CN113155914B - Interdigital electrode material with vertical orientation three-dimensional structure, and preparation method and application thereof - Google Patents
Interdigital electrode material with vertical orientation three-dimensional structure, and preparation method and application thereof Download PDFInfo
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Abstract
The interdigital electrode material with the vertical orientation three-dimensional structure is formed by compounding nano sheet layer structures stacked by nano materials and arranged between the fingers of the interdigital electrode at intervals in a near vertical orientation mode; the form of the nano material is one or more of zero-dimensional quantum dots, nano particles, one-dimensional nanotubes, nanorods, nanowires or two-dimensional nanosheets. The preparation method comprises the steps of coating the nano material dispersion liquid in a groove of the interdigital electrode, freezing, and freeze-drying. The interdigital electrode material with the vertically-oriented three-dimensional structure is applied to a sensor. The interdigital electrode material with the vertical orientation three-dimensional structure has wide raw material source, the thickness of the nano material is as low as 6 mu m, the composite state of the nano material can be regulated and controlled, and the gas sensing response degree is obviously improved. The method has simple process and low cost, and is suitable for industrial production.
Description
Technical Field
The invention relates to an interdigital electrode material, a preparation method and application thereof, in particular to an interdigital electrode material with a vertical orientation three-dimensional structure, and a preparation method and application thereof.
Background
The construction of the three-dimensional structure oriented perpendicular to the substrate is a major subject of the 'bottom-up' assembly of the nano material, and has good application prospects in the fields of energy, catalysis, seawater desalination and the like. Currently, researchers build vertically oriented three-dimensional structures by using ice crystals as templates. The nano material can be oriented and arranged by regulating and controlling the oriented growth of the ice crystal template, and the prepared three-dimensional structure has a convenient material transmission channel, so that the three-dimensional structure oriented perpendicular to the substrate has a good application prospect in the fields of energy, catalysis, gas sensing, seawater desalination and the like, and the nano material is assembled into the structure to endow the structure with more excellent performance.
In 2011, qiu et al obtained a three-dimensional structure of vertically oriented reduced graphene oxide by a directional freeze-drying method, opening a new chapter in the field of directional freeze-drying (Nature Communications, 2012, 1241. The orientation of the directional freeze-drying can be regulated and controlled in the following ways; (1) Controlling the temperature gradient by designing a die to regulate and control the three-dimensional structure; (2) regulating and controlling through the concentration distribution of the antifreeze agent; and (3) regulating and controlling the hydrophilic and hydrophobic characteristics of the substrate.
In 2017, zhang et al transferred a mixture of GO and ethanol (30, volume ratio) to a PTFE mold, and then placed the mold on the surface of liquid nitrogen for 10 minutes for directional freezing from bottom to top, and the resulting vertically oriented three-dimensional structure with continuous channels had good seawater desalination (ACS Nano 2017, 11, 6817-6824).
Although preliminary research results have been obtained in the field of methods for constructing vertically oriented three-dimensional structures by directional freeze-drying using ice crystals as templates and their applications, there are some limitations and disadvantages:
(1) The existing research is mainly used for constructing aerogel bulk materials, the construction of a three-dimensional structure of a nanometer material with the thickness of less than 30 mu m has certain challenge, and the report is not found at present;
(2) At present, methods for preparing a gas sensor mainly comprise a dripping coating method and a brush coating method, and although the preparation processes of the methods are simple, gas-sensitive materials are often stacked on electrodes in an agglomerated shape, and the composite state of the materials and the electrodes is difficult to regulate and control.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art and provide the interdigital electrode material with the vertical orientation three-dimensional structure, which has wide raw material source, the thickness of the nano material is as low as 6 mu m, the composite state of the nano material can be regulated and controlled, and the gas sensing response degree is obviously improved.
The invention further aims to solve the technical problem of overcoming the defects in the prior art and provide a preparation method and application of the interdigital electrode material with the vertical orientation three-dimensional structure, which has simple process and low cost and is suitable for industrial production.
The technical scheme adopted by the invention for solving the technical problem is as follows: the interdigital electrode material with a vertical orientation three-dimensional structure is formed by compounding interdigital electrodes with a nano-sheet structure stacked by nano materials and arranged at intervals in a nearly vertical orientation manner; the form of the nano material is one or more of zero-dimensional quantum dots, nano particles, one-dimensional nanotubes, nanorods, nanowires or two-dimensional nanosheets and the like. The nanometer material can adsorb the gas molecules that produce among the electrochemical reaction process to turn into the signal of telecommunication with the concentration of gas molecules, the orderly pile up of nanometer material not only can increase nanometer material's specific surface area, increases target gas's adsorption capacity, and the hole between the nanosheet layer more is favorable to target gas rapid, sensitive change resistance simultaneously, goes out quick, the accurate transmission of signal of telecommunication, thereby improves interdigital electrode's sensitivity and response degree. The sheet layer diameter of the quantum dots is 1-10 nm; the particle size of the nano particles is 10-100 nm; the length of the nanotube is 1-20 mu m, and the diameter is more than or equal to 50nm; the number of the nano sheet layers is 1-10, and the diameter of the sheet layer is 1-10 mu m.
Preferably, the nano-material layer formed by the nano-sheet layer structure has the thickness of more than or equal to 6 microns (more preferably 6 to 30 microns), the width of 20 to 500 microns (more preferably 50 to 300 microns), the orientation included angle of the nearly vertically oriented single sheet layer is 60 to 90 degrees, the vertical distance between the nearly vertically oriented single sheet layers is 1 to 12 microns, and the thickness of the single sheet layer is 0.1 to 1.0 micron (more preferably 0.3 to 0.8 micron). The thickness of the electrode layer of the interdigital electrode determines the thickness of the nanometer material layer to a great extent, generally, the thickness of the nanometer material layer is influenced by the coating process and is smaller or slightly larger than the thickness of the electrode layer of the interdigital electrode, and the width of the nanometer material layer is the line distance of the interdigital electrode. The smaller the thickness of the single-layer is, the higher the sensitivity and the response degree of the material are, but the structural performance of the material needs to be considered at the same time.
Preferably, the nano material is one or more of graphene oxide quantum dots, single-layer graphene oxide powder, multi-layer graphene oxide powder, carboxylated carbon nanotubes or zinc oxide nanoparticles. The sheet diameter size of the single-layer graphene oxide powder is more than or equal to 400nm.
Preferably, the thermal conductivity of the electrode layer material of the interdigital electrode is more than or equal to 50 W.m -1 ·K -1 (more preferably 75 W.m or more) -1 ·K -1 ) The surface of the substrate is flat and the thermal conductivity is less than or equal to 5 W.m -1 ·K -1 (more preferably ≦ 1 W.m -1 ·K -1 ) The electrode layer thickness of the interdigital electrode is more than or equal to 10 microns, the line width is 45-250 microns, and the line distance is 20-500 microns (more preferably 50-300 microns). The definition of the thickness, the line width and the line distance of the interdigital electrode material can adapt to the material with the particle diameter of only ten and several micrometers. The electrode material on the surface of the interdigital electrode has good heat conduction characteristic, and when the heat conductivity of the electrode layer is far greater than that of the substrate material, the temperature gradient distribution in the freezing process can be obviously changed, so that the crystal ice is regulated to grow in an orientation mode perpendicular to the arrangement direction of the electrode; the grooves formed by the electrode material microstructures protruding from the surface of the interdigital electrode can also be conveniently controlled in thickness and the freezing process thereof, and the temperature gradient in the preparation process can also be regulated, so that the three-dimensional junctions which are vertical to the electrode orientation arrangement and have the thickness of 6 mu m can be constructedAnd (5) forming. The interdigital electrode is mainly prepared by thick film technology, DPC technology or MEMS technology and the like. The substrate is PET, PDMS, PI or Al 2 O 3 。
Preferably, the finger length of the interdigital electrode is 2-20 mm, and the number of pairs of interdigital electrodes is 5-20. The interdigital electrode has the external dimension of (5-10) mm x (10-12) mm.
