A method of flexible sensor is made based on growth in situ silver electrode on paperTechnical field
It is especially a kind of flexible based on growth in situ silver electrode production on paper the present invention relates to flexible sensor technical fieldThe method of sensor.
Background technique
Flexible sensor is a kind of flexible electronic device strained under external force for perceiving body surface, existingThere is the force snesor of technology since the flexibility by its own is limited, cannot achieve the strain detecting to high-flexibility object, beMeet the application in fields such as medical treatment & health, robot, biomethanics, flexible sensor is gradually valued by people.With doctorFor treating health, wearable wrist guard, gloves or vest is made in flexible sensor, can be obtained the information of perception pulse, heartbeat；By taking intelligent robot as an example, essentially intelligent robot includes that perceptional function, decision making function and holding function three are wanted greatlyElement, wherein perceptional function is the bottleneck that intelligent robot is exchanged with external information, is the instantly mostly important skill for being also most difficult to captureArt difficult point, the problem is that, lack highly sensitive, response fastly, flexibility is good, and can be as the flexible sensing of robot skinDevice will improve robot for this purpose, designing the flexible sensor that a kind of high sensitivity, perceptibility are strong, can simulate human skinThe important breakthrough mouth of identification function, perceptional function.
Summary of the invention
The purpose of the present invention is in view of the deficiencies of the prior art and provide one kind be based on paper on growth in situ silver electrode systemMake the method for flexible sensor, the present invention is used on the basis of papery base, spun coating by PAA polyimides, obtains solidification PIPapery base, and silver layer papery base is obtained by silver-colored ammonia process, then silver electrode pattern papery base is obtained by photoetching corrosion method, it usesSensor print is obtained after Ecoflex solution spin coating, by the dielectric layer of two panels sensor print in opposite directions to folding, is finally prepared into softProperty pressure sensor.The present invention is simple with structure, preparation is convenient, perceptibility is strong, flexible and dynamic response high sensitivityAdvantage.
Realizing the specific technical solution of the object of the invention is:
A method of based on paper growth in situ silver electrode make flexible sensor, feature comprising the following specific steps
Step 1: selection glass slide cleans and dries glass slide, select paper substrate it is smooth be adhered to glass slideOn one face；
Step 2: selecting PAA polyimides, concentration 15%；Filling on a paper substrate, with photoresist spinner spin coating, obtains spin coating PAAPapery base；
Step 3: the papery base of spin coating PAA being placed on warm table, heating temperature: 60~100 DEG C；Heating time: 60 min；It is extensiveAgain to room temperature, solidification PI papery base is obtained；
Step 4: silver layer papery base is obtained with silver-colored ammonia process:
4.1: allotment silver nitrate solution, concentration are as follows: 0.02~0.03mol/L；
4.2: ammonium hydroxide being added dropwise in silver nitrate solution with titration, silver nitrate solution is made to fade to clarification from muddiness, it is molten to obtain silver-colored ammoniaLiquid；
4.3: step 3 solidification PI papery base obtained being immersed in silver ammino solution, concentration are as follows: 0.02mol/L；Soaking time:30 min；
4.4: the solidification PI papery base after immersion is rinsed with deionized water；Solidification PI papery base after flushing is immersed into peroxidatingSilver layer, hydrogenperoxide steam generator concentration are as follows: 0.32~0.4mmol/L are precipitated in hydrogen solution；Soaking time: 30 min；Obtain silver layerPapery base；
Step 5: attaching one layer of blue film on silver layer papery base, and mask plate is set on blue film, photoetching, light are implemented using UV methodCarve time, 1.5 min；Obtain photoetching indigo plant film papery base；
Step 6: photoetching indigo plant film papery base being placed in sodium hydroxide solution, the pH value of sodium hydroxide solution is 12；It is not exposedPhotosensitive indigo plant film is stripped, and obtains photosensitive blue film papery base；
Step 7: photosensitive blue film papery base being put into hydrogen peroxide silver etching agent, the concentration of hydrogen peroxide is 15%, by photosensitive indigo plantThe silver layer of film papery base etches away, and obtains silver electrode pattern papery base；
Step 8: cleaning silver electrode pattern, with acetone rinsing silver electrode pattern papery base；
Step: 9: being spin-coated on silver electrode pattern papery base with Ecoflex aliphatic-aromatic copolyester solution, in silver electrode patternDielectric layer is formed on papery base, obtains sensor print；
Step 10: by the dielectric layer of two panels sensor print in opposite directions to folded, and glass slide being removed, with PDMS poly dimethyl siliconThe encapsulation of oxygen alkane, is subsequently placed on warm table and is heating and curing, heating temperature: 70~90 DEG C；Heating time: 60 min；It obtains flexiblePressure sensor.
