CN110333010B - Interdigital large-area flexible array sensor and preparation method thereof - Google Patents
Interdigital large-area flexible array sensor and preparation method thereof Download PDFInfo
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- CN110333010B CN110333010B CN201910285025.3A CN201910285025A CN110333010B CN 110333010 B CN110333010 B CN 110333010B CN 201910285025 A CN201910285025 A CN 201910285025A CN 110333010 B CN110333010 B CN 110333010B
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- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/61—Additives non-macromolecular inorganic
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/18—Measuring force or stress, in general using properties of piezo-resistive materials, i.e. materials of which the ohmic resistance varies according to changes in magnitude or direction of force applied to the material
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- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/02—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning
- G01L9/06—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning of piezo-resistive devices
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
Abstract
The invention relates to the field of sensors, and discloses an interdigital large-area flexible array sensor and a preparation method thereof, wherein the sensor comprises a plate electrode provided with an interdigital array electrode and a lead, a flexible substrate, and an array pressure-sensitive layer and an insulating adhesive layer which are arranged between the plate electrode and the flexible substrate, the interdigital array electrode comprises a plurality of array units containing the same interdigital electrode, the lead comprises a row lead and a column lead, and two ends of each interdigital electrode are respectively connected with the row lead and the column lead, and the preparation method comprises the following steps: preparing an electrode plate by adopting a screen printing process; preparing a pressure-sensitive composite material; printing an uncured pressure-sensitive composite material on array units on the electrode plate by adopting a screen printing process to form an array pressure-sensitive layer; and the electrode plate and the flexible substrate are attached through insulating glue. The method has the advantages of simple process, higher efficiency and low cost, and the prepared large-area high-density flexible array sensor has high sensitivity, good stability and large pressure sensing range.
Description
Technical Field
The invention relates to the field of sensors, in particular to an interdigital large-area flexible array sensor and a preparation method thereof.
Background
With the improvement of scientific technology and modernization level, the requirement of people on pressure monitoring is higher and higher, the pressure monitoring on a regular rigid surface is not limited any more, the modes are also various, and the common rigid sensor can not meet the actual requirements of people. The flexible pressure sensor can be bent or even folded at will, is small in size and thin in thickness, and the flexible material is basically non-toxic and harmless, so that the flexible pressure sensor has good compatibility with a human body, and is widely researched and applied in the fields of medical equipment, intelligent robot bionic skin, wearable equipment and the like in recent years.
In recent years, with rapid development in the fields of robot bionic skin, flexible wearable equipment and the like, people have increasingly raised requirements on large-area high-density flexible sensor arrays, and although flexible pressure sensor technology has been developed greatly in recent years, research on large-area flexible array sensors is less.
In large area integration applications, a soft lithography process is generally adopted at present, for example, in chinese patent document, "a flexible wearable resistive strain sensor and a method for making the same", which is disclosed in publication No. CN108267078A, the resistive strain sensor includes a flexible substrate, a sensing layer, an electrode layer, and a protective layer. Compared with other sensors of the same type, the sensor has the characteristics of rapid large-area preparation, good stability, high sensitivity, simple and convenient operation and the like.
However, the sensor adopting the traditional photoetching process has low material utilization rate and overhigh manufacturing cost, and when the sensor is integrated in a large area, if the array density is higher, the efficiency is too low, the preparation difficulty is overlarge, and the application of the sensor is limited.
In addition, the large-area flexible array sensor in the prior art generally adopts a sandwich structure in which a pressure-sensitive layer is sandwiched between an upper polar plate and a lower polar plate, the upper polar plate and the lower polar plate of the sensor with the sandwich structure must be accurately aligned when the sensor is packaged, the process requirement is high, the packaging efficiency of the sensor is reduced, and the performance of the sensor is affected if the upper polar plate and the lower polar plate are not aligned.
Disclosure of Invention
The first invention aims to overcome the problems that the material utilization rate is low, the manufacturing cost is overhigh, and the efficiency is too low and the manufacturing difficulty is overlarge due to high array density in large-area integration when a large-area flexible array sensor is manufactured by adopting the traditional photoetching process in the prior art.
The second invention of the invention aims to overcome the problems that the upper and lower polar plates must be accurately aligned when the sensor adopting a sandwich structure in the prior art is packaged, the process requirement is higher, the packaging efficiency of the sensor is reduced, and the performance of the sensor is affected if the upper and lower polar plates are not aligned.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an interdigital large-area flexible array sensor comprises the following steps:
(1) preparing an electrode plate: printing an electrode material on a substrate material by adopting a screen printing process, forming an interdigital array electrode and a lead wire comprising a plurality of array units on the substrate material, and drying to obtain an electrode plate;
(2) preparing a pressure-sensitive composite material: the conductive particles and 5-20 parts of nano SiO by weight2And 15-40 parts of silane coupling agent Si-69 are dispersed in 85-115 parts of solvent to form dispersion liquid; adding 350-450 parts of silicon rubber into the dispersion liquid, and uniformly stirring to obtain a mixed liquid; vacuum drying the mixed solution for 20-30min to obtain an uncured pressure-sensitive composite material, wherein the conductive particles comprise 20-75 parts of carbon black and 5-25 parts of carbon nanotubes;
(3) manufacturing a pressure-sensitive layer of the sensor array: printing the uncured pressure-sensitive composite material on each array unit on the electrode plate by adopting a screen printing process to form an array pressure-sensitive layer;
(4) packaging a sensor: and coating the insulating glue on the electrode plates around the array pressure-sensitive layer, sealing the flexible substrate on the surfaces of the insulating glue and the array pressure-sensitive layer, and curing the insulating glue to obtain the interdigital large-area flexible array sensor.