Preferably, the metal layer structure of the interdigital electrode is Cu/Ni/Au, ag or Pt.
Preferably, the thicknesses of the Cu/Ni/Au metal layer structure Cu, ni and Au are 2-20 μm, 0.2-5.0 μm and 0.2-5.0 μm in sequence.
The technical scheme adopted for further solving the technical problems is as follows: the preparation method of the interdigital electrode material with the vertical orientation three-dimensional structure comprises the steps of coating the nano material dispersion liquid in the grooves of the interdigital electrode, freezing, and freeze-drying.
Preferably, the concentration of the nanomaterial dispersion is 0.5 to 20mg/mL (more preferably 3 to 15 mg/mL). The concentration of the dispersion directly affects the viscosity of the dispersion and thus the coating thickness; if the concentration is too low, the thickness of the resultant coating layer is too thin and is easily broken to form a continuous three-dimensional structure, and if the concentration is too high, the viscosity is too high to facilitate coating.
Preferably, the preparation method of the nano material dispersion liquid comprises the following steps: adding the nano material into water, and performing ultrasonic dispersion to obtain the nano material.
Preferably, the ultrasonic dispersion has a frequency of 20 to 60kHz, a power of 100 to 1500W (more preferably 200 to 1000W) and a time of 0.1 to 2.0h. If the dispersibility of the nano material is good, the shape of the electrode material after directional freeze drying is better, and if the dispersibility is not good, the nano material can be agglomerated, so that the specific surface area is reduced, and the sensing performance of the gas sensor is further deteriorated. The longer the ultrasonic dispersion time is, the better the ultrasonic dispersion time is, the more favorable the nano material is to be uniformly dispersed in water, but the production efficiency needs to be considered at the same time.
Preferably, an antifreeze agent is added to the water in an amount of 3 to 8% by mass. The antifreezing agent can reduce the interaction between water molecules and electrode materials in the directional freezing process, and Kong Duowei of the freeze-dried nano material is provided with holes.
Preferably, the antifreeze is one or more of absolute ethyl alcohol, methanol or dimethyl sulfoxide and the like.
Preferably, the thickness of the nano material dispersion liquid coated to the interdigital electrode groove is more than or equal to 6 μm (more preferably 6 to 30 μm). The grooves between the fingers of the interdigitated electrodes retain the dispersion applied thereto. The thickness of the coating is largely determined by the thickness of the electrode layer and is also influenced by the viscosity of the solution, the higher the viscosity, the greater the thickness.
Preferably, the coating is knife coating, dip coating, spin coating, drop coating or the like.
Preferably, the height of the scraper blade for scraping and coating is 1-3 μm higher relative to the thickness of the interdigital electrode, and the moving speed is 3-50 cm/min. If the speed is too slow, time is wasted, and if the speed is too fast, the instrument parameters are limited and the blade coating is not uniform.
Preferably, the speed of immersing the interdigital electrode into the nanomaterial dispersion liquid in dip coating is 1-10 cm/s (more preferably 2-5 cm/s). The dip coating is to dip the interdigital electrode into liquid and take out the interdigital electrode, the surface of the interdigital electrode becomes hydrophilic after surface plasma treatment, and a coating layer is left on the surface after the interdigital electrode is dipped into the liquid.
Preferably, the spin coating speed is 500 to 3000r/min (more preferably 1000 to 2000 r/min) and the time is 30 to 180s (more preferably 40 to 100 s). The spin coating can utilize centrifugal force to spin out liquid above the electrode layer and keep uniform coating; if the speed is too slow or the time is too short, the liquid is thicker, and if the speed is too fast or the time is too long, the liquid is thinner.
Preferably, the nanomaterial dispersion is pre-cooled to 0 to 10 ℃ (more preferably 2 to 4 ℃) prior to coating. The purpose of precooling is to regulate the water crystallization speed and further regulate the aperture, and if the crystallization speed is too high, the crystal nucleus is more and the aperture is more and smaller.
Preferably, the interdigital electrode is pretreated before use: and (3) placing the interdigital electrode in absolute ethyl alcohol, carrying out ultrasonic cleaning, carrying out vacuum drying, and carrying out surface plasma cleaning. The ultrasonic cleaning can clean dust and other substances adhered to the surface of the electrode, and the plasma cleaning can etch away organic substances adhered to the surface, improve the hydrophilic and hydrophobic properties of the substrate and change the surface from a hydrophobic state to a hydrophilic state.
Preferably, the frequency of the ultrasonic cleaning is 20-60 kHz, the power is 100-1500W, and the time is 2-5 min.
Preferably, the temperature of the vacuum drying is 30-90 ℃, the vacuum degree is 0-minus 0.1MPa, and the time is 10-30 min. The vacuum degree is 0, and no vacuum pumping is performed. Drying the water remained on the surface after ultrasonic cleaning by vacuum drying.
Preferably, the power of the surface plasma cleaning is 5-30W, and the time is 5-30 min (more preferably 15-25 min).
Preferably, before coating, the interdigital electrode is soaked in liquid nitrogen for 3-7 min.
Preferably, the freezing mode is one-way freezing or two-way freezing. More preferably, unidirectional freezing. The cold source for freezing is a metal block or a cooling table pre-cooled by liquid nitrogen or low-temperature ethanol, or a cooling table with a circulating cooling device, and the like, and the cooling table with the circulating cooling device is more preferable. The manner of the metal block pre-cooled by the liquid nitrogen is to soak the metal block in the liquid nitrogen for 3 to 7min. During the freezing process, the solvent (water) of the nano material dispersion liquid is crystallized, the nano material is discharged by the ice crystal, and then the ice crystal is removed after freeze drying, namely the original position of the ice crystal is changed into a hole, so that the porous nano material with the vertically oriented three-dimensional structure and taking the ice crystal as a template is obtained.
Preferably, the freezing temperature is-20 to-198 ℃ (more preferably-30 to-198 ℃) and the time is 0.5 to 5.0min. The freezing temperature is lower than the freezing point of water, and the lower the freezing temperature, the smaller the size of ice crystals, and it is possible to obtain better gas sensing performance.
Preferably, the interdigital electrodes are frozen by placing them on a wedge-shaped block having a slope of 5 to 30 ° (more preferably 10 to 15 °), wherein the direction of the slope is perpendicular to the inter-interdigital direction of the interdigital electrodes. And a unidirectional temperature gradient is added, so that the orientation degree of ice crystal crystallization in the crystallization process can be improved.
Preferably, the temperature of the freeze-drying cold trap is less than or equal to-50 ℃ (more preferably less than or equal to-58 ℃), the vacuum degree is less than or equal to 60Pa (more preferably less than or equal to 15 Pa), and the time is 0.5-4.0 h. The ice crystals change directly from solid to gaseous state during freeze-drying and maintain the pore structure without collapsing. The lower the cold trap temperature, the higher the vacuum, and the faster and more time-saving the drying process.
