CN109399556A - A kind of preparation method of the flexible micro-nano pressure sensor based on mode of printing - Google Patents
A kind of preparation method of the flexible micro-nano pressure sensor based on mode of printing Download PDFInfo
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- CN109399556A CN109399556A CN201811091480.1A CN201811091480A CN109399556A CN 109399556 A CN109399556 A CN 109399556A CN 201811091480 A CN201811091480 A CN 201811091480A CN 109399556 A CN109399556 A CN 109399556A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- 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
- B81C1/00349—Creating layers of material on a substrate
- B81C1/0038—Processes for creating layers of materials not provided for in groups B81C1/00357 - B81C1/00373
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B81B2201/0264—Pressure sensors
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Abstract
The preparation method of the present invention relates to a kind of flexible micro-nano pressure sensor based on mode of printing; the method constructs micro-nano layer and conductive layer: micro-nano layer by by the film of designed micro-nano pattern with polyacrylonitrile film is exposed, development treatment obtains the solidification photoresists with micro-nano structure; and the unprotected region N of energy dissolving films; dinethylformamide is partly melt through etching; it is ultrasonically treated again; cured photoresists are removed, the film with concaveconvex structure is obtained；Multi-walled carbon nanotube is then attached on film by conductive layer by liquid phase method by lifting mode, and carries out device assembling using opposite two-by-two.This method obtains a kind of controllable and easy to operate micro-nano structure by simple technique, cheap cost, this method has augmented the blank of micro-nano sensor process technique study, realizes that the manufacture of large area industrialization pliable pressure sensor has important research and application value to it.
Description
Technical field
The invention belongs to sensor technical field, especially a kind of flexible micro-nano pressure sensor based on mode of printing
Preparation method.
Background technique
It the use of flexibility function material production electronic device is current research hotspot, but there is also the systems of such as nano material
Standby complicated, at high price, unstable, the effect of organic semiconducting materials structure, which are paid no attention to, to be thought of same material molecular weight difference etc. and asks
Topic.The selection of polymer material is more single, is generally used together with nano material with organic semiconducting materials, as flexible liner
Bottom or intermediate material are more.And high, electrochemical conditions harshness is required for chemical deposition ambient in the method for attachment, use process
In pollutant process it is time-consuming and laborious, it is high that requirement for equipment is deposited, and can not achieve extensive, but plating can generally reach
The experiment effect of relative ideal, but lower for industrialized production referential, for ink-jet mode its to ink and set
Standby is more demanding, is favored because inkjet printing is theoretically able to achieve large-scale addition production method by researcher, grinds in recent years
Study carefully for exploitation can not blocking sprayer and environmental-friendly functional ink be the hot spot of its research be also difficult point, and the mode transferred is then
Be by various silicon substrate templates by with micro-nano structure dielectric layer or piezoelectric layer be transferred in conductive layer or flexible substrate,
This method requires height for the production and selection of template, and silica-base material patterning is generally divided into chemical method and physical method, and chemistry is logical
Chemical reagent corrosion is crossed, the method controllability is poor, and environmental factor dependence is stronger, and physical laws are etched by High-performance lasers,
High requirement is proposed for equipment.And be concentrated mainly in the research of material in the research of entire pliable pressure sensor, greatly
It is mostly performance in the sensor to the combination research of various functional materials or functional material performance boost research, about
The technical study of building process is relatively fewer.
Compared to traditional production method, the advantage that printing process prepares pressure sensor is: the importing of printing technology
Simplify process for manufacturing electronic product and period；Compared to conventional method, this method can greatly reduce the pollution of environment, while technique
Controllability also reinforced；Final products are frivolous, flexible, reduce volume and weight, realize the characteristic of flexibility；It saves
Expect saving of labor, reduces cost；Pliable pressure sensor polymer material, nano material, organic semiconducting materials etc., in maximum journey
The demand that flexibility is realized on degree can shorten the production cycle compared to chemical etching method, and machining process is simple；Green
Production, favorable environment protection；Printed electronics production waste is few, belongs to the increasing material manufacturing required on demand, is a clean manufacturing
Technology；Push the transition and upgrade of printing enterprise；Printing Industry is generally concentrated at the basic livings such as packaging, books, fabric use
Product field, estate income are relatively low compared to the electronic field at high tip, and the development of printed electronic is then to a certain extent
Printing Industry is redefined.
By retrieval, patent publication us relevant to present patent application is not yet found.
