CN108493338A - A kind of extendable buckling structure organic film function element and preparation method thereof - Google Patents
A kind of extendable buckling structure organic film function element and preparation method thereof Download PDFInfo
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- CN108493338A CN108493338A CN201810166241.1A CN201810166241A CN108493338A CN 108493338 A CN108493338 A CN 108493338A CN 201810166241 A CN201810166241 A CN 201810166241A CN 108493338 A CN108493338 A CN 108493338A
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- H—ELECTRICITY
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- H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having a potential-jump barrier or a surface barrier
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- H—ELECTRICITY
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Abstract
The invention discloses a kind of extendable buckling structure organic film function elements and preparation method thereof, are three-decker, and top layer is Au electrodes, and middle layer is organic function layer, and bottom is Au electrodes.Preparation method includes the following steps：（1）Prepare PVA and organic function layer solution；（2）It is prepared by sacrificial layer；（3）It is prepared by bottom electrode；（4）It is prepared by organic function layer；（5）It is prepared by top layer electrode；（6）Device micro Process；（7）Device is removed；（8）Transfer, unloads to obtain the final product.The present invention is using PVA as sacrificial layer, by the buckling degree for controlling the pre-tensioned adjustable control film of flexible substrate in transfer process（Period and amplitude）, to make device realize the functionality of organic film and have both ductility.PVA is can dissolve as sacrificial layer water to realize the transfer of device, nontoxic lossless, easy to operate, and without using expensive special equipment, cost substantially reduces and environmentally friendly.
Description
Technical field
The present invention relates to flexible electronic fields, specifically, being related to a kind of extendable buckling structure organic film function
Device and preparation method thereof.
Background technology
Flexible electronic device with its unique bending, stretches, folding characteristic, in biologic medical, military project space flight, information energy
The every field such as source all have very wide application prospect, such as wearable electronic, electronic skin health monitoring, flexibility
Solar cell etc..Research shows that its functional unit of flexible electronic product is based on inorganic material, such as Feng Xue more at present
Group prepares the ultrathin flexible PZT energy harvesters that can be integrated in and collect energy in biological tissue, and Juejun Hu groups are prepared soft
Property inorganic semiconductor light emitting diode matrix, is also prepared in complete detector (artificial compound eye, the artificial view of flexible substrate
Film) etc..It is difficult to overcome however, inorganic flexible electronic still has a disadvantage that：The intrinsic rigidity of inorganic material structure so that its
Fracture damage is inevitably easy to happen during bend tension, device is fragile and prepares difficulty raising；Inorganic material
600 ~ 1000 DEG C of even higher annealing temperatures are generally required, flexible substrate can not be directly integrated in, needed by a series of
Fine processing method：Such as the methods of sputtering, high-precision photoetching, wet etching, dry etching, process complex process, cost
High, agents useful for same has certain risk, will also result in larger burden to environment.Therefore, inorganic flexible device still there are many
Problems demand solves, and can yet be regarded as a kind of immediately possible method instead of inorganic functional layer using organic material.
Organic polymer has good flexibility, is combined with flexible substrates more preferably, annealing temperature is lower, and processing method is more
It is safe and simple.But flexible organic assembly at this stage, mostly directly prepare in PET, PC, Parylene, polyimides etc.
In flexible substrate, device is largely limited to substrate, i.e., can only be bent, and this strongly limits its application ranges.To
Realization is really extending to be distorted, then must pass through extremely complex stripping, the preparation of transfer step and inorganic flexible device
Equally there is higher difficulty of processing and larger danger.Such method needs higher technology, and application range is relatively narrow,
It is with high costs.Meanwhile multi-layer compound film function element has huge development prospect due to its significant multi-functional characteristic,
However laminated film middle level generally requires different micro-structure processing technologys from layer, this makes the lithography of laminated film and turns
Print still faces huge challenge.
Invention content
In view of the problems of the existing technology, the present invention proposes a kind of extendable buckling structure organic film function element
And preparation method thereof, this preparation method is easy to operate effectively, and safety and environmental protection is of low cost, flexible and changeable, and processing temperature is low, answers
With wide scope, and it can be used for the preparation of multilayer complex functional thin film flexible electronic device.
The invention is realized by the following technical scheme：
A kind of extendable buckling structure organic film function element is three-decker, and top layer is Au electrodes, and middle layer is organic
Functional layer, bottom are Au electrodes.The organic function layer can be the various organic layers needed according to application, be preferably P3HT/
PVDF-TrFE, PVDF-TrFE, P3HT or PVDF-TrFE-CFE.