The technical scheme adopted by the invention for further solving the technical problems is as follows: the application of the interdigital electrode material with the vertically-oriented three-dimensional structure to a sensor.
Preferably, the oxidized nano material is applied after reduction treatment.
Preferably, the specific operations of the reduction treatment are: and (3) placing the interdigital electrode material with the vertical orientation three-dimensional structure prepared on the basis of the graphene oxide nano material in hydrazine hydrate steam for reduction. The mass fraction of the hydrazine hydrate is more than or equal to 60 percent, and the hydrazine hydrate exists in the reducing atmosphere. In the reduction process, oxygen-containing functional groups of the graphene oxide lamella are reduced, defects are reduced, the resistance value is reduced, and an instrument can measure electrical signals conveniently.
Preferably, the temperature of the reduction is 80 to 100 ℃ (more preferably 85 to 95 ℃) and the time is 2 to 24 hours (more preferably 15 to 20 hours). The purpose of reduction is to adjust the resistance value to an appropriate range, typically around 10k Ω.
The invention has the following beneficial effects:
(1) The interdigital electrode material with the vertical orientation three-dimensional structure has wide raw material source, the thickness of the nanometer material layer is as low as 6 mu m, the composite state of the nanometer material is adjustable, and the gas sensing response degree is 4-19 times that of the interdigital electrode material which is randomly stacked by the nanometer material;
(2) The method has simple process and low cost, and is suitable for industrial production;
(3) The interdigital electrode material with the vertical orientation three-dimensional structure can contain various nano material systems, including zero-dimensional quantum dots, nano particles, one-dimensional nano tubes, nano rods, nano wires and the like, two-dimensional nano sheet layers and the like, has a wide application range, can be used for preparing gas sensors for detecting different target gases with quick response, flexibility and high sensitivity by changing the types of nano materials, and has a good application prospect in the field of environmental monitoring and treatment.
Drawings
FIG. 1 is an SEM image of an interdigital carboxylated carbon nanotube sheet of an interdigital electrode material having a vertically-oriented three-dimensional structure according to example 3 of the present invention;
FIG. 2 is a metallographic microscope photograph of an interdigital electrode material (multilayer graphene oxide) having a vertically-oriented three-dimensional structure according to example 4 of the present invention;
FIG. 3 is a graph comparing the degree of change in conductivity at 50 ℃ for 10ppm nitrogen dioxide for example 3 of the present invention and comparative example 1;
FIG. 4 is a graph comparing the degree of change in conductivity at 50 ℃ for 10ppm nitrogen dioxide for example 6 of the present invention and comparative example 2.
Detailed Description
The invention is further illustrated by the following examples and figures.
The PET interdigital electrode used in the embodiment of the invention has the external dimension of 5mm + 10mm, the MEMS process is commercially available, the PDMS interdigital electrode has the external dimension of 10mm + 12mm, the thick film process is commercially available, the PI interdigital electrode has the external dimension of 5mm + 10mm, the MEMS process is commercially available, the aluminum oxide interdigital electrode has the external dimension of 6mm + 12mm, the MEMS process is commercially available; the used graphene oxide quantum dot powder is a single layer, the diameter of a lamella is 5nm, and the graphene oxide quantum dot powder is purchased from Xianfeng nanometer; the used zinc oxide nano-particles with the particle size of 50nm are purchased from Xianfeng nano-particles; the length of the used carboxylated carbon nanotube is 2-10 mu m, the diameter is more than or equal to 50nm, and the carboxylated carbon nanotube is purchased from Xianfeng nanometer; the number of layers of the used multilayer graphene oxide powder is 1-6, the diameter of a sheet layer is 5 mu m, and the multilayer graphene oxide powder is purchased from Xianfeng nanometer; the sheet diameter size of the used single-layer graphene oxide powder is more than or equal to 500nm and is purchased from Heizhou element VI; the mass fraction of hydrazine hydrate used is 80%; the starting materials or chemicals used in the examples of the present invention were obtained by conventional commercial methods unless otherwise specified.
The detection method of each parameter in this embodiment is as follows: orientation included angle: the included angle between the arranged three-dimensional structure and the orientation of the electrode is obtained by photographing through a scanning electron microscope, measuring by using a protractor and calculating, wherein the value tends to 90 degrees, and the value represents that the vertical orientation degree is higher; calculating the thickness, spacing and height of the lamella: the scanning electron microscope is used for photographing, and then the width, the interval and the height are counted by software according to a photo ruler.
Reference example 1
The pretreatment method of the interdigital electrode comprises the following steps: the PET, PDMS, PI and aluminum oxide interdigital electrodes used in the embodiment of the invention are respectively placed in absolute ethyl alcohol, ultrasonic cleaning is carried out for 2min under the frequency of 28kHz and the power of 500W, vacuum drying is carried out for 30min under the temperature of 60 ℃ and the vacuum degree of-0.1 MPa, and surface plasma cleaning is carried out for 15min under the power of 15W, so that the surface plasma cleaning device is obtained.
Interdigital electrode material having vertically oriented three-dimensional Structure example 1
The interdigital electrode material with the vertical orientation three-dimensional structure is formed by compounding graphene oxide quantum dot lamellar structures stacked by graphene oxide quantum dots, wherein the graphene oxide quantum dot lamellar structures are arranged between the interdigital electrodes of the PET at intervals in a near vertical orientation mode; the thickness of the graphene oxide quantum dot material layer formed by the graphene oxide quantum dot sheet layer structure is 15 micrometers, the width of the graphene oxide quantum dot material layer is 55 micrometers, the orientation included angle of the nearly vertically oriented single sheet layers is 75 degrees, the vertical distance between the nearly vertically oriented single sheet layers is 10 micrometers, and the thickness of the single sheet layers is 0.5 micrometers; the thermal conductivity of the electrode layer material of the PET interdigital electrode is 75 W.m -1 ·K -1 The PET substrate has a flat surface and a thermal conductivity of 0.3 W.m -1 ·K -1 The thickness of an electrode layer of the PET interdigital electrode is 15.5 mu m, the line width is 45 mu m, and the line distance is 55 mu m; the finger length of the PET interdigital electrode is 3.3mm, the interdigital pair number is 15 pairs, the metal layer structure is Cu/Ni/Au, and the thicknesses of Cu, ni and Au are 13 mu m, 1.5 mu m and 1 mu m in sequence.
Through detection, the graphene oxide quantum dots in the interdigital electrode material with the vertical orientation three-dimensional structure in the embodiment of the invention show orientation arrangement after directional freeze drying, the width is 55 μm, the orientation included angle of the nearly vertical orientation monolithic layer is 75 degrees, the vertical distance between the nearly vertical orientation monolithic layers is 10 μm, and the thickness of the monolithic layer is 0.5 μm.
Preparation of interdigitated electrode Material with Vertically oriented three-dimensional Structure example 1
Coating a graphene oxide quantum dot powder dispersion liquid with the concentration of 4mg/mL in a groove of a PET interdigital electrode pretreated in reference example 1 at the height of a scraper which is 1 μm higher than the thickness of the PET interdigital electrode and the moving speed of 40cm/min until the thickness of the graphene oxide quantum dot powder dispersion liquid is 15 μm, placing the graphene oxide quantum dot powder dispersion liquid on a cooling table (4 cm x 2cm) cooled by ethanol at the temperature of-30 ℃, performing unidirectional freezing for 2min, and performing freeze drying for 4h at the temperature of-58 ℃ and the vacuum degree of 5Pa to obtain the graphene oxide quantum dot powder dispersion liquid; the preparation method of the graphene oxide quantum dot powder dispersion liquid comprises the following steps: and adding 200mg of graphene oxide quantum dot powder into 50mL of water, and performing ultrasonic dispersion for 1h under the frequency of 20kHz and the power of 500W to obtain the graphene oxide quantum dot powder.