The electrode plate and the array pressure-sensitive layer are manufactured by adopting a screen printing process, so that the process can be simplified, the cost can be reduced, and the processing efficiency can be improved. The silicon rubber is selected as a matrix material in the pressure-sensitive composite material, and has excellent electrical insulation performance and aging resistance, high mechanical strength, good elasticity, ultraviolet light resistance, ozone resistance, acid and alkali resistance, wide use temperature range, safety, no toxicity, good compatibility with a human body and excellent processability; the silicon rubber is doped with conductive particles, so that the silicon rubber has certain conductivity and certain pressure-sensitive performance.
The pressure-sensitive composite material of the invention adopts carbon black and carbon nano tubes as conductive particles, and the carbon black/carbon nano tubes can play a role of synergistic enhancement when being used together in the silicone rubber due to the larger length-diameter ratio of the carbon nano tubes and the relatively shorter silicone rubber molecular chains. The carbon black and the carbon nano tube can form a structure similar to a grape string, the carbon nano tube can be regarded as a stem and has the function of linking and fixing the carbon black, and the silicon rubber molecular chain is used as a framework of a conductive network chain and is mutually staggered with the grape string-shaped structure to form a stable reinforcing structure. Due to the larger length-diameter ratio of the carbon nano tube, the carbon nano tube can play a role in long-distance electric conduction in a system, and the carbon black can play a role in short-distance electric conduction on one hand and can also connect adjacent carbon nano tubes to play a role in bridging. The integral reinforcing structure has certain influence on the conductivity and stability of the composite system and the mechanical property of the composite material. Compared with a single system, the mechanical property is improved, the conductive network with the dotted line structure has higher sensing sensitivity, the number of conductive channels is increased in a certain pressure range, and the pressure sensing range is improved, so that the sensitivity and the measuring range of the sensor are improved.
The proportion of each component of the pressure-sensitive composite material is suitable for a screen printing process, the composite material can well penetrate through a screen printing plate during printing, the performance after printing is good, the film thickness is uniform and smooth, and the phenomena of paste surface deformation and the like are avoided.
Since the electrode, the lead and the pressure-sensitive layer prepared in the invention are directly printed on the substrate material, the sensor is easy to fall off or scratch to cause damage during the use process, the measured data is inaccurate if the measured data is light, and the sensor fails if the measured data is heavy. And the electrode material is exposed to air for a long time, so that oxidation reaction is easy to occur, the conductivity of the lead is deteriorated, and the performance of the sensor is seriously influenced. Therefore, the flexible substrate is attached to the surfaces of the electrode plate and the array pressure-sensitive layer through the insulating glue, so that the contact between the electrode and the lead and the air can be isolated, and the pressure-sensitive layer can be protected from being damaged.
Preferably, the electrode material in step (1) is a yutelin type ID01 conductive silver paste, and the base material is a PET substrate. The conductive silver paste has good conductivity and good fluidity, is suitable for screen printing, and the prepared electrode and lead have good strength and pressure resistance and strong adhesive force on a substrate material.
Preferably, a 300-420-mesh steel wire mesh plate or a polyester mesh plate is adopted during screen printing in the step (1), the electrode material can well penetrate through the screen plate during printing, and the printed electrode and the printed lead are uniform and smooth and have good performance.
Preferably, the drying temperature in the step (1) is 120-140 ℃, and the drying time is 40-60 min. The printed electrode and the printed lead can be better cured and formed and attached to the surface of the base material, so that the prepared upper and lower polar plates have good performance.
