photo-thermal electric sensitive layer is 3-8 mu m.
In the step S2, the 3A S is formed on the substrate layer by using an electron beam evaporator -1 Ti with the thickness of 800-1500 mu m is deposited as a bottom electrode layer;
in the step S4, the same electron beam evaporator is used for forming 1.5A S on the photo-thermal sensitive layer -1 And (3) depositing Ag with the thickness of 30-100 mu m as a top electrode layer.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention provides a flexible photo-thermal electric detection device based on a spraying method and a preparation method thereof, wherein Ag is used for preparing the flexible photo-thermal electric detection device 2 Preparation of Ag by mixture of Se nanorods and PVP (polyvinylpyrrolidone) 2 Se printing ink is sprayed by a spray gun to prepare a photo-thermal sensitive layer by a spray method, and the preparation process is simple, efficient and nontoxic; also, on the one hand, PVP can protect Ag 2 The Se nano rod is not easy to oxidize, so that the thermoelectric performance of the device can be kept stable for a long time in a dry environment, and the service life of the device is prolonged; PVP, on the other hand, as a viscous material, helps to better bind Ag 2 The Se nano rods are attached to the bottom electrode layer, so that the combination and stability between materials are enhanced, and the excellent performance of the sensor is realized. The invention can prepare the flexible photo-thermal detector with excellent photo-voltage response. The photoelectric detector is suitable for the fields of medical health monitoring, intelligent wearing, environment monitoring and the like, and has wide application prospect.
2. In the invention, the preparation process of each film layer of the device is realized by a mask technology, so that the pollution of Ag by a complex photoetching method can be avoided 2 Se material, the rejection rate in the preparation process is reduced.
3. In the invention, ag used for the photo-thermal sensitive layer 2 The Se nano rod is synthesized by a template method, has specific size and shape, has a light trapping effect by multiple reflection of light in the nano rod, and can strengthen light absorption, so that larger conversion of the photo-thermal effect is obtained. In addition, the bottom electrode layer is made of Ti material and can help the photo-thermal sensitive layer Ag 2 Adhesion of Se/PVP material.
Drawings
Fig. 1 is a schematic structural diagram of a flexible photo-thermal electric detecting device based on a spraying method according to a first embodiment of the present invention;
FIG. 2 shows Ag obtained in accordance with the second embodiment of the present invention 2 Scanning Electron Microscope (SEM) images of Se nanorods;
FIG. 3 is a schematic structural diagram of a photo-thermal electric detecting device prepared according to a second embodiment of the present invention;
FIG. 4 is a graph showing the change rate of the conductivity of the photo-thermal sensitive layer film with the number of bends in a conductivity bend cycle test;
fig. 5 is a graph of the conductivity and seebeck coefficient of a photothermographic element film over time.
In the figure: 1 is a substrate layer, 2 is a bottom electrode layer, 3 is a photo-thermal sensitive layer, and 4 is a top electrode layer.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments; all other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
As shown in fig. 1, a first embodiment of the present invention provides a flexible photothermal detection device based on a spraying method, which includes a substrate layer 1, a bottom electrode layer 2, a photothermal sensitive layer 3, and a top electrode layer 4 that are sequentially disposed; the material of the photo-thermal electric sensitive layer 3 is Ag 2 A mixture of Se nanorods and PVP (polyvinylpyrrolidone) was prepared on the bottom electrode layer 2 by a spray process.
Specifically, in this embodiment, the material of the substrate layer 1 is PI (polyimide), the material of the bottom electrode layer 2 is Ti, and the material of the top electrode layer 4 is Ag.
