CN106946221A - Pliable pressure sensor production method based on " V " type groove array electrode - Google Patents
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- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
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- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00134—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems comprising flexible or deformable structures
- B81C1/00166—Electrodes
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- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00841—Cleaning during or after manufacture
- B81C1/00849—Cleaning during or after manufacture during manufacture
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/0002—Lithographic processes using patterning methods other than those involving the exposure to radiation, e.g. by stamping
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- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/16—Coating processes; Apparatus therefor
- G03F7/162—Coating on a rotating support, e.g. using a whirler or a spinner
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- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/40—Treatment after imagewise removal, e.g. baking
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
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- B81C2201/00—Manufacture or treatment of microstructural devices or systems
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- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C2201/00—Manufacture or treatment of microstructural devices or systems
- B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
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Abstract
The invention belongs to flexible sensing field and micro-nano system regions, specially the pliable pressure sensor production method based on " V " type groove array electrode.Pliable pressure sensor production method based on " V " type array electrode, the preparation of preparation and CNT/PDMS polymer including pliable pressure sensor " V " type groove array electrode, obtained two pliable pressure sensors " V " type groove array electrode is taken respectively as Top electrode and bottom electrode, CNT/PDMS laminated films form pliable pressure sensor as intermediate dielectric layer, encapsulation.The problem of for metal material and flexible substrate poor adhesion, the present invention selects dimethyl silicone polymer（PDMS）It is used as flexible substrate material, metal Ag is used as electrode material, and PDMS flexible substrates surface progress moditied processing is used to using plasma techniques to strengthen metal Ag and PDMS adhesiveness, " V " type groove Array microelectrode structure of design efficiently solves pliable pressure sensor metal electrode when occurring compared with large deformation and produces the problem of being broken.
Description
Technical field
The invention belongs to flexible sensing field and micro-nano system regions, the specially flexibility based on " V " type groove array electrode
Pressure sensor preparation method.
Background technology
Sensing technology is one of critical function unit of sociometry now, observing and controlling and intelligent automation system, senses skill
The research and development of art becomes the development field that each country attaches great importance to.In recent years, flexible electronic technology is huge with its
Performance advantage worldwide starts a field technology revolution with quick development speed.The research of flexible sensor, which also turns into, grinds
Study carefully new challenge, frontier that personnel face.
Pressure sensor be it is a kind of can sense ambient pressure change sensor, and be widely used in it is wearable, can paste
In attached electronic skin and electronic device.In order to the ability of increase sharply, require with information age information content capture and processing information
Increasingly enhanced technology trends are consistent, and electronic skin or electronic device are to flexibility, accuracy, reliability, sensitivity
Requirement etc. performance indications is more and more stricter, correspondingly, and the performance indications to pressure sensor require also more and more stricter.And pass
The weak function sensor of large volume of system is difficult often to meet above-mentioned requirements, and therefore, they are progressively by various types of height
Performance microsensor is replaced.
The predominantly research of pliable pressure sensor from the point of view of current research both at home and abroad to flexible sensor, conventional is soft
Property backing material be pet resin（Poly ethylene terephthalate, abbreviation PET）, it is poly-
Vinylidene (Polyvinylidene fluoride, abbreviation PVDF) film, polyethylene dioxythiophene（Poly
Ethylenedioxythiophene, abbreviation PEDOT）Conducting polymer etc., flexible pressure is realized based on nano silver wire, CNT
Prepared by force snesor, but there is metal electrode when metal material easily comes off with flexible substrate, occurred compared with large deformation and easily break
Split the problem of causing sensor failure.
The content of the invention
There is provided the pliable pressure sensor production based on " V " type groove array electrode in order to solve the above problems by the present invention
Method.