Preferably, the conductive particles in step (2) are surface-modified conductive particles, and the preparation method thereof is as follows:
(A) dispersing conductive particles in 0.4-0.6mol/L nitric acid solution, carrying out oscillation reaction for 2-3h, filtering, washing with water to neutrality, and drying at 60-70 ℃ for 12-24 h;
(B) dissolving the obtained product in thionyl chloride, adding 2-3 drops of N, N-dimethylformamide, and reacting at 50-60 ℃ for 12-24 h;
(C) dispersing the obtained product in ethylene glycol, and carrying out reflux reaction at the temperature of 100-120 ℃ for 20-30 h;
(D) mixing 4-dimethylamino pyridine and triethylamine in the mass ratio of 1 (10-15) to (15-20) and the product obtained in the step (C), adding CHCl3Adding a chloroform solution of 2-bromoisobutyl acyl bromide with the mass ratio of 1:1-2:1 to the product obtained in the step (C) under the protection of nitrogen, stirring at 0-4 ℃ for 1-2h, and continuing to react at room temperature for 20-30 h;
(E) diluting the obtained solution with chloroform, filtering, repeatedly washing, and drying at 50-60 deg.C for 10-20 h;
(F) mixing the dried pentamethyl diethylenetriamine and CuBr in the mass ratio of 1 (1-2) to 5-7 with the product obtained in the step (E), adding N, N-dimethylformamide, adding vinyl pyrrolidone in the mass ratio of 10:1-15:1 with the product obtained in the step (E) under the protection of nitrogen, and stirring and reacting for 20-30h at the temperature of 60-70 ℃;
(G) and after the obtained solution is filtered, washing the solution to be neutral by water, and drying the solution for 6 to 12 hours at the temperature of between 60 and 70 ℃ to obtain the surface modified conductive particles.
Introducing carboxylic acid groups on the surfaces of the conductive particles through nitric acid treatment; then reacting with thionyl chloride in the step (B) to obtain conductive particles for acyl chlorination; then, conducting reaction with ethylene glycol in the step (C) to obtain surface hydroxylated conductive particles; reacting with a brominating reagent in the step (D) to obtain brominating conductive particles; and (F) initiating vinyl pyrrolidone monomer polymerization by using the brominated conductive particles as an initiator, and grafting the vinyl pyrrolidone monomer on the surface of the conductive particles to finally obtain the surface modified conductive particles.
Because carbon black and carbon nano tubes both have larger specific surface area and surface energy, larger interparticle force is easy to be wound and agglomerated with rubber, so that the dispersibility of the carbon black and the carbon nano tubes is poor, and the performance of the pressure-sensitive composite material is influenced. According to the invention, the dispersant polyvinylpyrrolidone is grafted on the surface of the conductive particle, so that the hydrophobic group of the dispersant is firmly adsorbed on the surface of the conductive particle, the hydrophilic group extends in an aqueous system, the surface free energy of the conductive particle is reduced, the steric hindrance is increased, and the conductive particle after surface modification has high dispersion stability, thereby improving the piezoresistive performance of the pressure-sensitive composite material and improving the sensitivity of the sensor.
Preferably, the solvent in step (2) comprises at least one of n-hexane, naphtha and absolute ethyl alcohol. The solvent can dilute the high molecular silicon rubber matrix, and creates a favorable environment for the uniform dispersion of the conductive particles and the nano modified particles.
Preferably, a 100-mesh and 300-mesh nylon screen plate is adopted for screen printing in the step (3). The surface of the printed array pressure-sensitive layer is smooth, the thickness is moderate, and a better printing effect can be achieved.
Preferably, the insulating paste is PDMS. PDMS has good chemical inertness, no toxicity, non-flammability, low cost, simple use and good adhesion with PET material.
The invention also provides an interdigital large-area flexible array sensor prepared by the method, which comprises a plate electrode provided with interdigital array electrodes and wires, a flexible substrate, and an array pressure-sensitive layer and an insulating adhesive layer which are positioned between the plate electrode and the flexible substrate, wherein the interdigital array electrodes comprise a plurality of array units which are arranged in a row-column structure, the same interdigital electrodes are arranged in each array unit, the wires comprise row wires and column wires, two ends of each interdigital electrode are respectively connected with the row wires and the column wires, and the insulating adhesive layer is hollowed in positions corresponding to the array pressure-sensitive layer.
The interdigital array electrode and the row and column conducting wires are manufactured on the same substrate material to form the electrode plate, so that the process flow of accurately aligning the array electrodes on the upper and lower electrode plates in the preparation of the traditional sandwich-type sensor is avoided, and the assembly efficiency is improved. The array electrodes are uniformly arranged, the spatial distribution is reasonable, the manufacturing process is simple, the large-area high-density array is convenient to realize, and the prepared large-area high-density flexible sensor is high in sensitivity and large in pressure sensing range.
Preferably, the row and column conductors lead from opposite sides of the electrode plate, respectively. The wires are reasonably arranged, the manufacture and the subsequent connection are convenient, and the manufacture process is simplified.
Therefore, the invention has the following beneficial effects:
(1) the polar plate and the array pressure-sensitive layer are manufactured by adopting a screen printing process, so that the process can be simplified, the cost can be reduced, and the processing efficiency can be improved;
(2) the proportion of each component of the pressure-sensitive composite material is suitable for a screen printing process, the composite material can well penetrate through a screen printing plate during printing, the performance after printing is good, the film thickness is uniform and smooth, and the phenomena of paste surface deformation and the like are avoided;
(3) the pressure-sensitive composite material adopts carbon black and carbon nano tubes as conductive particles together, the carbon black/carbon nano tubes are used in the silicone rubber together to play a role in synergistic enhancement, the carbon black and the carbon nano tubes can form a structure similar to a grape string, silicone rubber molecular chains are used as frameworks of conductive network chains and are mutually staggered with the grape string-shaped structure to form a stable reinforcement structure, and the integral reinforcement structure has certain influence on the conductivity and stability of a composite system and the mechanical property of the composite material;
(4) the interdigital array electrode and the row and column conducting wires are manufactured on the same substrate material to form a plate electrode, so that the process flow of accurately aligning the array electrodes on the upper and lower plate electrodes in the preparation of the traditional sandwich-type sensor is avoided, and the assembly efficiency is improved.