Specifically, in this embodiment, the thickness of the bottom electrode layer 2 is 800-1500 μm, the thickness of the top electrode layer 4 is 30-100 μm, and the thickness of the photo-thermal sensitive layer 3 is 3-8 μm. Ag in the material of the photothermal sensitive layer 3 2 The mass ratio of the Se nano rod to PVP is as follows: 1: 0.02-1: 0.05.
preferably, in the present embodiment, the thickness of the bottom electrode layer 2 is 1000 μm, the thickness of the top electrode layer 4 is 50 μm, and the thickness range of the photothermal sensitive layer 3 is 5 μm. Ag in the material of the photothermal sensitive layer 3 2 The mass ratio of the Se nano rod to PVP is as follows: 1:0.034.
example two
The second embodiment of the invention provides a preparation method of a flexible photo-thermal electric detection device based on a spraying method, which comprises the following steps:
step S1: synthesis of Ag using template method 2 Se nano rod and preparing Ag 2 Se ink specifically comprises the following steps:
step S101: synthesizing Se nanowires.
The specific method comprises the following steps: seO is carried out 2 And adding the beta-cyclodextrin into a beaker containing 100 ml deionized water, and magnetically stirring to form a solution A; adding L-ascorbic acid into another beaker containing 100 ml deionized water to form a solution B; slowly dropping the solution A into the solution B, magnetically stirring for 4 hours until the solution is completely reacted, then removing the supernatant by centrifugation, washing and drying, and collecting Se nanowires.
Specifically, in the step S101, 0.5g of SeO is added 2 And 0.5g beta-cyclodextrin was added to a beaker containing 100 ml deionized water and magnetically stirred to form solution a; 2 g L-ascorbic acid was added to another beaker containing 100 ml deionized water to form solution B.
Step S102: synthesis of Ag 2 Se nanorods.
The specific method comprises the following steps: adding the obtained Se nanowire into 10ml glycol, and performing ultrasonic dispersion to form a solution C; adding AgNO into 10ml absolute ethanol 3 Magnetically stirring to form a solution D; adding L-ascorbic acid into 20 ml deionized water, and magnetically stirring to form a solution E; slowly dripping the solution D and the solution E into the solution C successively, continuously stirring to react, centrifuging, washing and drying, and collecting Ag with the shape of powder 2 The SEM image of Se nanorods is shown in fig. 2.
Specifically, in the step S102, 0.3 g of Se nanowires are added to 10ml glycol, and the solution C is formed by ultrasonic dispersion. 1.3g AgNO was added to 10ml glycol 3 Magnetically stirring to form a solution D; 4.0g of L-ascorbic acid was added to 20 ml deionized water and magnetically stirred to form solution E.
Step S103: preparation of Ag 2 Se ink.
The specific method comprises the following steps: ag with 2 Mixing Se nano rod and PVP, dispersing in ethanol solution, and performing ultrasonic treatment by an ultrasonic dispersing instrument to obtain Ag 2 Se inkThe method comprises the steps of carrying out a first treatment on the surface of the After the ink is obtained, the preparation of the photo-thermal electric device can be carried out.
Specifically, in the step S103, ag is mixed 2 The mass ratio of the Se nano rod to PVP is as follows: 1: 0.02-1: 0.05. preferably, in this example, 0.5g of Ag is used 2 Mixing Se nano rod and 0.017g PVP, dispersing in 10ml absolute ethyl alcohol solution, obtaining absolute ethyl alcohol solution with PVP concentration of 0.2wt%, and then carrying out ultrasonic treatment by an ultrasonic dispersing instrument to obtain Ag 2 Se ink.
Step S2: a bottom electrode layer 2 is deposited on the substrate layer 1 through a first shadow mask.
Prior to deposition, the surface of the substrate layer 1 is cleaned to remove organic residues to avoid re-agglomeration.
Specifically, in the step S2, the substrate layer 1 is irradiated with 3 a S by an electron beam evaporator -1 Ti with the thickness of 800-1500 mu m is deposited as a bottom electrode layer 2; preferably, the bottom electrode layer 2 has a thickness of 1000 μm.
Specifically, in the step S2, the substrate layer 1 is a PI substrate.
Step S3: transferring the device into a clean room, spraying Ag on the bottom electrode layer 2 through a second shadow mask 2 Se printing ink is sprayed until the film is uniform, and then the film is dried under a vacuum drying oven at 60 ℃ to obtain the photothermal sensitive layer 3.