Interdigital electrode material having vertically oriented three-dimensional Structure example 2
The interdigital electrode material with the vertical orientation three-dimensional structure is formed by compounding zinc oxide nano-particle lamellar structures stacked by zinc oxide nano-particles, wherein the zinc oxide nano-particle lamellar structures are arranged between the interdigital of the PET interdigital electrodes at intervals in a near-vertical orientation manner; the thickness of a zinc oxide nano material layer formed by the zinc oxide nano particle lamellar structure is 15 micrometers, the width of the zinc oxide nano material layer is 55 micrometers, the orientation included angle of the nearly vertically oriented single-chip layers is 75 degrees, the vertical distance between the nearly vertically oriented single-chip layers is 4 micrometers, and the thickness of the single-chip layer is 0.3 micrometer; the thermal conductivity of the electrode layer material of the PET interdigital electrode is 75 W.m -1 ·K -1 The PET substrate has a flat surface and a thermal conductivity of 0.3 W.m -1 ·K -1 The thickness of an electrode layer of the PET interdigital electrode is 15.5 mu m, the line width is 100 mu m, and the line distance is 55 mu m; the finger length of the PET interdigital electrode is 3.3mm, the interdigital pair number is 15 pairs, the metal layer structure is Cu/Ni/Au, and the thicknesses of Cu, ni and Au are 13 mu m, 1.5 mu m and 1 mu m in sequence.
Through detection, the zinc oxide nanoparticles in the interdigital electrode material with the vertical orientation three-dimensional structure in the embodiment of the invention are oriented and arranged after being subjected to directional freeze drying, the width is 55 microns, the orientation included angle of the nearly vertical orientation single-chip layer is 75 degrees, the vertical distance between the nearly vertical orientation single-chip layers is 4 microns, and the thickness of the single-chip layer is 0.3 micron.
Preparation of interdigitated electrode Material with Vertically oriented three-dimensional Structure example 2
Coating zinc oxide nanoparticle dispersion liquid with the concentration of 3mg/mL in a groove of a PET interdigital electrode pretreated in reference example 1 at the height of a scraper which is 1 μm higher than the thickness of the PET interdigital electrode and the moving speed of 20cm/min until the thickness of graphene oxide quantum dot powder dispersion liquid is 15 μm, placing the dispersion liquid on a cooling table (4 cm x 2cm) cooled by liquid nitrogen circulation, performing unidirectional freezing for 1min, and performing freeze drying for 3h at-78 ℃ and the vacuum degree of 10Pa to obtain the graphene oxide quantum dot powder dispersion liquid; the preparation method of the zinc oxide nanoparticle dispersion liquid comprises the following steps: adding 150mg of zinc oxide nano particles into 50mL of water, and performing ultrasonic dispersion for 0.5h at the frequency of 40kHz and the power of 200W to obtain the zinc oxide nano particles.
Interdigitated electrode material with vertically oriented three-dimensional structure example 3
The interdigital electrode material with the vertical orientation three-dimensional structure is formed by compounding a carboxylated carbon nano tube laminated structure formed by stacking carboxylated carbon nano tubes, wherein the laminated structure is arranged between the interdigital of the PET interdigital electrodes at intervals in a nearly vertical orientation manner; the thickness of a carboxylated carbon nanotube material layer formed by the carboxylated carbon nanotube lamellar structure is 15 micrometers, the width of the carboxylated carbon nanotube material layer is 55 micrometers, the orientation included angle of the nearly vertically oriented single-chip layers is 75 degrees, the vertical distance between the nearly vertically oriented single-chip layers is 3 micrometers, and the thickness of the single-chip layers is 0.5 micrometers; the thermal conductivity of the electrode layer material of the PET interdigital electrode is 75 W.m -1 ·K -1 The PET substrate has a flat surface and a thermal conductivity of 0.3 W.m -1 ·K -1 The thickness of an electrode layer of the PET interdigital electrode is 15.5 mu m, the line width is 45 mu m, and the line distance is 55 mu m; the finger length of the PET interdigital electrode is 3.3mm, the interdigital pair number is 15 pairs, the metal layer structure is Cu/Ni/Au, and the thicknesses of Cu, ni and Au are 13 mu m, 1.5 mu m and 1 mu m in sequence.
As shown in FIG. 1, the carboxylated carbon nanotubes in the interdigital electrode material with a vertically-oriented three-dimensional structure according to the embodiment of the present invention exhibit an oriented arrangement after being subjected to directional freeze-drying, the width is 55 μm, the orientation included angle of the nearly vertically-oriented monolithic layers is 75 °, the vertical distance between the nearly vertically-oriented monolithic layers is 3 μm, and the thickness of the monolithic layers is 0.5 μm.
Preparation of interdigitated electrode Material with Vertically oriented three-dimensional Structure example 3
Coating a carboxylated carbon nanotube dispersion liquid with the concentration of 5mg/mL in the groove of the PET interdigital electrode pretreated in the reference example 1 at the height of a scraper which is 1 μm higher than the thickness of the PET interdigital electrode and the moving speed of 40cm/min till the thickness of the graphene oxide quantum dot powder dispersion liquid is 15 μm, placing the graphene oxide quantum dot powder dispersion liquid on a cooling table (4 cm x 4cm 2cm) cooled by ethanol at the temperature of minus 30 ℃, performing unidirectional freezing for 2min, and performing freeze drying for 4h at the temperature of minus 58 ℃ and the vacuum degree of 5Pa to obtain the graphene oxide quantum dot powder dispersion liquid; the preparation method of the carboxylated carbon nanotube dispersion liquid comprises the following steps: adding 250mg of carboxylated carbon nanotubes into 50mL of water, and performing ultrasonic dispersion for 1h at the frequency of 40kHz and the power of 500W to obtain the nano-carbon composite material.
Interdigitated electrode material with vertically oriented three-dimensional structure example 4
The interdigital electrode material with the vertical orientation three-dimensional structure is formed by compounding a plurality of layers of graphene oxide powder laminated structures stacked by a plurality of layers of graphene oxide powder and arranged between the interdigital electrodes of PDMS at intervals in a near vertical orientation manner; the thickness of a multilayer graphene oxide powder material layer formed by the multilayer graphene oxide powder lamellar structure is 25 micrometers, the width of the multilayer graphene oxide powder material layer is 200 micrometers, the orientation included angle of the nearly-vertically-oriented single-layer layers is 75 degrees, the vertical distance between the nearly-vertically-oriented single-layer layers is 12 micrometers, and the thickness of the single-layer is 0.5 micrometer; the thermal conductivity of the electrode layer material of the PDMS interdigital electrode is 100 W.m -1 ·K -1 The PDMS substrate has a flat surface and a thermal conductivity of 0.2 W.m -1 ·K -1 The thickness of an electrode layer of the PDMS interdigital electrode is 50 μm, the line width is 45 μm, and the line distance is 200 μm; the PDMS interdigital electrode has the finger length of 10mm, the number of pairs of interdigital electrodes is 15, the metal layer structure is Ag, and the thickness is 25 μm.