The present invention uses on the basis of papery base, is spun coating by PAA polyimides, obtains solidification PI papery base, and lead toIt crosses silver-colored ammonia process and obtains silver layer papery base, then silver electrode pattern papery base is obtained by photoetching corrosion method, with Ecoflex solution spin coatingSensor print is obtained afterwards, by the dielectric layer of two panels sensor print in opposite directions to folding, is finally prepared into pliable pressure sensor.ThisInvention has the advantages that structure is simple, preparation is convenient, perceptibility is strong, flexible and dynamic response high sensitivity.
Detailed description of the invention
Fig. 1 is production process schematic diagram of the invention.
Specific embodiment
Refering to fig. 1, the present invention comprising the following specific steps
Step 1: selection glass slide 1 cleans and dries glass slide 1, and the glass that is adhered to for selecting paper substrate 11 smooth carriesOn one face of piece 1；
Step 2: selecting PAA polyimides, concentration 15%；Filling, with photoresist spinner spin coating, obtains spin coating in paper substrate 11PAA papery base 12；
Step 3: the papery base 12 of spin coating PAA being placed on warm table, heating temperature: 60~100 DEG C；Heating time: 60 min；Restore to room temperature, obtains solidification PI papery base 13；
Step 4: silver layer papery base is obtained with silver-colored ammonia process:
4.1: allotment silver nitrate solution, concentration are as follows: 0.02~0.03mol/L；
4.2: ammonium hydroxide being added dropwise in silver nitrate solution with titration, silver nitrate solution is made to fade to clarification from muddiness, it is molten to obtain silver-colored ammoniaLiquid；
4.3: step 3 solidification PI papery base 13 obtained being immersed in silver ammino solution, concentration are as follows: 0.02mol/L；When immersionBetween: 30 min；
4.4: the solidification PI papery base 13 after immersion is rinsed with deionized water；Solidification PI papery base 13 after flushing was immersedSilver layer, hydrogenperoxide steam generator concentration are as follows: 0.32~0.4mmol/L are precipitated in hydrogen peroxide solution；Soaking time: 30 min；It obtainsSilver layer papery base 14；
Step 5: one layer of blue film is attached on silver layer papery base 14, and mask plate is set on blue film, and photoetching is implemented using UV method,Photoetching time, 1.5 min；Obtain photoetching indigo plant film papery base 15；
Step 6: photoetching indigo plant film papery base 15 being placed in sodium hydroxide solution, the pH value of sodium hydroxide solution is 12；It is not exposedPhotosensitive blue film be stripped, obtain photosensitive blue film papery base 16；
Step 7: photosensitive blue film papery base 16 being put into hydrogen peroxide silver etching agent, the concentration of hydrogen peroxide is 15%, will be photosensitiveThe silver layer of blue film papery base 16 etches away, and obtains silver electrode pattern papery base 17；
Step 8: cleaning silver electrode pattern, with acetone rinsing silver electrode pattern papery base 17；
Step: 9: being spin-coated on silver electrode pattern papery base 17 with Ecoflex aliphatic-aromatic copolyester solution, in silver electrode figureDielectric layer 171 is formed on case papery base 17, obtains sensor print 18；
Step 10: by the dielectric layer 171 of two panels sensor print 18 in opposite directions to folded, and glass slide 1 being removed, with PDMS poly- twoMethylsiloxane encapsulation, is subsequently placed on warm table and is heating and curing, heating temperature: 70~90 DEG C；Heating time: 60 min；It obtainsObtain pliable pressure sensor 19.