Drawings
FIG. 1 is a schematic diagram of an exploded structure of an interdigital large-area flexible array sensor in the present invention;
FIG. 2 is a schematic view of the structure of the electrode plate of the present invention.
In the figure: the flexible printed circuit board comprises a 1 electrode plate, a 2 flexible substrate, a 3 array pressure-sensitive layer, a 4 insulating adhesive layer, 5 interdigital electrodes, 6 row leads and 7 column leads.
Detailed Description
The invention is further described with reference to the following detailed description and accompanying drawings.
As shown in fig. 1 and fig. 2, the interdigital large-area flexible array sensor manufactured in each embodiment and comparative example of the present invention includes an electrode plate 1 provided with an interdigital array electrode and a lead, a flexible substrate 2, and an array pressure-sensitive layer 3 and an insulating adhesive layer 4 located between the electrode plate and the flexible substrate, the interdigital array electrode includes 5 × 5 array units, each array unit is a square with a side length of 1mm, a distance between two adjacent array units is 0.8mm, the same interdigital electrode 5 is provided in each array unit, the lead includes a row lead 6 and a column lead 7, two ends of each interdigital electrode are respectively connected with the row lead and the column lead, the row lead is led out from the right side of the electrode plate, the column lead is led out from the left side of the electrode plate, and the insulating adhesive layer is hollowed out in a position corresponding to the array pressure-sensitive.
According to the invention, before preparing the polar plate, a PET substrate with the thickness of 0.125mm is cut into the size of 1cm multiplied by 1cm according to the size occupied by the required electrode and the required lead, the PET substrate is used as a base material and a flexible substrate of the polar plate, the cut PET substrate is cleaned by absolute ethyl alcohol and deionized water, surface impurities are removed, the adhesive force of a printing material is improved, and then a silk screen printing screen plate is manufactured according to the patterns of the electrode and the lead.
Example 1:
preparing a polar plate: printing Uygnew ID01 type conductive silver paste on a PET (polyethylene terephthalate) substrate by using a 420-mesh steel wire mesh plate through a screen printing process, forming an array electrode and a lead wire containing 25 array units on the PET substrate, placing the printed array electrode and lead wire in a forced air oven, and drying the printed array electrode and lead wire at 120 ℃ for 40min to obtain an electrode plate;
preparing a pressure-sensitive composite material: 20g of Keqin carbon black ECP600JD, 5g of carbon nano tube and 5g of nano SiO2Adding 10g of 2% silane coupling agent Si-69 into 85g of naphtha, stirring, performing ultrasonic dispersion for 30min to form dispersion liquid, adding 350g of room-temperature vulcanized silicone rubber Dow Corning 184 into the dispersion liquid, performing magnetic stirring for 3h at room temperature to form viscous mixed liquid, placing the mixed liquid into a vacuum drying oven, drying for 20min at 40 ℃, and removing bubbles and incompletely volatilized naphtha to obtain the uncured pressure-sensitive composite material;
manufacturing a pressure-sensitive layer of the sensor array: using a 300-mesh nylon screen plate, printing an uncured pressure-sensitive composite material on each array unit on the electrode plate by a screen printing process to form an array pressure-sensitive layer, and performing printing once again after the composite material layer is completely cured in one-time printing in order to avoid the problems of cracks and the like of the composite material layer possibly existing as much as possible, so as to ensure the effectiveness of the sensor;
packaging a sensor: and coating PDMS on the electrode plates around the array pressure-sensitive layer, sealing the flexible substrate on the surfaces of the PDMS and the array pressure-sensitive layer, and curing the PDMS to obtain the interdigital large-area flexible array sensor.