As shown in fig. 2, the multilayer graphene oxide powder in the interdigital electrode material with a vertically-oriented three-dimensional structure according to the embodiment of the present invention exhibits an oriented arrangement after directional freeze-drying, the width is 200 μm, the orientation included angle of the nearly vertically-oriented monolithic layers is 75 °, the vertical distance between the nearly vertically-oriented monolithic layers is 12 μm, and the thickness of the monolithic layer is 0.5 μm.
Preparation of interdigitated electrode Material with Vertically oriented three-dimensional Structure example 4
Carrying out blade coating on 12mg/mL multilayer graphene oxide powder dispersion liquid in a groove of a PDMS interdigital electrode pretreated in reference example 1 at a moving speed of 40cm/min and a scraper height of 3 μm higher than the thickness of the PDMS interdigital electrode, placing the multilayer graphene oxide powder dispersion liquid with a thickness of 25 μm on a cooling table (4 cm x 4cm 2cm) cooled by ethanol at-30 ℃, carrying out unidirectional freezing for 2min, and carrying out freeze drying for 4h at-58 ℃ and a vacuum degree of 5Pa to obtain the final product; the preparation method of the multilayer graphene oxide powder dispersion liquid comprises the following steps: adding 600mg of multilayer graphene oxide powder into 50mL of water, and performing ultrasonic dispersion for 1h at the frequency of 40kHz and the power of 300W to obtain the graphene oxide powder.
Interdigitated electrode material with vertically oriented three-dimensional Structure example 5
The interdigital electrode material with the vertical orientation three-dimensional structure is formed by compounding a single-layer graphene oxide powder laminated structure formed by stacking single-layer graphene oxide powder, wherein the single-layer graphene oxide powder laminated structure is arranged between the interdigital of the PET interdigital electrode at intervals in a near vertical orientation mode; the thickness of a single-layer graphene oxide powder material layer formed by the single-layer graphene oxide powder lamellar structure is 10 micrometers, the width of the single-layer graphene oxide powder material layer is 200 micrometers, the orientation included angle of the nearly-vertically-oriented single-layer layers is 75 degrees, the vertical distance between the nearly-vertically-oriented single-layer layers is 7 micrometers, and the thickness of the single-layer layers is 0.4 micrometer; the thermal conductivity of the electrode layer material of the PET interdigital electrode is 100 W.m -1 ·K -1 The PET substrate has a flat surface and a thermal conductivity of 0.3 W.m -1 ·K -1 The thickness of an electrode layer of the PET interdigital electrode is 15.5 mu m, the line width is 45 mu m, and the line distance is 55 mu m; the length of the PET interdigital electrode is 10mm, the number of pairs of interdigital electrodes is 15, the structure of the metal layer is Ag,the thickness was 25 μm.
Through detection, the single-layer graphene oxide powder in the interdigital electrode material with the vertical orientation three-dimensional structure in the embodiment of the invention is oriented and arranged after being subjected to directional freeze drying, the width is 200 μm, the orientation included angle of the nearly vertical orientation single-layer is 75 degrees, the vertical distance between the nearly vertical orientation single-layer is 7 μm, and the thickness of the single-layer is 0.4 μm.
Preparation of interdigitated electrode Material with Vertically oriented three-dimensional Structure example 5
Immersing the pretreated PET interdigital electrode in reference example 1 into a single-layer graphene oxide powder dispersion liquid with the concentration of 3mg/mL at the speed of 3cm/s, dip-coating the single-layer graphene oxide powder dispersion liquid into a groove of the PET interdigital electrode till the thickness of the single-layer graphene oxide powder dispersion liquid is 10 micrometers, performing unidirectional freezing on a copper block of 4cm 2cm soaked for 5min by liquid nitrogen, and freeze-drying for 2h at the temperature of minus 78 ℃ and the vacuum degree of 15Pa to obtain the PET interdigital electrode; the preparation method of the single-layer graphene oxide powder dispersion liquid comprises the following steps: and adding 150mg of single-layer graphene oxide powder into a mixed solution of 50mL of water and 1.5g of dimethyl sulfoxide, and performing ultrasonic dispersion for 1.5h at the frequency of 60kHz and the power of 200W to obtain the graphene oxide powder.
Interdigitated electrode material having vertically oriented three-dimensional Structure example 6
The interdigital electrode material with the vertical orientation three-dimensional structure is formed by compounding a single-layer graphene oxide powder laminated structure formed by stacking single-layer graphene oxide powder, wherein the single-layer graphene oxide powder laminated structure is arranged between the interdigital of the PET interdigital electrode at intervals in a near vertical orientation mode; the thickness of a single-layer graphene oxide powder material layer formed by the single-layer graphene oxide powder lamellar structure is 6 micrometers, the width of the single-layer graphene oxide powder material layer is 200 micrometers, the orientation included angle of the nearly-vertically-oriented single-layer layers is 75 degrees, the vertical distance between the nearly-vertically-oriented single-layer layers is 12 micrometers, and the thickness of the single-layer is 0.5 micrometer; the thermal conductivity of the electrode layer material of the PET interdigital electrode is 100 W.m -1 ·K -1 The PET substrate has a flat surface and a thermal conductivity of 0.3 W.m -1 ·K -1 The thickness of an electrode layer of the PET interdigital electrode is 15.5 mu m, the line width is 45 mu m, and the line distance is 200 mu m; the finger length of the PET interdigital electrode is 10mm, and the number of pairs of interdigital electrodes is 15The metal layer structure is Ag, and the thickness is 25 μm.
Through detection, the single-layer graphene oxide powder in the interdigital electrode material with the vertical orientation three-dimensional structure in the embodiment of the invention presents orientation arrangement after directional freeze drying, the width is 200 μm, the orientation included angle of the nearly vertical orientation single-layer is 75 degrees, the vertical distance between the nearly vertical orientation single-layer layers is 12 μm, and the thickness of the single-layer is 0.5 μm.
Preparation of interdigitated electrode Material with Vertically oriented three-dimensional Structure example 6
Spin-coating a monolayer graphene oxide powder dispersion liquid with the concentration of 3mg/mL in surface grooves of the pretreated PET interdigital electrodes in the reference example 1 at the speed of 1200r/min for 45s by using a desktop spin coater till the thickness of the monolayer graphene oxide powder dispersion liquid is 6 microns, soaking the monolayer graphene oxide powder dispersion liquid on a copper block of 4cm x 2cm for 5min in liquid nitrogen, performing unidirectional freezing for 2min, and performing freeze drying for 4h at the temperature of minus 58 ℃ and the vacuum degree of 5Pa to obtain the graphene oxide powder dispersion liquid; the preparation method of the single-layer graphene oxide powder dispersion liquid comprises the following steps: and adding 150mg of single-layer graphene oxide powder into 50mL of water, and performing ultrasonic dispersion for 1h at the frequency of 40kHz and the power of 500W to obtain the graphene oxide powder.
Interdigitated electrode material with vertically oriented three-dimensional Structure example 7
The interdigital electrode material with the vertical orientation three-dimensional structure is formed by compounding a single-layer graphene oxide powder laminated structure formed by stacking single-layer graphene oxide powder, wherein the single-layer graphene oxide powder laminated structure is arranged between the interdigital of the PET interdigital electrode at intervals in a near vertical orientation mode; the thickness of a single-layer graphene oxide powder material layer formed by the single-layer graphene oxide powder lamellar structure is 15 micrometers, the width of the single-layer graphene oxide powder material layer is 200 micrometers, the orientation included angle of the nearly-vertically-oriented single lamellar layer is 70 degrees, the vertical distance between the nearly-vertically-oriented single lamellar layers is 9 micrometers, and the thickness of the single lamellar layer is 0.5 micrometer; the thermal conductivity of the electrode layer material of the PET interdigital electrode is 100 W.m -1 ·K -1 The PET substrate has a flat surface and a thermal conductivity of 0.3 W.m -1 ·K -1 The thickness of an electrode layer of the PET interdigital electrode is 15.5 mu m, the line width is 100 mu m, and the line distance is 100 mu m; the finger length of the PET interdigital electrode is 10mm, the interdigital number is 15 pairs,the metal layer structure is Ag, and the thickness is 25 μm.