In the step S3, the sprayer pressure was 1bar, and the outlet diameter of the sprayer was selected to be 0.2mm. The thickness range of the finally obtained photo-thermal electric sensitive layer 3 is 3-8 mu m; preferably, the thickness of the photothermographic element layer 3 is 5.+ -. 0.5. Mu.m.
Step S4: a top electrode layer 4 is deposited on the photo and thermal sensitive layer 3 through a third shadow mask.
In the step S4, the same electron beam evaporator is used to form 1.5A S on the photo-thermal sensitive layer 3 -1 Ag with the thickness of 30-80 mu m is deposited as a top electrode layer 4; preferably, the top electrode layer 4 has a thickness of 50 μm. In addition, in this embodiment, after the bottom electrode layer 2 and the top electrode layer 4 are deposited, they are baked at a certain time and temperature to form a stable structure.
As shown in fig. 3, which is a schematic structural diagram of the photo-thermal detection device prepared in this embodiment, it can be seen from the figure that the shapes of the bottom electrode layer 2 corresponding to the photo-thermal sensitive layer 3 and the top electrode layer 4 may be different, and in particular, the shapes of the first, second and third shadow masks may be adjusted.
The invention utilizes the mask technology to control the preparation procedures of all layers, and can avoid the pollution of Ag by a complex photoetching method 2 Se materials.
As shown in FIG. 4, ag is shown 2 The rate of change of conductivity of Se/PVP films is shown graphically as a curve of the film around a bar with a radius of 8 mm. It can be seen that the conductivity of the film was slowly decreased with the increase of the number of bends, reaching 89.8% and 76% of the initial values at the bending numbers of 500 and 1000, respectively, demonstrating the good flexibility stability of the photothermal sensitive layer 3 employed in the present invention. In addition, in order to test the stability of the film, the change in thermoelectric properties of the film after being left in an indoor environment for a certain period of time is shown in fig. 5. It can be seen that the thermoelectric properties can be kept stable for 40 days, then after 50 days only the conductivity drops to 89% of the initial value, while the Seebeck coefficient remains almost unchanged. The decrease in film conductivity is mainly due to Ag 2 Oxidation of Se nano rod, and PVP plays a role in protection, so that the thermoelectric performance of the film can be kept stable for a long time in a dry environment.
The sensitivity mechanism of the prepared photo-thermal electric detector is as follows: when light is irradiated on the top of the device, as shown in fig. 1, the energy of photons is transferred to the top of the photothermographic layer through the top electrode layer 4, so that the temperature of the top is increased, a temperature difference is generated between the top and the bottom electrode layer 2, and a voltage is generated on both sides thereof based on the seebeck effect. The performance parameters of the optothermoelectric device can be obtained by testing the output voltage between the top electrode layer 4 and the bottom electrode layer 2. The prepared photoelectric detection device is suitable for the fields of medical health monitoring, intelligent wearing, environmental monitoring and the like, can be practically applied to photovoltaic power generation and optical imaging, and has wide application prospect.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (10)
1. The flexible photo-thermal electric detection device based on the spraying method is characterized by comprising a substrate layer (1), a bottom electrode layer (2), a photo-thermal electric sensitive layer (3) and a top electrode layer (4) which are sequentially arranged; the material of the photo-thermal electric sensitive layer (3) is Ag 2 The mixture of Se nano rod and PVP is prepared on the bottom electrode layer (2) by a spraying method.
2. The flexible photo-thermal detection device based on the spraying method according to claim 1, wherein the material of the substrate layer (1) is PI, the material of the bottom electrode layer (2) is Ti, and the material of the top electrode layer (4) is Ag.
3. The flexible photothermal electrical detection device based on the spraying method according to claim 1, wherein the thickness of the bottom electrode layer (2) is 800-1500 μm, the thickness of the top electrode layer (4) is 30-100 μm, and the thickness of the photothermal electrical sensitive layer (3) is 3-8 μm; ag in the material of the photothermal sensitive layer (3) 2 The mass ratio of the Se nano rod to PVP is as follows: 1: 0.02-1: 0.05.