Embodiment
Step 1: selecting a block size is the glass slide 1 of 3 × 3cm, and the acetone for being 1:1 with ratio, ethyl alcohol remove surfaceGreasy dirt, then it is cleaned by ultrasonic 5 min with deionized water, it is then placed in baking oven and dries, paper substrate 11 is smooth is adhered to for selectionOn one face of glass slide 1；
Step 2: selecting PAA polyimides, concentration 15%；In paper substrate 11, the forward that photoresist spinner is arranged is for filling700r/min, time 12s, after turn 2500r/min, time 40s is revolved so that PAA polyimides is evenly coated in paper substratesApply PAA papery base 12；
Step 3: the papery base 12 of spin coating PAA being placed on warm table, heating temperature: 80 DEG C；Heating time: 60 min；ThenRestore to room temperature, obtains solidification PI papery base 13；
Step 4: silver layer papery base is obtained with silver-colored ammonia process:
4.1: allotment silver nitrate solution, concentration are as follows: 0.02mol/L；
4.2: ammonium hydroxide being added dropwise in silver nitrate solution with titration, silver nitrate solution is made to fade to clarification from muddiness, it is molten to obtain silver-colored ammoniaLiquid；
4.3: step 3 solidification PI papery base 13 obtained being immersed in silver ammino solution, soaking time: 30 min；
4.4: the solidification PI papery base 13 after immersion is rinsed with deionized water；Solidification PI papery base 13 after flushing was immersedSilver layer, hydrogenperoxide steam generator concentration are as follows: 0.32mmol/L are precipitated in hydrogen peroxide solution；Soaking time: 30 min；It is allowed to that silver is precipitatedLayer obtains silver layer papery base 14；
Step 5: one layer of blue film is attached on silver layer papery base 14, and mask plate is set on blue film, and photoetching is implemented using UV method,Photoetching time, 1.5 min；Obtain photoetching indigo plant film papery base 15；
Step 6: photoetching indigo plant film papery base 15 being placed in sodium hydroxide solution and is developed, the pH value of sodium hydroxide solution is 12；MakeThe photosensitive blue film not being exposed be stripped, obtain photosensitive blue film papery base 16；
Step 7: photosensitive blue film papery base 16 being put into hydrogen peroxide silver etching agent, the concentration of hydrogen peroxide is 15%；It will be photosensitiveIt is not etched away by the silver layer that blue film covers on blue film papery base 16, obtains silver electrode pattern papery base 17；
Step 8: then cleaning silver electrode pattern is dried with acetone rinsing silver electrode pattern papery base 17；
Step: 9: being spin-coated on silver electrode pattern papery base 17 with Ecoflex aliphatic-aromatic copolyester solution, photoresist spinner is setForward be 700r/min, time 12s, after turn 3000r/min, time 40s；It is formed and is situated between on silver electrode pattern papery base 17Matter layer 171 obtains sensor print 18；
Step 10: by the dielectric layer 171 of two panels sensor print 18 in opposite directions to folded, and glass slide 1 being removed, with PDMS poly- twoMethylsiloxane encapsulation, is subsequently placed on warm table and is heating and curing, heating temperature: 80 DEG C；Heating time: 60 min；It obtains softProperty pressure sensor 19.
Pliable pressure sensor 19 is attached at wrist, the diastole of blood vessels will make by the present invention for measuring human pulseThe capacitance for obtaining pressure sensor generates variation, and 19 electrode of pliable pressure sensor is connected to single-chip simulation port, externalOne circuit RC by detecting the variation of 19 capacitance of pliable pressure sensor, and then acquires beat pulse curve.
The present invention is affectedly bashful soft work for manipulator, and pliable pressure sensor 19 is attached on manipulator, can getMost preferably be affectedly bashful power when manipulator touches soft work, not only will not defective work piece, but also not will cause slippage, as robot sense of touchFlexible sensor, the identification function and perceptional function of robot can be greatly improved.