Through detection, the single-layer graphene oxide powder in the interdigital electrode material with the vertical orientation three-dimensional structure in the embodiment of the invention presents orientation arrangement after directional freeze drying, the width is 200 μm, the orientation included angle of the nearly vertical orientation single-layer is 70 degrees, the vertical distance between the nearly vertical orientation single-layer layers is 9 μm, and the thickness of the single-layer is 0.5 μm.
Preparation of interdigitated electrode Material with Vertically oriented three-dimensional Structure example 7
Pre-cooling a single-layer graphene oxide powder dispersion liquid with the temperature of 2 ℃ and the concentration of 3mg/mL, under the conditions that the height of a scraper is 1 mu m higher than the thickness of a PET interdigital electrode and the moving speed is 30cm/min, blade-coating the single-layer graphene oxide powder dispersion liquid in a groove of the PET interdigital electrode (the PET interdigital electrode is soaked in liquid nitrogen for 3min before dip-coating) pretreated in the reference example 1 until the thickness of the single-layer graphene oxide powder dispersion liquid is 15 mu m, pressing a copper block of 4cm 2cm soaked in liquid nitrogen for 5min on a pin of the interdigital electrode, performing unidirectional freezing for 3min, and then performing freeze-drying for 4h at the temperature of minus 78 ℃ and the vacuum degree of 5Pa to obtain the single-layer graphene oxide powder dispersion liquid; the preparation method of the single-layer graphene oxide powder dispersion liquid comprises the following steps: adding 150mg of single-layer graphene oxide powder into 50mL of water, and performing ultrasonic dispersion for 2 hours under the frequency of 20kHz and the power of 400W to obtain the graphene oxide powder.
Interdigital electrode material having vertically oriented three-dimensional Structure example 8
The interdigital electrode material with the vertical orientation three-dimensional structure is formed by compounding a single-layer graphene oxide powder laminated structure formed by stacking single-layer graphene oxide powder, wherein the single-layer graphene oxide powder laminated structure is arranged between the interdigital of the PET interdigital electrodes at intervals in a nearly vertical orientation manner; the thickness of a single-layer graphene oxide powder material layer formed by the single-layer graphene oxide powder lamellar structure is 15 micrometers, the width of the single-layer graphene oxide powder material layer is 200 micrometers, the orientation included angle of the nearly-vertically-oriented single lamellar layer is 83 degrees, the vertical distance between the nearly-vertically-oriented single lamellar layers is 10 micrometers, and the thickness of the single lamellar layer is 0.5 micrometer; the thermal conductivity of the electrode layer material of the PET interdigital electrode is 100 W.m -1 ·K -1 The PET substrate has a flat surface and a thermal conductivity of 0.3 W.m -1 ·K -1 Electric of interdigitated electrodes of PETThe thickness of the electrode layer is 15.5 μm, the line width is 45 μm, and the line distance is 55 μm; the length of the PET interdigital electrode is 10mm, the number of pairs of interdigital electrodes is 15, the metal layer structure is Ag, and the thickness is 25 mu m.
Through detection, the single-layer graphene oxide powder in the interdigital electrode material with the vertical orientation three-dimensional structure in the embodiment of the invention presents orientation arrangement after directional freeze drying, the width is 200 μm, the orientation included angle of the nearly vertical orientation single-layer is 83 degrees, the vertical distance between the nearly vertical orientation single-layer layers is 10 μm, and the thickness of the single-layer is 0.5 μm.
Preparation of interdigitated electrode Material with A Vertically oriented three-dimensional Structure example 8
Coating a monolayer graphene oxide powder dispersion liquid with the concentration of 3mg/mL in a groove of a PET interdigital electrode pretreated in reference example 1 at the height of a scraper which is 1 μm higher than the thickness of the PET interdigital electrode and the moving speed of 40cm/min until the thickness of the monolayer graphene oxide powder dispersion liquid is 15 μm, placing the monolayer graphene oxide powder dispersion liquid on a PDMS wedge block which is placed on a copper block (4 cm x 2 cm) soaked for 5min by liquid nitrogen and has the gradient of 10 degrees (the gradient direction is vertical to the inter-finger direction of the interdigital electrode), performing unidirectional freezing for 2min, and then performing freeze drying for 1h at the temperature of-58 ℃ and the vacuum degree of 5Pa to obtain the PET interdigital electrode dispersion liquid; the preparation method of the single-layer graphene oxide powder dispersion liquid comprises the following steps: and adding 150mg of single-layer graphene oxide powder into 50mL of water, and performing ultrasonic dispersion for 1h at the frequency of 40kHz and the power of 500W to obtain the graphene oxide powder.
Interdigitated electrode material having vertically oriented three-dimensional Structure example 9
The interdigital electrode material with the vertical orientation three-dimensional structure is formed by compounding a single-layer graphene oxide powder laminated structure formed by stacking single-layer graphene oxide powder and arranging the single-layer graphene oxide powder laminated structure between the interdigital of the PI interdigital electrode at intervals in a near-vertical orientation mode; the thickness of a single-layer graphene oxide powder material layer formed by the single-layer graphene oxide powder lamellar structure is 16 micrometers, the width of the single-layer graphene oxide powder material layer is 200 micrometers, the orientation included angle of the nearly-vertically-oriented single lamellar layer is 70 degrees, the vertical distance between the nearly-vertically-oriented single lamellar layers is 8 micrometers, and the thickness of the single lamellar layer is 0.4 micrometers; the thermal conductivity of the electrode layer material of the PI interdigital electrode is 75 W.m -1 ·K -1 The PI substrate has a flat surface and a thermal conductivity of 0.3 W.m -1 ·K -1 The thickness of an electrode layer of the PI interdigital electrode is 15.5 mu m, the line width is 45 mu m, and the line distance is 55 mu m; the length of the PI interdigital electrode is 10mm, the number of pairs of interdigital electrodes is 15, the metal layer structure is Cu/Ni/Au, and the thicknesses of Cu, ni and Au are 12 micrometers, 3 micrometers and 1 micrometer in sequence.
Through detection, the single-layer graphene oxide powder in the interdigital electrode material with the vertical orientation three-dimensional structure in the embodiment of the invention presents orientation arrangement after directional freeze drying, the width is 200 μm, the orientation included angle of the nearly vertical orientation single-layer is 70 degrees, the vertical distance between the nearly vertical orientation single-layer layers is 8 μm, and the thickness of the single-layer is 0.4 μm.