The present invention adopts the following technical scheme that realization：Pliable pressure sensor based on " V " type groove array electrode
Preparation method, includes the preparation and the preparation of CNT/PDMS polymer of pliable pressure sensor " V " type groove array electrode,
The preparation of pliable pressure sensor " V " type groove array electrode comprises the following steps：
The first step：Choose silicon chip and clean, remove silicon chip surface hydrocarbon, basic ion, metal pollutant；
Second step：Silicon chip after cleaning is put into baking oven and toasted, surface active, the adhesion of enhancing photoresist and silicon chip is carried out
Property；
3rd step：The even photoresist of rotation is carried out using sol evenning machine to the silicon chip after baking, front baking is carried out after spin coating；
4th step：Silicon chip photo-etching machine exposal after front baking, uses supporting developing liquid developing, and hot plate post bake；
5th step：BOE is used to corrode SiO using photoresist as mask2, obtained after removing photoresist with SiO2For mask window
First template；
6th step：First template KOH is corroded, groove and the removal of the inverted trapezoidal at some intervals are formed in silicon chip surface
SiO2；
7th step：RCA cleanings are carried out to the silicon chip of above-mentioned formation groove, and complete PECVD depositions SiO2It is prepared by layer；
8th step：Carry out second of spin coating, photoetching, BOE corrosion SiO2, obtained after removing photoresist with SiO2For mask window
Second template；
9th step：Second template KOH is corroded, " V " type groove Array microelectrode is formed in silicon chip surface and removes SiO2, obtain
Pliable pressure sensor silicon template；
Tenth step：The silicon template and polycarbonate substrate prepared are put into nano marking press sample stage, make the knot in silicon template
In structure press-in makrolon, the making of nano-imprint stamp is completed after demoulding；
11st step：Dimethyl silicone polymer is mixed with curing agent, vacuum defoamation processing is carried out after being sufficiently stirred for, deaeration is completed
Dimethyl silicone polymer is evenly coated in nano-imprint stamp surface afterwards, secondary vacuum deaeration processing is carried out, when bubble disappears completely
After mistake, it is put into baking oven and is solidified；
12nd step：By the dimethyl silicone polymer demoulding after solidification, using magnetic control sputtering device in dimethyl silicone polymer surface
Enter row metal Ag thin film sputtering process, pliable pressure sensor " V " the type groove array electrode obtained after sputtering；
The preparation of CNT/PDMS laminated films comprises the following steps：Carbon nanotube particulate is added after absolute ethyl alcohol, in ultrasound
Ultrasonic disperse in ripple washer, the localized hyperthermia produced when ultrasonic or strong shock wave, slacken the active force between nano particle, prevent
Only nanoparticle agglomerates, obtain carbon nano tube suspension, add glue PDMS polymer, are heated on baking machine, treat anhydrous second
Alcohol volatilization is complete, and the stirring of PDMS curing agent is added after cooling, places into vacuum drying oven, vacuumizes removing bubble, finally, will be de-
Mixture after bubble removing is poured into mould to be vacuumized again, solidifies obtained CNT/PDMS laminated films in an oven；
Take two pliable pressure sensors " V " type groove array electrode obtained above respectively as Top electrode and bottom electrode, carbon is received
Mitron/PDMS laminated films form pliable pressure sensor as intermediate dielectric layer, encapsulation.
The problem of for metal material and flexible substrate poor adhesion, the present invention selects dimethyl silicone polymer（PDMS）Make
For flexible substrate material, metal Ag is modified PDMS flexible substrates surface as electrode material, and using plasma techniques
Handle for strengthening metal Ag and PDMS adhesiveness, " V " type groove Array microelectrode structure of design efficiently solves flexible pressure
Force snesor metal electrode when occurring compared with large deformation produces the problem of being broken, and Jie is used as by the use of CNT/PDMS polymer
Electric layer, improves the sensitivity of sensor.
Brief description of the drawings
Fig. 1 is pliable pressure sensor parallel plate electrode preparation technology flow chart.
Fig. 2 is pliable pressure sensor silicon template surface shape appearance figure.
Fig. 3 is pliable pressure sensor silicon template lithography array of figure.
Fig. 4 is the high uniform array template Corrosion results SEM figures of " V " type groove.
Fig. 5 is wafer scale silicon microelectrode surface topography map.
Fig. 6 is the high uniform array electrode 3 d surface topography figure of " V " type groove.
Fig. 7 is the pliable pressure sensor and sensor capacitance cut-away view after encapsulation.
Fig. 8 is various sizes of pressure sensor to applying stressed response curve.
Fig. 9 is the pressure sensor capacitance variations curve map for testing different number of times.