Summary of the invention
It is an object of the invention to provide a kind of flexible micro-nano based on mode of printing in place of overcome the deficiencies in the prior art
The preparation method of pressure sensor, this method use for reference the pressure sensing of printing plate manufacturing process production micro-nano structure in flexographic printing
Device obtains a kind of controllable and easy to operate micro-nano structure by simple technique, cheap cost, and this method has augmented micro-nano
The blank of sensor process technique study realizes that the manufacture of large area industrialization pliable pressure sensor has important grind to it
Study carefully and application value.
The present invention solves its technical problem and adopts the following technical solutions to achieve:
A kind of preparation method of the flexible micro-nano pressure sensor based on mode of printing, the method is to micro-nano layer and conduction
Layer is constructed:
Micro-nano layer by the way that the film of designed micro-nano pattern is exposed with polyacrylonitrile film, development treatment obtains
To the solidification photoresists with micro-nano structure, and unprotected region is carried out with the n,N-Dimethylformamide of energy dissolving films
Partly be melt through etching, then is ultrasonically treated to it, removes cured photoresists, obtains the film with concaveconvex structure；Conductive layer
Multi-walled carbon nanotube is attached on film by liquid phase method by lifting mode then, and carries out device group using opposite two-by-two
Dress, obtains the flexible micro-nano pressure sensor based on mode of printing.
Moreover, steps are as follows:
(1) the production of transparent PAN film；
(2) micro-nano patterning is realized；
(3) the dispersion of carbon nanotube；
(4) the attachment of carbon nanotube；
(5) the encapsulation of sensor.
Moreover, the step (1) in the production of transparent PAN film specific step is as follows:
0.5g, 1g, 1.5g, 2g, 3g, 4g polyacrylonitrile solid powder are weighed by electronic balance, is respectively put into 6
Spare in 100mL beaker, adhesive label paper is to show difference；The DMF of 50ml is separately added into load weighted polyacrylonitrile beaker
Solution, and solution is put in water-bath and carries out heating water bath, temperature is set as 70 DEG C, to guarantee that DMF can cmpletely dissolve
Powder, setting time are 1 hour；By dissolved yellow solution, 15ml is taken to pour into the glass plate of 12 × 12cm respectively, and
Glass plate is placed in draught cupboard and is heated, to guarantee that rate of volatilization is gentle, sets heating temperature as 45 DEG C, PAN is molten
Solvent volatilization in liquid, finally obtains the transparent PAN film of different-thickness.
Moreover, (2) micro-nano patterning realizes that specific step is as follows to the step:
By step, (1) transparent PAN film obtained attaches to by polyimides double faced adhesive tape the sheet glass of 2.5 × 8cm
On；One layer of photoresists will be coated on sheet glass in a dark environment, it is 65 DEG C dry that the sheet glass of coating, which is put into set temperature,
It is dried in dry case；By after drying film and designed patterning film carry out it is compound；To the compound film and thin
Film is exposed processing；Film after exposure is rinsed in clear water, will have after cleaning solidify the films of photoresists into
Row naturally dry；By what is obtained there is the film for solidifying photoresists to carry out DMF etching, using diluted DMF solution on film
Coating is volatilized by 50 DEG C of heating, obtains having etching depth and solidify the film of photoresists；To have etching depth and solidification
The film of photoresists is ultrasonically treated in ultrasonic disperse machine, and removal solidification photoresists obtain the PAN film of micro-nano structure.
Moreover, described in a dark environment by the photoresists on sheet glass in one layer of photoresists of coating with a thickness of 50 ± 5 μ
m；The mass concentration of the diluted DMF solution is 3%；The sonication treatment time control is in 1 ± 0.2h.
Moreover, specific step is as follows for the dispersion of the step (3) carbon nanotube:
Weigh the multi-walled carbon nanotube of 5 parts of different qualities with electronic balance, quality be respectively 0.1mg, 0.2mg,
0.3mg,0.4mg,0.5mg；Being mixedly configured into concentration with DMF solution and weighed 5 parts of multi-wall carbon nano-tube pipe powders is 0.1mg/
The initial soln of ml, 0.2mg/ml, 0.3mg/ml, 0.4mg/ml, 0.5mg/ml；By configured solution on magnetic stirring apparatus
Carry out tentatively being dispersed with stirring for 1h；The solution being stirred is put into the ultrasonic disperse for carrying out 12h in ultrasonic disperse machine, obtains multi wall
Carbon nano tube dispersion liquid, for use.