Example 2:
preparing a polar plate: printing Uetnew ID01 type conductive silver paste on a PET (polyethylene terephthalate) substrate by using a 300-mesh polyester screen plate through a screen printing process, forming an array electrode and a lead wire containing 25 array units on the PET substrate, placing the printed array electrode and the lead wire in a blast oven, and drying the printed array electrode and the lead wire at 140 ℃ for 60min to obtain an electrode plate;
preparing a pressure-sensitive composite material: 75g of Keqin carbon black ECP600JD, 25g of carbon nano tube and 20g of nano SiO2And 40g of 2% silane coupling agent Si-69, adding into a mixed solution of 25g of n-hexane, 65g of naphtha and 25g of absolute ethyl alcohol, stirring, and performing ultrasonic dispersion for 60min to form a dispersion liquidAdding 450g of room temperature vulcanized silicone rubber downing 184 into the dispersion, magnetically stirring for 8 hours at room temperature to form viscous mixed liquid, placing the mixed liquid in a vacuum drying oven, drying for 30 minutes at 100 ℃, and removing bubbles and incompletely volatilized solvents to obtain an uncured pressure-sensitive composite material;
manufacturing a pressure-sensitive layer of the sensor array: printing an uncured pressure-sensitive composite material on each array unit on the electrode plate by using a 100-mesh nylon screen plate through a screen printing process to form an array pressure-sensitive layer, and performing printing once again after the composite material layer is completely cured in one-time printing in order to avoid the possible problems of cracks and the like of the composite material layer as much as possible, so as to ensure the effectiveness of the sensor;
packaging a sensor: and coating PDMS on the electrode plates around the array pressure-sensitive layer, sealing the flexible substrate on the surfaces of the PDMS and the array pressure-sensitive layer, and curing the PDMS to obtain the interdigital large-area flexible array sensor.
Example 3:
preparing a polar plate: printing Uygnew ID01 type conductive silver paste on a PET substrate by using a 400-mesh polyester screen plate through a screen printing process, forming an array electrode and a lead wire containing 25 array units on the PET substrate, placing the printed array electrode and lead wire in a forced air oven, and drying the printed array electrode and lead wire at 130 ℃ for 50min to obtain an electrode plate;
preparing a pressure-sensitive composite material: 50g of Keqin carbon black ECP600JD, 10g of carbon nano tube and 15g of nano SiO2Adding 30g of 2% silane coupling agent Si-69 into a mixed solution of 70g of naphtha and 30g of absolute ethyl alcohol, stirring and then ultrasonically dispersing for 40min to form a dispersion liquid, adding 400g of room-temperature vulcanized silicone rubber Dow Corning 184 into the dispersion liquid, magnetically stirring for 6h at room temperature to form a viscous mixed liquid, placing the mixed liquid into a vacuum drying oven to dry for 25min at 70 ℃, and removing bubbles, and naphtha and absolute ethyl alcohol which are not completely volatilized to obtain an uncured pressure-sensitive composite material;
manufacturing a pressure-sensitive layer of the sensor array: printing an uncured pressure-sensitive composite material on each array unit on the electrode plate by using a 200-mesh nylon screen plate through a screen printing process to form an array pressure-sensitive layer, and performing printing once again after the composite material layer is completely cured in one-time printing in order to avoid the possible problems of cracks and the like of the composite material layer as much as possible, so as to ensure the effectiveness of the sensor;
packaging a sensor: and coating PDMS on the electrode plates around the array pressure-sensitive layer, sealing the flexible substrate on the surfaces of the PDMS and the array pressure-sensitive layer, and curing the PDMS to obtain the interdigital large-area flexible array sensor.
Example 4:
preparing a polar plate: printing Uygnew ID01 type conductive silver paste on a PET (polyethylene terephthalate) substrate by using a 420-mesh steel wire mesh plate through a screen printing process, forming an array electrode and a lead wire containing 25 array units on the PET substrate, placing the printed array electrode and lead wire in a forced air oven, and drying the printed array electrode and lead wire at 120 ℃ for 40min to obtain an electrode plate;
preparing surface modified conductive particles: dispersing 20g of Keqin carbon black ECP600JD and 5g of carbon nano tubes in 0.4mol/L nitric acid solution, carrying out oscillation reaction for 3h, filtering, washing with water to be neutral, and drying at 70 ℃ for 24 h; the resulting product was dissolved in SOCl2Dropwise adding two drops of N, N-dimethylformamide, and reacting at 60 ℃ for 24 hours; dispersing the obtained product in ethylene glycol, and carrying out reflux reaction for 30h at the temperature of 120 ℃; to the resulting product were added 1.67g of 4-dimethylaminopyridine, 16.7g of triethylamine and 532mL of CHCl3Mixing, adding a solution of 25g of 2-bromoisobutyl acyl bromide dissolved in 250mL of chloroform under the protection of nitrogen, stirring at 4 ℃ for 2h, and continuing to react at room temperature for 30 h; diluting the obtained solution with chloroform, filtering, repeatedly washing, and drying at 60 deg.C for 20 h; mixing the dried product with 5g of pentamethyldiethylenetriamine, 5g of CuBr and 250mL of N, N-dimethylformamide, adding 250g of vinyl pyrrolidone under the protection of nitrogen, and stirring and reacting at 70 ℃ for 30 hours; after the obtained solution is filtered, washing the solution to be neutral by water, and drying the solution for 12 hours at 70 ℃ to obtain surface modified conductive particles;
preparing a pressure-sensitive composite material: 25g of the surface-modified conductive particles prepared above and 5g of nano SiO2And 10g of 2% silane coupling agent Si-69, adding into 85g of naphtha, stirring, and performing ultrasonic dispersion for 30min to form a dispersion liquid. Adding 350g of room temperature vulcanized silicone rubber Dow Corning 184 into the dispersion, magnetically stirring at room temperature for 3h to form viscous mixed solution, and drying the mixed solution in a vacuum drying oven at 40 DEG CRemoving bubbles and incompletely volatilized naphtha for 20min to obtain an uncured pressure-sensitive composite material; manufacturing a pressure-sensitive layer of the sensor array: using a 300-mesh nylon screen plate, printing an uncured pressure-sensitive composite material on each array unit on the electrode plate by a screen printing process to form an array pressure-sensitive layer, and performing printing once again after the composite material layer is completely cured in one-time printing in order to avoid the problems of cracks and the like of the composite material layer possibly existing as much as possible, so as to ensure the effectiveness of the sensor;
packaging a sensor: and coating PDMS on the electrode plates around the array pressure-sensitive layer, sealing the flexible substrate on the surfaces of the PDMS and the array pressure-sensitive layer, and curing the PDMS to obtain the interdigital large-area flexible array sensor.