Embodiment
Pliable pressure sensor preparation technology flow is as shown in figure 1, technique is summarized simply as follows：（1）Oxidation；（2）Photoetching；
（3）Wet etching；（4）Nano impression；（5）PDMS reverse moulds；（6）Sputtering, encapsulation.
The making of pliable pressure sensor " V " type groove array electrode
Using 4 inches of single-sided polishing<100>Face N-type oxidized silicon chip（Suzhou Rui Cai Semiconductor Co., Ltd）, resistance is 2-5 Ω,
Thickness is 500 μm.H is used respectively thousand grades of toilets2SO4（It is dense）：H2O2=3:1st, SC1 liquid, SC2 liquid are cleaned to silicon chip,
Remove surface hydrocarbon, basic ion, metal pollutant.For prevent silicon chip surface adsorb water produce in the photoresist pin hole and
Bubble causes the drift of photoresist to damage litho pattern, and silicon chip is placed into 135 DEG C of bakings in HMDS baking ovens before photoetching and entered within 1 hour
The adhesiveness of row surface active, enhancing photoresist and silicon chip.Sol evenning machine is used hundred grades of toilets（KW-4A）To positive photoresist
（MICROPOSIT S1800 G2 SERIES PHOTORESISTS）Rotation spin coating is carried out with 3000rad/min rotating speed, used
105 DEG C of hot plate carries out front baking 90s.Contact exposure, exposure dose 135mj/cm are carried out using EVG-610 types litho machine2, with
Cover developing liquid developing, developing time 40s.115 DEG C of post bake 120s of hot plate, it is therefore an objective to remove remained in post-develop photoresist molten
Agent, improves the adhesive force and corrosion resistance of photoresist.
First time corrosion is carried out after photoetching, uses BOE to corrode SiO using photoresist as mask first2, remove after photoresist
Obtain with SiO2For the first template of mask window.KOH corrodes in the first template, using DF-101T-10L thermostatted water liquid furnaces, temperature
It is ± 1 DEG C to control precision, keeps reaction temperature constant at 80 DEG C, KOH corrosive liquids volume is 1000mL in etching system, mass ratio is
40wt%, mixing speed is that 1500rad/min keeps corrosive liquid even concentration, prevents the complex compound that reaction is generated in the corruption of silicon chip
Lose surface enrichment and prevent reaction from carrying out.Corrosion carries out RCA cleanings again after terminating, complete PECVD depositions SiO2It is prepared by layer.
SiO2Layer carries out second of photoetching, corrosion after the completion of preparing, complete the system of " V " type groove Array microelectrode on parallel-plate electrode
It is standby, corrosion 22min is carried out using 15wt%TMAH+17vol%IPA in anticaustic, SiO is finally removed2Complete pliable pressure
The making of sensor silicon template, as shown in Figure 2.
By the silicon template and makrolon prepared（PC）Substrate is put into nano marking press sample stage, sets heating-up temperature
For 150 DEG C, pressure size is 0.65MPa, and soaking time is 5min, and the dwell time is 40min, and then heating is heated to PC glass
More than glass temperature soften it, repressurization makes to be taken off after keeping 40min, natural cooling in the structure press-in PC in silicon template
Film, completes nano-imprint stamp and makes.Dimethyl silicone polymer（PDMS）With curing agent according to mass ratio 10:1 is mixed,
Vacuum defoamation processing is carried out after being sufficiently stirred for.PDMS is evenly coated in nano-imprint stamp surface after the completion of deaeration, passes through spin coating
It is 300 μm that machine, which keeps thickness, carries out secondary vacuum deaeration processing.After bubble is wholly absent, it is put into baking oven and is heated to 90 DEG C
At a temperature of carry out solidification 2 hours.By the PDMS demouldings after solidification, ION40 plasma systems are utilized（plasma）Power 120W,
Throughput 150SCCM, surface treatment 20s enhancing metals Ag and PDMS adhesiveness is carried out to PDMS, magnetron sputtering is finally utilized
Base pressure maintains 8.0 × 10-3Torr or so, power to instrument (Mantis Qprep Deposition System types) in cavity
60W enters row metal Ag thin film sputtering process on PDMS surfaces, and unencapsulated pliable pressure sensor " V " type groove battle array is obtained after sputtering
Row electrode, the size of parallel-plate electrode is 9 × 9mm2, 6 × 6mm2, 3 × 3mm2。
The making of CNT/PDMS laminated films
The raw material needed for CNT/PDMS laminated films are prepared, it is 10nm-20nm mainly to have grain size, and length is 1-3
μm the CNT with alkyl（CNTs）Particle, glue PDMS polymer and PDMS curing agent.Prepared thousand grades of toilets
CNT/PDMS laminated films, clean room temperature is 20 DEG C, and relative humidity is 60%.First, certain volume fraction is weighed
CNTs is simultaneously poured into beaker, is added after a certain amount of absolute ethyl alcohol, the ultrasonic disperse in ultrasonic cleaner, the office produced when ultrasonic