Moreover, specific step is as follows for the attachment of the step (4) carbon nanotube:
(3) multi-walled carbon nanotube dispersion liquid that step obtains is centrifuged 10min under conditions of 2000r/min, after taking centrifugation
Supernatant liquor, be slowly added dropwise into the beaker equipped with deionized water of 250ml, formed in water and Air Interface uniform, thoroughly thin
Multi-walled carbon nanotube conductive layer；Sided corona treatment is carried out to the PAN film of (2) micro-nano structure that step obtains, increases its surface
Can, it prepares for carbon nanotube attachment；It with micro-nano structure and the film on glass will be attached to slowly is inserted into water, with 45 °
Angle slowly lifts thin slice, and the carbon nanotube layer on surface is allowed to be attached on film；The film of multi-walled carbon nanotube will be attached with
In an oven with the deionized water on its surface of 60 DEG C of temperature heating evaporation；The film for needing to adhere to 2 layers or more is repeated above-mentioned
Step；
To guarantee rate of addition in whole process, remain a constant speed, be added dropwise from the edge close to beaker, while lifting
Guarantee that slowly hand is not shaken in journey, shake is easy the aggregation for the fracture or attachment for adhering to conductive layer, guarantees external environment
It is clean and closed.
Moreover, specific step is as follows for the encapsulation of the step (5) sensor:
It is obtaining with micro-nano structure and after being attached to the film of conductive layer, will sticked by polyimides double faced adhesive tape
Film on glass is attached in transparent PVC film, and two measurement electricity are drawn by copper foil in the both sides of the layer film
Pole, will have mutually isostructural MWCNTs/PAN/PVC/ copper foil membrane by sandwich structure facing each other assemble to get
To the final flexible micro-nano pressure sensor based on mode of printing.
It is sensed made from the preparation method of the flexible micro-nano pressure sensor based on mode of printing as described above
Application of the device in pressure change context of detection.
Moreover, the application be medical detection, physical training, sealing propertytest field pressure change context of detection in
Application.
The advantages of present invention obtains and good effect are:
1, the method for the present invention uses for reference the pressure sensor of printing plate manufacturing process production micro-nano structure in flexographic printing, passes through letter
Technique, the cheap cost of list obtain a kind of controllable and easy to operate micro-nano structure, and this method has augmented micro-nano sensor work
The blank of process research realizes that the manufacture of large area industrialization pliable pressure sensor has important research and application to it
Value.
2, the importing of printing technology simplifies process for manufacturing electronic product and period；It can be with compared to conventional method the method for the present invention
The pollution of environment is greatly reduced, while the controllability of technique is also reinforced；Final products are frivolous, flexible, reduce volume
With weight, the characteristic of flexibility is realized；Material-saving saving of labor reduces cost；Pliable pressure sensor polymer material, nanometer material
Material, organic semiconducting materials etc. realize the demand of flexibility to the full extent, can shorten production compared to chemical etching method
Period, and machining process is simple；Green production, favorable environment protection；Printed electronics production waste is few, belongs on demand
It is required that increasing material manufacturing, be a process for cleanly preparing technology；Push the transition and upgrade of printing enterprise；Printing Industry is generally concentrated at
The basic livings articles such as packaging, books, fabric field, estate income are relatively low compared to the electronic field at high tip, and print
The development of brush electronics then to a certain extent redefines Printing Industry.
3, the method for the present invention is mainly the flexible compression layer that a kind of wiener structure is constructed by way of printing, then by leading
The attachment of electric layer obtains the pressure sensor of " sandwich ".The present invention mainly obtains patterned wiener knot by new mode
Structure, carries out pressure sensor production, and the main technique by using for reference printing plate production in offset printing obtains the wiener of concaveconvex structure
Layer, then conductive layer is attached to patterned micro-nano structure layer by way of lifting compound obtains micro-nano by two layers
The structure of layer/conductive layer, then micro-nano layer/conductive layer composite layer protection insulation is got up by protective layer, and by opposite two-by-two
Mode, it is compound by two layers of same structure, be aided with test electrode obtain final device.This method is by changing two conductions
The contact area of layer realizes the variation of resistance, reaches the detection function of device.
The measurement of device is obtained: there is best spirit when micro-nano shape is diamond shape, and micro-nano cell spacing is 90 microns
Sensitivity, the sensitivity of low pressure area are 0.458kPa-1, High Voltage area is then 0.033kPa-1, response time 0.032s, and
For the device of final molding, its transmissivity is then 60% or so.