Example 5:
preparing a polar plate: printing Uetnew ID01 type conductive silver paste on a PET (polyethylene terephthalate) substrate by using a 300-mesh polyester screen plate through a screen printing process, forming an array electrode and a lead wire containing 25 array units on the PET substrate, placing the printed array electrode and the lead wire in a blast oven, and drying the printed array electrode and the lead wire at 140 ℃ for 60min to obtain an electrode plate;
preparing surface modified conductive particles: dispersing 75g of Keqin carbon black ECP600JD and 25g of carbon nano tubes in 0.5mol/L nitric acid solution, carrying out oscillation reaction for 2.5h, filtering, washing with water to be neutral, and drying at 65 ℃ for 20 h; the resulting product was dissolved in SOCl2Dropwise adding 3 drops of N, N-dimethylformamide, and reacting at 55 ℃ for 20 hours; dispersing the obtained product in ethylene glycol, and carrying out reflux reaction for 25h at the temperature of 110 ℃; to the resulting product were added 5g of 4-dimethylaminopyridine, 75g of triethylamine and 2150mL of CHCl3Mixing, adding a solution of 200g of 2-bromoisobutyl acyl bromide dissolved in 2000mL of chloroform under the protection of nitrogen, stirring at 2 ℃ for 1.5h, and continuing to react at room temperature for 25 h; diluting the obtained solution with chloroform, filtering, repeatedly washing, and drying at 55 deg.C for 15 h; mixing the dried product with 14.3g of pentamethyldiethylenetriamine, 28.6g of CuBr and 1000mL of N, N-dimethylformamide, adding 1500g of vinyl pyrrolidone under the protection of nitrogen, and stirring and reacting at 65 ℃ for 25 h; after the obtained solution is filtered, washing the solution to be neutral by water, and drying the solution for 8 hours at 65 ℃ to obtain surface modified conductive particles;
preparation of pressure-sensitive compositeMaterial preparation: 100g of the surface-modified conductive particles prepared above and 20g of nano SiO2Adding 40g of 2% silane coupling agent Si-69 into a mixed solution of 25g of n-hexane, 65g of naphtha and 25g of absolute ethyl alcohol, stirring, performing ultrasonic dispersion for 60min to form a dispersion solution, adding 450g of room temperature vulcanized silicone rubber Dow Corning 184 into the dispersion solution, performing magnetic stirring for 8h at room temperature to form a viscous mixed solution, placing the mixed solution into a vacuum drying oven, drying for 30min at 100 ℃, removing bubbles and incompletely volatilized solvent, and thus obtaining the uncured pressure-sensitive composite material;
manufacturing a pressure-sensitive layer of the sensor array: printing an uncured pressure-sensitive composite material on each array unit on the electrode plate by using a 100-mesh nylon screen plate through a screen printing process to form an array pressure-sensitive layer, and performing printing once again after the composite material layer is completely cured in one-time printing in order to avoid the possible problems of cracks and the like of the composite material layer as much as possible, so as to ensure the effectiveness of the sensor;
packaging a sensor: and coating PDMS on the electrode plates around the array pressure-sensitive layer, sealing the flexible substrate on the surfaces of the PDMS and the array pressure-sensitive layer, and curing the PDMS to obtain the interdigital large-area flexible array sensor.