Preparation of interdigitated electrode Material with Vertically oriented three-dimensional Structure example 9
Coating a monolayer graphene oxide powder dispersion liquid with the concentration of 3mg/mL in a groove of a PI interdigital electrode pretreated in reference example 1 at the height of a scraper which is 2 micrometers higher than the thickness of the PI interdigital electrode and the moving speed of 40cm/min until the thickness of the monolayer graphene oxide powder dispersion liquid is 16 micrometers, pressing a copper block of 4cm x 2cm soaked for 5min by liquid nitrogen on a pin of the interdigital electrode, performing unidirectional freezing for 5min, and performing freeze drying for 4h at the temperature of-58 ℃ and the vacuum degree of 10Pa to obtain the graphene oxide powder dispersion liquid; the preparation method of the single-layer graphene oxide powder dispersion liquid comprises the following steps: and adding 150mg of single-layer graphene oxide powder into a mixed solution of 50mL of water and 2.5g of absolute ethyl alcohol, and performing ultrasonic dispersion for 1h at the frequency of 40kHz and the power of 500W to obtain the graphene oxide powder.
Example 10 interdigital electrode Material having a Vertically oriented three-dimensional Structure
The interdigital electrode material with the vertical orientation three-dimensional structure is formed by compounding a single-layer graphene oxide powder laminated structure formed by stacking single-layer graphene oxide powder and arranging the single-layer graphene oxide powder laminated structure between the interdigital of the aluminum oxide interdigital electrode at intervals in a near-vertical orientation mode; the thickness of a single-layer graphene oxide powder material layer formed by the single-layer graphene oxide powder lamellar structure is 18 micrometers, the width of the single-layer graphene oxide powder material layer is 200 micrometers, the orientation included angle of the nearly-vertically-oriented single lamellar layer is 73 degrees, and the nearly-vertically-oriented single lamellar layerThe vertical distance between the sheet layers is 8 μm, and the thickness of the single sheet layer is 0.4 μm; the thermal conductivity of the electrode layer material of the aluminum oxide interdigital electrode is 75 W.m -1 ·K -1 The surface of the aluminum oxide base is flat and the thermal conductivity is 3 W.m -1 ·K -1 The thickness of an electrode layer of the aluminum oxide interdigital electrode is 15.5 mu m, the line width is 45 mu m, and the line distance is 55 mu m; the finger length of the aluminum oxide interdigital electrode is 10mm, the interdigital pair number is 15 pairs, the metal layer structure is Cu/Ni/Au, and the thicknesses of Cu, ni and Au are 12 micrometers, 3 micrometers and 1 micrometer in sequence.
Through detection, the single-layer graphene oxide powder in the interdigital electrode material with the vertical orientation three-dimensional structure in the embodiment of the invention presents orientation arrangement after directional freeze drying, the width is 200 μm, the orientation included angle of the nearly vertical orientation single-layer is 73 degrees, the vertical distance between the nearly vertical orientation single-layer layers is 8 μm, and the thickness of the single-layer is 0.4 μm.
Preparation of interdigitated electrode Material with Vertically oriented three-dimensional Structure example 10
Immersing the pre-treated aluminum oxide interdigital electrode in reference example 1 (before dip-coating, immersing the aluminum oxide interdigital electrode in liquid nitrogen for 5 min) into a monolayer graphene oxide powder dispersion liquid with the concentration of 3mg/mL and the pre-cooled temperature of 4 ℃ at the speed of 5cm/s, dip-coating the monolayer graphene oxide powder dispersion liquid into a groove of the aluminum oxide interdigital electrode until the thickness of the monolayer graphene oxide powder dispersion liquid is 18 mu m, placing the monolayer graphene oxide powder dispersion liquid on a cooling table (4 cm 2cm) cooled by ethanol at the temperature of-30 ℃, performing unidirectional freezing for 2min, and performing freeze drying for 4h at the temperature of-58 ℃ and the vacuum degree of 5Pa to obtain the aluminum oxide interdigital electrode; the preparation method of the single-layer graphene oxide powder dispersion liquid comprises the following steps: adding 150mg of single-layer graphene oxide powder into 50mL of water, and performing ultrasonic dispersion for 1h at the frequency of 40kHz and the power of 300W to obtain the graphene oxide powder.
Examples 2 and 3 of the use of interdigitated electrode materials with a vertically oriented three-dimensional structure
The interdigital electrode material examples 2 and 3 having a vertically-oriented three-dimensional structure are applied to gas sensing, respectively.
Application examples 1, 4 to 10 of interdigital electrode materials having a vertically oriented three-dimensional structure
The interdigital electrode materials of examples 1, 4 to 10 with the vertical orientation three-dimensional structure are respectively placed in hydrazine hydrate (the mass fraction of hydrazine hydrate is 80%) steam, and are applied to a gas sensor after being reduced for 20 hours at 90 ℃.
Comparative example 1
The carboxylated carbon nanotube dispersion liquid with the concentration of 5mg/mL is blade-coated in the groove of the PET interdigital electrode pretreated in the reference example 1 at the scraper height which is 1 μm higher than the thickness of the PET interdigital electrode and the moving speed of 40cm/min until the thickness of the graphene oxide quantum dot powder dispersion liquid is 15 μm, and the material is oven-dried for 0.5h at 50 ℃ to obtain the disordered-stacked carboxylated carbon nanotube interdigital electrode material.
Comparative example 2
The monolayer graphene oxide powder dispersion liquid with the concentration of 3mg/mL is coated in the surface groove of the PET interdigital electrode pretreated in the reference example 1 by a bench-type glue homogenizer for 45s at the temperature of 25 ℃ and the speed of 1200r/min until the thickness of the monolayer graphene oxide powder dispersion liquid is 6 mu m, and the monolayer graphene oxide powder interdigital electrode material stacked in disorder is obtained after drying in an oven for 0.5h at the temperature of 50 ℃.
The randomly stacked single-layer graphene oxide powder interdigital electrode material is placed in hydrazine hydrate (the mass fraction of the hydrazine hydrate is 80%) steam, and is applied to a gas sensor after being reduced for 20 hours at 90 ℃.
In order to evaluate the degree of response of the interdigital electrode materials with a vertically-oriented three-dimensional structure of the invention in gas sensor applications, examples 1 to 10 and comparative examples 1 and 2 were tested under the same environment for the response to 10ppm nitrogen dioxide, respectively, with the gas inlet time fixed at 600s, and the peak values of the relative change degrees of the electrical conductivity thereof were respectively detected.
Through detection, the peak values of the relative change degrees of the conductivities of the embodiments 1 to 10 are respectively 6.5%, 4%, 11.2%, 5.4%, 7.6%, 7.73%, 11%, 15%, 9.6% and 7.8%; the peak values of the conductivity ratios of comparative examples 1 and 2 are only 0.8% and 1%, respectively; as shown in fig. 3, the peak value of the relative change degree of the conductivity of example 3 corresponds to 14 times the peak value of the relative change degree of the conductivity of comparative example 1; as shown in fig. 4, the peak value of the conductivity ratio of example 6 corresponds to 7.73 times the peak value of the conductivity ratio of comparative example 2; compared with the interdigital electrode materials with the vertical orientation three-dimensional structure disclosed by the invention in the embodiments 1-10, the nano materials obtained by directly drying the comparative examples 1 and 2 are stacked in disorder in the interdigital electrode, so that the adsorption of the nano materials on target gas and the influence of gas concentration on the resistance of the interdigital electrode are greatly influenced, and the response degree and sensitivity of the interdigital electrode are influenced.