Detailed description of the invention
Fig. 1 is the comparison diagram of the sensitivity of different micro-nano shapes and different spacing in the present invention；
Fig. 2 is that difference adheres to the numbers of plies to the influence diagram of resistance in the present invention；
Fig. 3 is the stability test figure of device made from the method for the present invention；
Fig. 4 is sampling time partial enlarged view in the present invention.
Specific embodiment
Below with reference to the invention will be further described by specific embodiment, following embodiment be it is descriptive, no
It is restrictive, this does not limit the scope of protection of the present invention.
Raw material used in the present invention is unless otherwise specified conventional commercial product；Used in the present invention
Method is unless otherwise specified the conventional method of this field.
Embodiment 1
A kind of preparation method of the flexible micro-nano pressure sensor based on mode of printing, steps are as follows:
(1) 0.5g, 1g, 1.5g, 2g, 3g, 4g polyacrylonitrile solid powder are weighed with electronic balance, is respectively put into 6
Spare in 100mL beaker, adhesive label paper is to show difference；The DMF of 50ml is separately added into load weighted polyacrylonitrile beaker
Solution, and solution is put in water-bath and carries out heating water bath, temperature is set as 70 DEG C, to guarantee that DMF can cmpletely dissolve
Powder, setting time are 1 hour；By dissolved yellow solution, 15ml is taken to pour into the glass of 12 × 12cm with graduated cylinder respectively
In plate, and glass plate is placed in draught cupboard and is heated；By heater plate, the solvent in PAN solution volatilizees, most
The transparent membrane of different-thickness is obtained eventually.To guarantee that rate of volatilization is gentle, heating temperature is set as 45 DEG C.
(2) obtained transparent membrane is attached on the sheet glass of 2.5 × 8cm by polyimides double faced adhesive tape；Black
One layer of photoresists of very thin (50 μm or so best) will be coated in dark situation on sheet glass, the sheet glass of coating is put into setting temperature
It is dried in the drying box that degree is 65 DEG C；By after drying film and designed patterning film carry out it is compound；To multiple
The film and film of conjunction are exposed processing；Film after exposure is rinsed in clear water, will there is solidification sense after cleaning
The film of optical cement carries out naturally dry；By what is obtained there is the film for solidifying photoresists to carry out DMF etching, uses diluted DMF
Solution (mass concentration is that 3% effect is best) coats on film, is volatilized by 50 DEG C of heating, obtains with etching depth and consolidate
The film of allelopathic optical cement；By with etching depth and solidify photoresists film be ultrasonically treated in ultrasonic disperse machine (control
System is in 1h or so).Removal solidification photoresists, obtain the PAN film of micro-nano structure.
(3) weigh the multi-walled carbon nanotube of 5 parts of different qualities with electronic balance, quality be respectively 0.1mg, 0.2mg,
0.3mg,0.4mg,0.5mg；Being mixedly configured into concentration with DMF solution and weighed 5 parts of multi-wall carbon nano-tube pipe powders is 0.1mg/
The initial soln of ml, 0.2mg/ml, 0.3mg/ml, 0.4mg/ml, 0.5mg/ml；By configured solution on magnetic stirring apparatus
Carry out tentatively being dispersed with stirring for 1h；The solution being stirred is put into the ultrasonic disperse for carrying out 12h in ultrasonic disperse machine, obtains multi wall
Carbon nano tube dispersion liquid is stand-by.
(4) obtained multi-walled carbon nanotube dispersion liquid is centrifuged 10min under conditions of 2000r/min, after centrifugation
Solution draws supernatant liquor with liquid-transfering gun, is slowly added dropwise into the beaker equipped with deionized water of 250ml, in water and Air Interface
Form uniform, saturating thin multi-walled carbon nanotube conductive layer；Sided corona treatment is carried out to the film with micro-nano structure, increases its surface
Can, it prepares for carbon nanotube attachment；It with micro-nano structure and the film on glass will be attached to slowly is inserted into water, with 45 °
Angle slowly lifts thin slice, and the carbon nanotube layer on surface is allowed to be attached on film；The film of multi-walled carbon nanotube will be attached with
In an oven with the deionized water on its surface of 60 DEG C of temperature heating evaporation；It repeats the above steps to 2 layers and 3 layers of film of attachment
?.To guarantee rate of addition in whole process, remain a constant speed as far as possible, be added dropwise as far as possible from the edge close to glass beaker, together
When during lifting as far as possible guarantee slowly, hand do not shake (shake be easy the fracture or attachment for adhering to conductive layer gather
Collection) guarantee the clean and closed of external environment as far as possible.