Portion's high temperature or strong shock wave, can greatly slacken the active force between nano particle, effectively prevent nanoparticle agglomerates, temperature
Degree control ultrasonic 8 h at 30 DEG C, you can obtain well dispersed CNT suspension.Then, glue PDMS polymer is added,
Heated on 150 DEG C of baking machine, treat that absolute ethyl alcohol volatilization is complete, a certain proportion of curing agent stirring is added after cooling, then will
Beaker is put into vacuum drying oven, vacuumizes removing bubble about 1 h.Finally, the mixture removed after bubble is poured into mould again
Vacuumize, solidify 2h (temperature be 70 DEG C) in an oven, be so far made volume fraction be CNT that 2%, thickness is 50 μm/
PDMS laminated films.
Pliable pressure sensor silicon template pattern test
Silicon chip is by preparing pliable pressure sensor silicon mould after cleaning, spin coating, front baking, photoetching, development, post bake, wet etching
Plate, the clean structure of silicon template surface is neatly clear.Observation by light microscope lithographic results are used after photoetching, as shown in Figure 3.Can be with
Find out that " V " type groove Array microelectrode structure made by lithography has uniform lines, illustrate that photoresist is good with silicon chip adhesiveness, solve
Glue problem is floated caused by adsorbing water.In wet etching, due to there is the anisotropic etch of silicon, ultimately form（111）
Crystal face with（111）Crystal face angle is 70.52 ° " V " type groove.Corrosion uses field emission scanning electron microscope observation table after terminating
Face pattern, observed result is as shown in Figure 4.From observed result it can be seen that " V " type groove microelectrode body structure surface produced is smooth,
Cycle consistent and uniform.
The PDMS configured is evenly coated in PC templates prepare with the mutually isostructural PDMS flexible substrates of silicon template, make
Enter row metal Ag electrodes on PDMS surfaces with magnetic control sputtering device to prepare, complete pliable pressure sensor electrode and prepare, such as Fig. 5 institutes
Show, three-dimensional appearance " V " type groove structure by copolymerization Jiao's observation is highly consistent, as shown in Figure 6.
Pliable pressure sensor performance is tested
Pressure sensor is packaged by PDMS itself adhesions.It is illustrated in figure 7 the pliable pressure sensor after encapsulation
And sensor capacitance cut-away view.Three kinds of pliable pressure sensors are encapsulated in experiment, pliable pressure sensor is by upper flat
Plate electrodes, CNT/PDMS laminated films and lower parallel-plate electrode encapsulate to be formed, and CNT/PDMS laminated films are made
For intermediate dielectric layer, " V " the type groove size of parallel-plate electrode is different in every kind of pliable pressure sensor.It will be made using conductive copper films
The lead made is connected the test for carrying out output capacitance with Agilent 4156C electric impedance analyzers, uses PACE5000 pressure controls
Device processed applies pressure to sensor surface, applies the situation of change that sensor capacitance is recorded in press process.Various sizes of pressure
Force snesor is to applying stressed response curve as shown in figure 8, as a result showing, the capacitance change of sensor is with external load
Increase be in increased trend, this is due to the increase with external pressure, each " V " type electrode and bottom crown of top crown
The increase of effective active area between the reduction of the distance between " V " type electrode, each " V " type electrode and carbon nanometer
The voltage capacitance effect of pipe/PDMS laminated films causes.But, when pressure increase to a certain extent, parallel-plate electrode can be produced up and down
Raw big deformation, up and down the high shear force at parallel-plate electrode edge can not be ignored, cause the non-linear of sensor capacitance and pressure
Increase.In addition, when the parallel-plate electrode area of sensor is by 3 × 3mm2, 6 × 6 mm2Increase to 9 × 9 mm2When, sensor
Pressure-sensitivity is by 2.26%kPa-1, 3.45% kPa-1Increase to 3.98%kPa-1, this is led by the amount of deflection of parallel-plate electrode up and down
Cause.So, under identical external pressure, size is larger, and the sensitivity of sensor is of a relatively high.In actual applications, pass
The stability of sensor is that good repeatability is also very important.As shown in figure 9, carrying out 100 times, 200 to sensor respectively
Secondary, 300 times capacitance after bending is tested.As a result show, after the bend test of 300 times, in identical pressure value,
The rate of change of sensor does not change significantly, and the pressure sensor of making has good stability and good repeatability.