Example 6:
preparing a polar plate: printing Uygnew ID01 type conductive silver paste on a PET substrate by using a 400-mesh polyester screen plate through a screen printing process, forming an array electrode and a lead wire containing 25 array units on the PET substrate, placing the printed array electrode and lead wire in a forced air oven, and drying the printed array electrode and lead wire at 130 ℃ for 50min to obtain an electrode plate;
preparing surface modified conductive particles: dispersing 50g of Keqin carbon black ECP600JD and 10g of carbon nano tubes in 0.6mol/L nitric acid solution, carrying out oscillation reaction for 2h, filtering, washing with water to be neutral, and drying at 60 ℃ for 12 h; the resulting product was dissolved in SOCl2Dropwise adding two drops of N, N-dimethylformamide, and reacting at 50 ℃ for 12 hours; dispersing the obtained product in ethylene glycol, and carrying out reflux reaction for 20h at 100 ℃; to the resulting product was added 3.3g of 4-dimethylaminopyridine, 40g of triethylamine and 1200mL of CHCl3Mixing, adding 90g 2-bromoisobutyl acyl bromide solution in 650mL chloroform under nitrogen protection, stirring at 0 deg.C for 1h, and continuing at room temperatureReacting for 20 hours; diluting the obtained solution with chloroform, filtering, repeatedly washing, and drying at 50 deg.C for 10 hr; mixing the dried product with 10g of pentamethyldiethylenetriamine, 15g of CuBr and 600mL of N, N-dimethylformamide, adding 720g of vinyl pyrrolidone under the protection of nitrogen, and stirring and reacting for 20 hours at 60 ℃; after the obtained solution is filtered, washing the solution to be neutral by water, and drying the solution for 6 hours at the temperature of 60 ℃ to obtain surface modified conductive particles;
preparing a pressure-sensitive composite material: 60g of the surface-modified conductive particles prepared above and 15g of nano SiO2And 30g of 2% silane coupling agent Si-69, adding the mixture into a mixed solution of 70g of naphtha and 30g of absolute ethyl alcohol, stirring, and performing ultrasonic dispersion for 40min to form a dispersion liquid. Adding 400g of room-temperature vulcanized silicone rubber downing 184 into the dispersion, magnetically stirring for 6 hours at room temperature to form viscous mixed liquid, placing the mixed liquid in a vacuum drying oven, drying for 25 minutes at 70 ℃, and removing bubbles, naphtha which is not completely volatilized and absolute ethyl alcohol to obtain an uncured pressure-sensitive composite material;
manufacturing a pressure-sensitive layer of the sensor array: printing an uncured pressure-sensitive composite material on each array unit on the electrode plate by using a 200-mesh nylon screen plate through a screen printing process to form an array pressure-sensitive layer, and performing printing once again after the composite material layer is completely cured in one-time printing in order to avoid the possible problems of cracks and the like of the composite material layer as much as possible, so as to ensure the effectiveness of the sensor;
packaging a sensor: and coating PDMS on the electrode plates around the array pressure-sensitive layer, sealing the flexible substrate on the surfaces of the PDMS and the array pressure-sensitive layer, and curing the PDMS to obtain the interdigital large-area flexible array sensor.
Comparative example 1:
preparing a polar plate: printing Uygnew ID01 type conductive silver paste on a PET (polyethylene terephthalate) substrate by using a 420-mesh steel wire mesh plate through a screen printing process, forming an array electrode and a lead wire containing 25 array units on the PET substrate, placing the printed array electrode and lead wire in a forced air oven, and drying the printed array electrode and lead wire at 120 ℃ for 40min to obtain an electrode plate;
preparing a pressure-sensitive composite material: 25g of Keqin carbon black ECP600JD and 20g of nano SiO240g of 2% silane coupling agent Si-69, 115g of naphthaStirring in oil, and ultrasonically dispersing for 30min to obtain dispersion. Adding 450g of room temperature vulcanized silicone rubber into the dispersion, magnetically stirring for 3 hours at room temperature to form viscous mixed liquid, placing the mixed liquid into a vacuum drying oven, drying for 20 minutes at 40 ℃, and removing bubbles and incompletely volatilized naphtha to obtain the uncured pressure-sensitive composite material.
Manufacturing a pressure-sensitive layer of the sensor array: using a 300-mesh nylon screen plate, printing an uncured pressure-sensitive composite material on each array unit on the electrode plate by a screen printing process to form an array pressure-sensitive layer, and performing printing once again after the composite material layer is completely cured in one-time printing in order to avoid the problems of cracks and the like of the composite material layer possibly existing as much as possible, so as to ensure the effectiveness of the sensor;
packaging a sensor: and coating PDMS on the electrode plates around the array pressure-sensitive layer, sealing the flexible substrate on the surfaces of the PDMS and the array pressure-sensitive layer, and curing the PDMS to obtain the interdigital large-area flexible array sensor.
The performance of the interdigital large-area flexible array sensor prepared in the above examples and comparative examples was tested, and the test results are shown in table 1.
Table 1: and (5) performance test results of the interdigital large-area flexible array sensor.
As can be seen from Table 1, the sensor has a significant positive pressure resistance effect only in the range of 0-2N when only carbon black is used as the conductive particles in comparative example 1, while the sensor has a significant positive pressure resistance effect in the range of 0-4N when carbon black and carbon nanotubes are used together as the conductive particles in examples 1-6, so that the pressure sensing range of the sensor is wider when carbon black and carbon nanotubes are used together as the conductive particles.
When the ordinary conductive particles are used in the embodiments 1-3, the sensitivity of the sensor is less than or equal to 70 Ω/N, while when the surface modified conductive particles are used in the embodiments 4-6, the sensitivity of the sensor can be raised to 114-121 Ω/N, so that when the surface modified conductive particles are used, the sensor can have higher sensitivity.