(5) it is obtaining with micro-nano structure and after being attached to the film of conductive layer, it is glutinous by polyimides double faced adhesive tape
The film being attached on glass is attached in transparent PVC film, and two measurements are drawn by copper foil in the both sides of the layer film
Electrode will have mutually isostructural MWCNTs/PAN/PVC/ copper foil membrane to assemble by " sandwich " structure facing each other
Final device is obtained to get the final flexible micro-nano pressure sensor based on mode of printing is arrived.
Embodiment 2
A kind of preparation method of the flexible micro-nano pressure sensor based on mode of printing, the method is to micro-nano layer and conduction
Layer is constructed:
Micro-nano layer by the way that the film of designed micro-nano pattern is exposed with polyacrylonitrile film, development treatment obtains
To the solidification photoresists with micro-nano structure, and unprotected region is carried out with the n,N-Dimethylformamide of energy dissolving films
Partly be melt through etching, then is ultrasonically treated to it, removes cured photoresists, obtains the film with concaveconvex structure；Conductive layer
Multi-walled carbon nanotube is attached on film by liquid phase method by lifting mode then, and carries out device group using opposite two-by-two
Dress, obtains the flexible micro-nano pressure sensor based on mode of printing.
More preferably, steps are as follows:
(1) the production of transparent PAN film；
(2) micro-nano patterning is realized；
(3) the dispersion of carbon nanotube；
(4) the attachment of carbon nanotube；
(5) the encapsulation of sensor.
More preferably, the step (1) in the production of transparent PAN film specific step is as follows:
0.5g, 1g, 1.5g, 2g, 3g, 4g polyacrylonitrile solid powder are weighed by electronic balance, is respectively put into 6
Spare in 100mL beaker, adhesive label paper is to show difference；The DMF of 50ml is separately added into load weighted polyacrylonitrile beaker
Solution, and solution is put in water-bath and carries out heating water bath, temperature is set as 70 DEG C, to guarantee that DMF can cmpletely dissolve
Powder, setting time are 1 hour；By dissolved yellow solution, 15ml is taken to pour into the glass plate of 12 × 12cm respectively, and
Glass plate is placed in draught cupboard and is heated, to guarantee that rate of volatilization is gentle, sets heating temperature as 45 DEG C, PAN is molten
Solvent volatilization in liquid, finally obtains the transparent PAN film of different-thickness.
More preferably, (2) micro-nano patterning realizes that specific step is as follows to the step:
By step, (1) transparent PAN film obtained attaches to by polyimides double faced adhesive tape the sheet glass of 2.5 × 8cm
On；One layer of photoresists will be coated on sheet glass in a dark environment, it is 65 DEG C dry that the sheet glass of coating, which is put into set temperature,
It is dried in dry case；By after drying film and designed patterning film carry out it is compound；To the compound film and thin
Film is exposed processing；Film after exposure is rinsed in clear water, will have after cleaning solidify the films of photoresists into
Row naturally dry；By what is obtained there is the film for solidifying photoresists to carry out DMF etching, using diluted DMF solution on film
Coating is volatilized by 50 DEG C of heating, obtains having etching depth and solidify the film of photoresists；To have etching depth and solidification
The film of photoresists is ultrasonically treated in ultrasonic disperse machine, and removal solidification photoresists obtain the PAN film of micro-nano structure.
More preferably, the photoresists that will be coated on sheet glass in one layer of photoresists in a dark environment with a thickness of 50 ±
5μm；The mass concentration of the diluted DMF solution is 3%；The sonication treatment time control is in 1 ± 0.2h.
More preferably, specific step is as follows for the dispersion of the step (3) carbon nanotube:
Weigh the multi-walled carbon nanotube of 5 parts of different qualities with electronic balance, quality be respectively 0.1mg, 0.2mg,
0.3mg,0.4mg,0.5mg；Being mixedly configured into concentration with DMF solution and weighed 5 parts of multi-wall carbon nano-tube pipe powders is 0.1mg/
The initial soln of ml, 0.2mg/ml, 0.3mg/ml, 0.4mg/ml, 0.5mg/ml；By configured solution on magnetic stirring apparatus
Carry out tentatively being dispersed with stirring for 1h；The solution being stirred is put into the ultrasonic disperse for carrying out 12h in ultrasonic disperse machine, obtains multi wall
Carbon nano tube dispersion liquid, for use.