4. the method for manufacturing the flexible photo-thermal electric detection device based on the spraying method as claimed in claim 1, comprising the following steps:
step S1: synthesis of Ag using template method 2 Se nano rod and preparing Ag 2 Se ink specifically comprises the following steps:
step S101: seO is carried out 2 And beta-ringAdding dextrin into a beaker containing 100 ml deionized water, and magnetically stirring to form a solution A; adding L-ascorbic acid into another beaker containing 100 ml deionized water to form a solution B; slowly dripping the solution A into the solution B, magnetically stirring until the solution is completely reacted, centrifuging to remove supernatant, washing and drying, and collecting Se nanowires;
step S102: adding the obtained Se nanowire into 10ml glycol, and performing ultrasonic dispersion to form a solution C; adding AgNO into 10ml absolute ethanol 3 Magnetically stirring to form a solution D; adding L-ascorbic acid into 20 ml deionized water, and magnetically stirring to form a solution E; slowly dripping the solution D and the solution E into the solution C in sequence, continuously stirring to react, centrifuging, washing and drying, and collecting Ag 2 Se nanorods;
step S103: ag with 2 Mixing Se nano rod and PVP, dispersing in ethanol solution, and performing ultrasonic treatment by an ultrasonic dispersing instrument to obtain Ag 2 Se ink;
step S2: depositing a bottom electrode layer (2) on the substrate layer (1) through a first shadow mask;
step S3: transferring the device into a clean room, spraying Ag on the bottom electrode layer (2) through a second shadow mask 2 Se ink is uniformly mixed with the film to obtain a photothermal sensitive layer (3);
step S4: a top electrode layer (4) is deposited on the photothermographic layer (3) through a third shadow mask.
5. The method for manufacturing a flexible photo-thermal electric detector based on spray coating according to claim 4, wherein in said step S101, 0.5g of SeO is added 2 And 0.5g beta-cyclodextrin was added to a beaker containing 100 ml deionized water and magnetically stirred to form solution a; 2 g L-ascorbic acid was added to another beaker containing 100 ml deionized water to form solution B.
6. The method for preparing a flexible photothermal electrical detection device based on a spraying method according to claim 4, wherein in the step S102, 0.3 g Se nanowires are added to 10ml glycol, and the solution C is formed by ultrasonic dispersion.
7. The method for preparing a flexible photo-thermal electric detector based on spray coating method as claimed in claim 4, wherein in said step S102, 1.3g AgNO is added into 10ml glycol 3 Magnetically stirring to form a solution D; 4g of L-ascorbic acid was added to 20 ml deionized water and magnetically stirred to form solution E.
8. The method for manufacturing a flexible photo-thermal electric detector based on spray coating according to claim 4, wherein in said step S103, 0.5g Ag is used 2 Mixing Se nano rod with 0.017g PVP, dispersing in 10ml absolute ethyl alcohol solution, and performing ultrasonic treatment by an ultrasonic dispersing instrument to obtain Ag 2 Se ink.
9. The method for manufacturing a flexible photo-thermal detector based on a spraying method according to claim 4, wherein in the step S3, the pressure of a sprayer is 1bar, the diameter of an outlet of the sprayer is 0.2mm, the sprayer is dried in a vacuum drying oven at 60 ℃ after the spraying is finished, and the thickness range of a photo-thermal sensitive layer (3) obtained by spraying is 3-8 μm.
10. The method of fabricating a flexible photothermal electrical detector device according to claim 4, wherein in the step S2, the substrate layer (1) is coated with 3 a S by electron beam evaporator -1 Ti with the thickness of 800-1500 mu m is deposited as a bottom electrode layer (2);
in the step S4, the same electron beam evaporator is used for forming 1.5A S on the photo-thermal sensitive layer (3) -1 Is used as a top electrode layer (4) and is deposited with Ag with the thickness of 30-100 mu m.
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