Simultaneously it is observed that with the increase of number of times, the capacitance of sensor has relative decline, this is the sluggishness effect by PDMS
It should cause.
Claims (1)
1. the pliable pressure sensor production method based on " V " type array electrode, it is characterised in that including pliable pressure sensor
The preparation of " V " type groove array electrode and the preparation of CNT/PDMS polymer, pliable pressure sensor " V " type groove array electricity
Pole comprises the following steps：
The first step：Choose silicon chip and clean, remove silicon chip surface hydrocarbon, basic ion, metal pollutant；
Second step：Silicon chip after cleaning is put into baking oven and toasted, surface active, the adhesion of enhancing photoresist and silicon chip is carried out
Property；
3rd step：The even photoresist of rotation is carried out using sol evenning machine to the silicon chip after baking, front baking is carried out after spin coating；
4th step：Silicon chip photo-etching machine exposal after front baking, uses supporting developing liquid developing, and hot plate post bake；
5th step：BOE is used to corrode SiO using photoresist as mask2, obtained after removing photoresist with SiO2For mask window
First template；
6th step：First template KOH is corroded, the groove of the inverted trapezoidal at some intervals is formed in silicon chip surface and SiO is removed2；
7th step：RCA cleanings are carried out to the silicon chip of above-mentioned formation groove, and complete PECVD depositions SiO2It is prepared by layer；
8th step：Carry out second of spin coating, photoetching, BOE corrosion SiO2, obtained after removing photoresist with SiO2For mask window
Second template；
9th step：Second template KOH is corroded, " V " type groove array is formed in silicon chip surface and removes SiO2, obtain flexible pressure
Force snesor silicon template；
Tenth step：The silicon template and polycarbonate substrate prepared are put into nano marking press sample stage, make the knot in silicon template
In structure press-in makrolon, the making of nano-imprint stamp is completed after demoulding；
11st step：Dimethyl silicone polymer is mixed with curing agent, vacuum defoamation processing is carried out after being sufficiently stirred for, deaeration is completed
Dimethyl silicone polymer is evenly coated in nano-imprint stamp surface afterwards, secondary vacuum deaeration processing is carried out, when bubble disappears completely
After mistake, it is put into baking oven and is solidified；
12nd step：By the dimethyl silicone polymer demoulding after solidification, using magnetic control sputtering device in dimethyl silicone polymer surface
Enter row metal Ag thin film sputtering process, pliable pressure sensor " V " the type groove array electrode obtained after sputtering；
The preparation of CNT/PDMS laminated films comprises the following steps：Carbon nanotube particulate is added after absolute ethyl alcohol, in ultrasound
Ultrasonic disperse in ripple washer, the localized hyperthermia produced when ultrasonic or strong shock wave, slacken the active force between nano particle, prevent
Only nanoparticle agglomerates, obtain carbon nano tube suspension, add glue PDMS polymer, are heated on baking machine, treat anhydrous second
Alcohol volatilization is complete, and the stirring of PDMS curing agent is added after cooling, places into vacuum drying oven, vacuumizes removing bubble, finally, will be de-
Mixture after bubble removing is poured into mould to be vacuumized again, solidifies obtained CNT/PDMS laminated films in an oven；
Take two pliable pressure sensors " V " type groove array electrode obtained above respectively as Top electrode and bottom electrode, carbon is received
Mitron/PDMS laminated films form pliable pressure sensor as intermediate dielectric layer, encapsulation.
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