More preferably, specific step is as follows for the attachment of the step (4) carbon nanotube:
(3) multi-walled carbon nanotube dispersion liquid that step obtains is centrifuged 10min under conditions of 2000r/min, after taking centrifugation
Supernatant liquor, be slowly added dropwise into the beaker equipped with deionized water of 250ml, formed in water and Air Interface uniform, thoroughly thin
Multi-walled carbon nanotube conductive layer；Sided corona treatment is carried out to the PAN film of (2) micro-nano structure that step obtains, increases its surface
Can, it prepares for carbon nanotube attachment；It with micro-nano structure and the film on glass will be attached to slowly is inserted into water, with 45 °
Angle slowly lifts thin slice, and the carbon nanotube layer on surface is allowed to be attached on film；The film of multi-walled carbon nanotube will be attached with
In an oven with the deionized water on its surface of 60 DEG C of temperature heating evaporation；The film for needing to adhere to 2 layers or more is repeated above-mentioned
Step；
To guarantee rate of addition in whole process, remain a constant speed, be added dropwise from the edge close to beaker, while lifting
Guarantee that slowly hand is not shaken in journey, shake is easy the aggregation for the fracture or attachment for adhering to conductive layer, guarantees external environment
It is clean and closed.
More preferably, specific step is as follows for the encapsulation of the step (5) sensor:
It is obtaining with micro-nano structure and after being attached to the film of conductive layer, will sticked by polyimides double faced adhesive tape
Film on glass is attached in transparent PVC film, and two measurement electricity are drawn by copper foil in the both sides of the layer film
Pole, will have mutually isostructural MWCNTs/PAN/PVC/ copper foil membrane by sandwich structure facing each other assemble to get
To the final flexible micro-nano pressure sensor based on mode of printing.
It is sensed made from the preparation method of the flexible micro-nano pressure sensor based on mode of printing as described above
Application of the device in pressure change context of detection.
More preferably, the application be medical detection, physical training, sealing propertytest field pressure change context of detection
In application.
Coherent detection of the invention:
The contrasting detection of the sensitivity of different micro-nano shapes and different spacing, the different attachment numbers of plies are to resistance in the present invention
The stability test of device made from detection, the method for the present invention is influenced, which can be used this field
Interior conventional method is detected, therefore the present invention is not described in detail.
When micro-nano shape is diamond shape, and micro-nano cell spacing is 90 microns, there is optimum sensitivity, low pressure area is sensitive
Degree is 0.458kPa-1, High Voltage area is then 0.033kPa-1, response time 0.032s, and for the device of final molding
Its transmissivity is then 60% or so.
From figure 1 it appears that sensitivity is tended towards stability afterwards as the increase of pressure first increases, mainly due to
The increase of pressure, the power for acting on device surface is continuously increased, and forced area has not been changed, decrement not up to compress it is full
And when, conductive layer contacts rapidly, and resistance value rapidly changes, i.e. sensitivity relative increase is very fast, when pressure increase to certain value,
Two conductive layers contact is more and more closer, and resistance no longer changes substantially.Therefore low pressure range high sensitivity is in High Voltage range.From
It can be found that the sensitivity of low-pressure area and higher-pressure region when spacing is 90 microns, and micro-nano pattern is diamond shape all reaches in data
Similar maximum value.And the shape of low-pressure area micro-nano structure is affected to sensitivity, and higher-pressure region is substantially unrelated with shape, and
The sensitivity of higher-pressure region and spacing correlation are larger.Mainly since being under pressure for low-pressure area micro-nano structure generates the more of deformation
It is few larger with the relationship of micro-nano structure, and reached in higher-pressure region since the compression of micro-nano structure has reached the i.e. contact area of saturation
Maximum is arrived, the resistance of conductive layer no longer changes or varies less.
As can be seen from Figure 2 adhere to the device of the identical conduction number of plies, resistance overall variation amount is essentially identical, with micro-nano
Structural relation correlation is smaller, and mainly since when compression reaches saturation, i.e., conductive layer contact is complete, resistance is not changing,
It could also be possible that diamond shape is more similar to square configuration, therefore the influence of micro-nano shape is unobvious, and leads for adhering to the different numbers of plies
The device of electric layer, two layers the variable quantity of resistance is also big when Datong District than adhering to three layers of resistance starting resistance for attachment, mainly by
It is big compared to three layers in two layers of resistance, therefore two layers to three layer of starting resistance is big, and than three layers adhesive layer entirety of two layers of adhesive layer
Variable quantity is big, and mainly not close compared to what three-layered node closed due to two layers of adhesive layer, the resistance of beginning is with regard to big, when the pressure is exerted
The variable quantity of the conductive layer contact area of two layers of adhesive layer is bigger than three layers, therefore whole two layers to three layer of adhesive layer of resistance change
Greatly.