Claims (9)
1. A preparation method of an interdigital large-area flexible array sensor is characterized by comprising the following steps:
(1) preparing an electrode plate: printing an electrode material on a substrate material by adopting a screen printing process, forming an interdigital array electrode and a lead wire comprising a plurality of array units on the substrate material, and drying to obtain an electrode plate;
(2) preparing a pressure-sensitive composite material: the conductive particles and 5-20 parts of nano SiO by weight2And 15-40 parts of silane coupling agent Si-69 are dispersed in 85-115 parts of solvent to form dispersion liquid; adding 350-450 parts of silicon rubber into the dispersion liquid, and uniformly stirring to obtain a mixed liquid; and drying the mixed solution in vacuum for 20-30min to obtain the uncured pressure-sensitive composite material, wherein the conductive particles comprise 20-75 parts of carbon black and 5-25 parts of carbon nanotubes, and the conductive particles are surface-modified conductive particles, and the preparation method comprises the following steps:
(A) dispersing conductive particles in 0.4-0.6mol/L nitric acid solution, carrying out oscillation reaction for 2-3h, filtering, washing with water to neutrality, and drying at 60-70 ℃ for 12-24 h;
(B) dissolving the obtained product in thionyl chloride, adding 2-3 drops of N, N-dimethylformamide, and reacting at 50-60 ℃ for 12-24 h;
(C) dispersing the obtained product in ethylene glycol, and carrying out reflux reaction at the temperature of 100-120 ℃ for 20-30 h;
(D) mixing 4-dimethylamino pyridine and triethylamine in the mass ratio of 1 (10-15) to (15-20) and the product obtained in the step (C), adding CHCl3Adding a chloroform solution of 2-bromoisobutyl acyl bromide with the mass ratio of 1:1-2:1 to the product obtained in the step (C) under the protection of nitrogen, stirring at 0-4 ℃ for 1-2h, and continuing to react at room temperature for 20-30 h;
(E) diluting the obtained solution with chloroform, filtering, repeatedly washing, and drying at 50-60 deg.C for 10-20 h;
(F) mixing the dried pentamethyl diethylenetriamine and CuBr in the mass ratio of 1 (1-2) to 5-7 with the product obtained in the step (E), adding N, N-dimethylformamide, adding vinyl pyrrolidone in the mass ratio of 10:1-15:1 with the product obtained in the step (E) under the protection of nitrogen, and stirring and reacting for 20-30h at the temperature of 60-70 ℃;
(G) after the obtained solution is filtered, washing the solution to be neutral by water, and drying the solution for 6 to 12 hours at the temperature of between 60 and 70 ℃ to obtain surface modified conductive particles;
(3) manufacturing a pressure-sensitive layer of the sensor array: printing the uncured pressure-sensitive composite material on each array unit on the electrode plate by adopting a screen printing process to form an array pressure-sensitive layer;
(4) packaging a sensor: and coating the insulating glue on the electrode plates around the array pressure-sensitive layer, sealing the flexible substrate on the surfaces of the insulating glue and the array pressure-sensitive layer, and curing the insulating glue to obtain the interdigital large-area flexible array sensor.
2. The method as claimed in claim 1, wherein the electrode material in step (1) is Eudragit ID01 conductive silver paste, and the base material is PET substrate.
3. The preparation method of the interdigital large-area flexible array sensor according to claim 1 or 2, wherein a 300-420 mesh steel wire mesh plate or a polyester mesh plate is adopted in the screen printing in the step (1).
4. The preparation method of the interdigital large-area flexible array sensor as claimed in claim 1 or 2, wherein the drying temperature in step (1) is 120-.
5. The method for preparing an interdigital large-area flexible array sensor according to claim 1, wherein the solvent in step (2) comprises at least one of n-hexane, naphtha and absolute ethyl alcohol.
6. The method as claimed in claim 1, wherein a 100-mesh 300-mesh nylon screen is used for screen printing in step (3).
7. The method for preparing an interdigital large-area flexible array sensor according to claim 1, wherein the insulating paste in step (4) is PDMS.
8. An interdigital large-area flexible array sensor prepared by the method of any one of claims 1 to 7, which is characterized by comprising an electrode plate provided with interdigital array electrodes and wires, a flexible substrate, and an array pressure-sensitive layer and an insulating adhesive layer which are arranged between the electrode plate and the flexible substrate, wherein the interdigital array electrodes comprise a plurality of array units which are arranged in a row-column structure, the same interdigital electrodes are arranged in each array unit, the wires comprise row wires and column wires, two ends of each interdigital electrode are respectively connected with the row wires and the column wires, and the insulating adhesive layer is hollowed in positions corresponding to the array pressure-sensitive layer.
9. An interdigitated large area flexible array sensor according to claim 8 in which the row conductors and the column conductors lead from opposite sides of the electrode plate.
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