Claims (10)
1. An interdigital electrode material having a vertically-oriented three-dimensional structure, characterized in that: the nano-sheet structure is formed by stacking nano materials, is arranged between the fingers of the finger electrodes at intervals in a nearly vertical orientation mode, and is compounded; the form of the nano material is one or more of zero-dimensional quantum dots, nano particles, one-dimensional nanotubes, nano rods, nano wires or two-dimensional nano sheet layers; the thickness of the nano material layer formed by the nano sheet layer structure is more than or equal to 6 microns, the width of the nano material layer is 20-500 microns, the orientation included angle of the nearly vertically oriented single sheet layer is 60-90 degrees, the vertical distance between the nearly vertically oriented single sheet layers is 1-12 microns, and the thickness of the single sheet layer is 0.1-1.0 micron;
the preparation method of the interdigital electrode material with the vertical orientation three-dimensional structure comprises the steps of coating a nano material dispersion liquid in a groove of an interdigital electrode, freezing, and freeze-drying to obtain the interdigital electrode material; the freezing mode is unidirectional freezing or bidirectional freezing; the freezing temperature is-20 to-198 ℃, and the time is 0.5 to 5.0min; placing the interdigital electrode on a wedge-shaped block with the gradient of 5-30 degrees for freezing, wherein the gradient direction is vertical to the interdigital electrode inter-finger direction; the temperature of the freeze-drying cold trap is less than or equal to minus 50 ℃, the vacuum degree is less than or equal to 60Pa, and the time is 0.5 to 4.0 hours.
2. The interdigital electrode material having a vertically-oriented three-dimensional structure according to claim 1, wherein: the nano material is graphene oxide quantum dots, single-layer graphene oxide powder, multi-layer graphene oxide powder, carboxylated carbon nanotubes or oxidized grapheneOne or more of zinc nanoparticles; the thermal conductivity of the electrode layer material of the interdigital electrode is more than or equal to 50 W.m -1 ·K -1 The surface of the substrate is flat and the thermal conductivity is less than or equal to 5 W.m -1 ·K -1 The electrode layer thickness of the interdigital electrode is more than or equal to 10 mu m, the line width is 45-250 mu m, and the line distance is 20-500 mu m; the finger length of the interdigital electrode is 2-20 mm, and the number of interdigital pairs is 5-20 pairs; the metal layer structure of the interdigital electrode is Cu/Ni/Au, ag or Pt; the thicknesses of Cu, ni and Au in the Cu/Ni/Au metal layer structure are 2-20 μm, 0.2-5.0 μm and 0.2-5.0 μm in sequence.
3. The interdigital electrode material having a vertically-oriented three-dimensional structure according to claim 1 or 2, wherein: the concentration of the nano material dispersion liquid is 0.5-20 mg/mL; the preparation method of the nano material dispersion liquid comprises the following steps: adding the nano material into water, and performing ultrasonic dispersion to obtain the nano material; the frequency of the ultrasonic dispersion is 20-60 kHz, the power is 100-1500W, and the time is 0.1-2.0 h; adding an antifreezing agent which accounts for 3-8% of the mass of the mixture into water; the antifreezing agent is one or more of absolute ethyl alcohol, methanol or dimethyl sulfoxide.
4. The interdigital electrode material having a vertically-oriented three-dimensional structure according to claim 1 or 2, wherein: the thickness of the nano material dispersion liquid coated in the interdigital electrode groove is more than or equal to 6 microns; the coating is blade coating, dip coating, spin coating or drop coating; the height of the scraper blade for scraping and coating is 1-3 mu m higher than the thickness of the interdigital electrode, and the moving speed is 3-50 cm/min; during dip coating, the speed of immersing the interdigital electrode into the nano material dispersion liquid is 1-10 cm/s; the spin coating speed is 500-3000 r/min, and the time is 30-180 s; before coating, the nano material dispersion liquid is pre-cooled to 0-10 ℃.
5. The interdigital electrode material having a vertically-oriented three-dimensional structure according to claim 3, wherein: the thickness of the nano material dispersion liquid coated in the interdigital electrode groove is more than or equal to 6 microns; the coating is blade coating, dip coating, spin coating or drop coating; the height of the scraper blade for scraping and coating is 1-3 mu m higher than the thickness of the interdigital electrode, and the moving speed is 3-50 cm/min; during dip coating, the speed of immersing the interdigital electrode into the nano material dispersion liquid is 1-10 cm/s; the spin coating speed is 500-3000 r/min, and the time is 30-180 s; before coating, the nano material dispersion liquid is pre-cooled to 0-10 ℃.
6. The interdigital electrode material having a vertically-oriented three-dimensional structure according to claim 1 or 2, wherein: the interdigital electrode is pretreated before use: placing the interdigital electrode in absolute ethyl alcohol, carrying out ultrasonic cleaning, vacuum drying, and carrying out surface plasma cleaning; the ultrasonic cleaning frequency is 20-60 kHz, the power is 100-1500W, and the time is 2-5 min; the temperature of the vacuum drying is 30-90 ℃, the vacuum degree is 0-minus 0.1MPa, and the time is 10-30 min; the power for cleaning the surface plasma is 5-30W, and the time is 5-30 min; before coating, the interdigital electrode is soaked in liquid nitrogen for 3-7 min.
7. The interdigital electrode material having a vertically-oriented three-dimensional structure according to claim 3, wherein: the interdigital electrode is pretreated before use: placing the interdigital electrode in absolute ethyl alcohol, carrying out ultrasonic cleaning, vacuum drying, and carrying out surface plasma cleaning; the ultrasonic cleaning frequency is 20-60 kHz, the power is 100-1500W, and the time is 2-5 min; the temperature of the vacuum drying is 30-90 ℃, the vacuum degree is 0-minus 0.1MPa, and the time is 10-30 min; the power for cleaning the surface plasma is 5-30W, and the time is 5-30 min; before coating, the interdigital electrode is soaked in liquid nitrogen for 3-7 min.
8. The interdigital electrode material having a vertically-oriented three-dimensional structure according to claim 4, wherein: the interdigital electrode is pretreated before use: placing the interdigital electrode in absolute ethyl alcohol, carrying out ultrasonic cleaning, vacuum drying, and carrying out surface plasma cleaning; the frequency of the ultrasonic cleaning is 20-60 kHz, the power is 100-1500W, and the time is 2-5 min; the temperature of the vacuum drying is 30-90 ℃, the vacuum degree is 0-minus 0.1MPa, and the time is 10-30 min; the power for cleaning the surface plasma is 5-30W, and the time is 5-30 min; before coating, the interdigital electrode is soaked in liquid nitrogen for 3-7 min.
9. Use of an interdigitated electrode material with a vertically oriented three-dimensional structure according to any of claims 1 to 8, characterized in that: use of an interdigital electrode material having a vertically oriented three-dimensional structure according to any one of claims 1 to 8 in a sensor.
10. Use of the interdigitated electrode material with a vertically oriented three-dimensional structure according to claim 9, characterized in that: the oxidized nano material needs to be applied after reduction treatment; the reduction treatment comprises the following specific operations: placing the interdigital electrode material with a vertical orientation three-dimensional structure prepared on the basis of the graphene oxide nano material in hydrazine hydrate steam for reduction; the reduction temperature is 80-100 ℃, and the time is 2-24 h.
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| CN111349338A (en) * | 2018-12-21 | 2020-06-30 | 中国科学院大连化学物理研究所 | Lamellar array composite material for heat absorption and conduction and preparation and application thereof |
| CN110773003A (en) * | 2019-11-11 | 2020-02-11 | 清华大学 | Vertical orientation graphene/nano-fiber composite membrane material and preparation method and application thereof |
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| Acetone and ethanol solid-state gas sensors based on TiO2 nanoparticles;R. Rella et al.;《Sensors and Actuators B》;20071231;第127卷;第426-431页 * |
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