From figure 3, it can be seen that maintain good consistency in low-pressure area device, in higher-pressure region, the stability of device is not
Such as area of low pressure, under low voltage situations, the contact of conductive layer is also insufficient, and the change of decrement can guarantee conductive layer well
Changes in contact is conductive layer due to using multi-walled carbon nanotube, in high pressure feelings when reaching higher-pressure region with the increase of pressure
Under condition, conductive layer, which is likely to occur, to be pressed into recess, or even the tomography of part occurs, leads to the unstable of resistance.But on the whole
As can be seen that the variation of its repetition experiment resistance carried out has good consistency, therefore stability is preferable.
The detection method in sampling time is as follows in the present invention: microcomputer control universal electrical test machine, can record and applies object
Pressure, the variation of the decrement of object and corresponding time, wherein one group of data (diamond shape, 90 micro-nano spacing, 2 layers of adhesive layer) is logical for selection
Abscissa will be set as the time by crossing in origin software, ordinate value is set as 1, and ordinate is meaningless herein, be only mapping
It needs, partial enlargement, the time precision responded then is carried out to abscissa.As a result as shown in Figure 4.
By in Fig. 4 as can be seen that calculate the microcomputer control universal electrical test machine sampling minimum time be 0.032s,
Then the time is denoted as the response time of micro-nano sensor, i.e. the response time of the micro-nano sensor is 0.032s.
Although disclosing the embodiment of the present invention for the purpose of illustration, it will be appreciated by those skilled in the art that: not
Be detached from the present invention and spirit and scope of the appended claims in, various substitutions, changes and modifications be all it is possible, therefore, this
The range of invention is not limited to the embodiment disclosure of that.
Claims (10)
1. a kind of preparation method of the flexible micro-nano pressure sensor based on mode of printing, it is characterised in that: the method is to micro-
It receives layer and conductive layer is constructed:
Micro-nano layer by the way that the film of designed micro-nano pattern is exposed with polyacrylonitrile film, development treatment is had
There are the solidification photoresists of micro-nano structure, and unprotected region carries out fritting with the n,N-Dimethylformamide of energy dissolving films
Logical etching, then it is ultrasonically treated, cured photoresists are removed, the film with concaveconvex structure is obtained；Conductive layer then leads to
It crosses liquid phase method and is attached to multi-walled carbon nanotube on film by lifting mode, and carry out device assembling using opposite two-by-two, obtain
To the flexible micro-nano pressure sensor based on mode of printing.
2. the preparation method of the flexible micro-nano pressure sensor according to claim 1 based on mode of printing, feature exist
In: steps are as follows:
(1) the production of transparent PAN film；
(2) micro-nano patterning is realized；
(3) the dispersion of carbon nanotube；
(4) the attachment of carbon nanotube；
(5) the encapsulation of sensor.
3. the preparation method of the flexible micro-nano pressure sensor according to claim 2 based on mode of printing, feature exist
In: the step (1) in the production of transparent PAN film specific step is as follows:
0.5g, 1g, 1.5g, 2g, 3g, 4g polyacrylonitrile solid powder are weighed by electronic balance, is respectively put into 6 100mL
Spare in beaker, adhesive label paper is to show difference；The DMF solution of 50ml is separately added into load weighted polyacrylonitrile beaker,
And solution is put in water-bath and carries out heating water bath, temperature is set as 70 DEG C, for guarantee DMF can cmpletely dissolved powders,
Setting time is 1 hour；By dissolved yellow solution, 15ml is taken to pour into the glass plate of 12 × 12cm respectively, and by glass
Glass plate, which is placed in draught cupboard, to be heated, and to guarantee that rate of volatilization is gentle, sets heating temperature as 45 DEG C, in PAN solution
Solvent volatilization, finally obtain the transparent PAN film of different-thickness.
4. the preparation method of the flexible micro-nano pressure sensor according to claim 2 based on mode of printing, feature exist
In: (2) micro-nano patterning realizes that specific step is as follows to the step:
By step, (1) transparent PAN film obtained is attached on the sheet glass of 2.5 × 8cm by polyimides double faced adhesive tape；?
One layer of photoresists will be coated on sheet glass in dark surrounds, the sheet glass of coating is put into the drying box that set temperature is 65 DEG C
It is dried；By after drying film and designed patterning film carry out it is compound；The compound film and film are carried out
Exposure-processed；Film after exposure is rinsed in clear water, will there is the film for solidifying photoresists to carry out nature after cleaning
It dries；By what is obtained there is the film for solidifying photoresists to carry out DMF etching, is coated, led on film using diluted DMF solution
50 DEG C of heating volatilizations are crossed, obtains that there is etching depth and solidifies the film of photoresists；To have etching depth and solidification photoresists
Film be ultrasonically treated in ultrasonic disperse machine, removal solidification photoresists, obtain the PAN film of micro-nano structure.
5. the preparation method of the flexible micro-nano pressure sensor according to claim 4 based on mode of printing, feature exist
In: it is described in a dark environment by the photoresists on sheet glass in one layer of photoresists of coating with a thickness of 50 ± 5 μm；The dilution
DMF solution mass concentration be 3%；The sonication treatment time control is in 1 ± 0.2h.
6. the preparation method of the flexible micro-nano pressure sensor according to claim 2 based on mode of printing, feature exist
In the dispersion of: the step (3) carbon nanotube, specific step is as follows:
Weigh the multi-walled carbon nanotube of 5 parts of different qualities with electronic balance, quality be respectively 0.1mg, 0.2mg, 0.3mg,
0.4mg,0.5mg；With DMF solution and weighed 5 parts of multi-wall carbon nano-tube pipe powders be mixedly configured into concentration be 0.1mg/ml,
The initial soln of 0.2mg/ml, 0.3mg/ml, 0.4mg/ml, 0.5mg/ml；Configured solution is enterprising in magnetic stirring apparatus
Row 1h's is tentatively dispersed with stirring；The solution being stirred is put into the ultrasonic disperse for carrying out 12h in ultrasonic disperse machine, obtains multi wall carbon
Nanotube dispersion liquid, for use.
7. the preparation method of the flexible micro-nano pressure sensor according to claim 2 based on mode of printing, feature exist
In the attachment of: the step (4) carbon nanotube, specific step is as follows:
(3) multi-walled carbon nanotube dispersion liquid that step obtains is centrifuged 10min under conditions of 2000r/min, it is upper after taking centrifugation
Layer clear liquid, is slowly added dropwise into the beaker equipped with deionized water of 250ml, is formed in water and Air Interface uniform, saturating thin more
Wall carbon nano tube conductive layer；Sided corona treatment is carried out to the PAN film of (2) micro-nano structure that step obtains, increases its surface energy, is
Carbon nanotube attachment is prepared；It with micro-nano structure and the film on glass will be attached to slowly is inserted into water, it is slow with 45° angle degree
Thin slice is slowly lifted, the carbon nanotube layer on surface is allowed to be attached on film；The film of multi-walled carbon nanotube will be attached in baking oven
In with the deionized water on its surface of 60 DEG C of temperature heating evaporation；It repeats the above steps i.e. to the film for needing to adhere to 2 layers or more
It can；
To guarantee rate of addition in whole process, remain a constant speed, be added dropwise from the edge close to beaker, while during lifting
Guarantee that slowly hand is not shaken, shake is easy the aggregation for the fracture or attachment for adhering to conductive layer, guarantees the dry of external environment
It is net and closed.
8. according to the preparation method of the described in any item flexible micro-nano pressure sensors based on mode of printing of claim 2 to 7,
It is characterized by: specific step is as follows for the encapsulation of the step (5) sensor:
It is obtaining with micro-nano structure and after being attached to the film of conductive layer, glass will be attached on by polyimides double faced adhesive tape
Film on glass is attached in transparent PVC film, and two measuring electrodes are drawn by copper foil in the both sides of the layer film, will
It is assembled with mutually isostructural MWCNTs/PAN/PVC/ copper foil membrane by sandwich structure facing each other to get to most
The whole flexible micro-nano pressure sensor based on mode of printing.
9. the preparation of the flexible micro-nano pressure sensor based on mode of printing as claimed in any one of claims 1 to 8
Application of the sensor made from method in pressure change context of detection.
10. being passed made from the preparation method of the flexible micro-nano pressure sensor according to claim 9 based on mode of printing
Application of the sensor in terms of detecting pressure change, it is characterised in that: the application is in medical detection, physical training, leakproofness
Application in the pressure change context of detection of detection field.
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