The preparation method of above-mentioned extendable buckling structure organic film function element, includes the following steps：
（1）Solution is prepared：Prepare PVA and organic function layer solution；
（2）It is prepared by sacrificial layer：On clean glass substrate, PVA layers are prepared with spin-coating method, 1000 ~ 3000 r/ of spin coating rotating speed
Min, 90 ~ 180 s of time so that PVA layers of thickness control is in 200 ~ 400 nm.When thinner thickness, PVA film can be caused not connect
Continue or limit its lateral rate of dissolution, subsequent technique can not carry out；When thickness is thicker, difference is spent in surfacing, after being unfavorable for
The preparation of continuous metal, functional layer, and when follow-up water-bath removal sacrificial layer, PVA has certain residual, influences device performance；
（3）It is prepared by bottom electrode：Using hot evaporation method, evaporation rate is 0.4 ~ 0.5/s, according to device need on PVA film
It wants, the Au electrodes of different pattern is deposited, Au thickness of electrode is 40 ~ 60 nm.Au electrodes are excessively thin, are not turned on and easy fracture, blocked up
Then fold can occur in buckling or subsequent spreading process and waste precious metal material.Hot evaporation method vapor deposition is equal
Even densification, and processing temperature is low will not damage PVA film, unusable electron beam evaporation, ion sputtering or magnetron sputtering etc. easily make
Film temperature is excessively high or the preparation method of physical damnification is easily caused to film；
（4）It is prepared by organic function layer：It is needed according to application, the spin coating organic function layer on bottom Au electrodes, and to organic functions
Layer is heat-treated；
（5）It is prepared by top layer electrode：The Au top layer electrodes for being prepared 40 ~ 60 nm using hot evaporation method on organic function layer, are obtained
Complete organic film function element；
（6）Device micro Process：Organic film function element is fixed on to the workbench of high precision position moving stage, is walked by high-precision
Stepper motor control platform moves along the x-axis, and is cut in Y direction with glass cutter, organic film function element is processed
For required structure；
（7）Device is removed：PDMS is sticked on the active position of organic film function element, is soaked in 90 ~ 95 DEG C super
In pure water；It is calculated according to effective area, soaking time is with 12h/cm2It is advisable（I.e.：With 1cm2The device of effective pattern area, needs
Impregnate 12h）.PVA sacrificial layers fully dissolve, and the glutinous organic film function element for having PDMS is finally made to be taken off from glass substrate
It falls；
（8）Transfer：By the flexible substrate Ecoflex of pre-stretching ultraviolet lights 6 ~ 15 minutes, organic film function element
It is transferred on Ecoflex, extraction electrode, unloading can be obtained extendable buckling structure organic film function element.
Compared with prior art, the present invention has the advantages that：
1, the present invention is using PVA as sacrificial layer, by controlling the in the wrong of the pre-tensioned adjustable control film of flexible substrate in transfer process
Qu Chengdu（Period and amplitude）, to make device realize the functionality of organic film and have both ductility.
2, the present invention is can dissolve with water using PVA as sacrificial layer to realize the transfer of device, nontoxic lossless,
Easy to operate, without using expensive special equipment, cost substantially reduces and environmentally friendly.The micro-structure processing technology avoids
The complex operations such as conventional preparation techniques photoetching, etching avoid, using having dangerous chemical reagent and operation, having environmental protection
With the feature of safety.
3, preparation method of the invention is independent of intermediate functional layer, and no matter functional layer is monofilm or MULTILAYER COMPOSITE
Film only needs the characteristic of functional layer that can reach preparation condition（It is not soluble in water and 100 degree in it is all relatively stable）It can implement.
4, the organic film micro-structure processing dress that the present invention is built using high-precision electric displacement platform and T-type glass cutting table
It sets, PVA sacrificial layers, organic function layer and corresponding electrode layer can be processed as required structure, machining accuracy is up to micron dimension.
Description of the drawings
Fig. 1 is the flow chart of the extending organic film function element preparation method of buckling structure of the present invention；
Fig. 2 is the SEM shape appearance figures of 2 gained flexible device of the embodiment of the present invention；
Fig. 3 is 1 gained flexible memory of embodiment of the present invention I under stretching conditiondsResponse curve；
Fig. 4 is the I under light illumination of 1 gained flexible memory of the embodiment of the present inventiondsResponse curve；
Fig. 5 is the I under different grid voltages of 1 gained flexible memory of the embodiment of the present inventiondsResponse curve.
Specific implementation mode
Embodiment 1：
Configure PVA, P3HT and PVDF-TrFE solution.On clean glass substrate, 300 nm thickness are prepared with spin-coating method
PVA sacrificial layers, spin coating parameters：2000 r/min of rotating speed, 90 s of time.Mask plate is placed on PVA film, using hot evaporation side
50 nm Au source/drain electrodes, 0.4/s of evaporation rate is deposited in method.Then spin coating functional layer, one layer of P3HT of first spin coating, spin coating ginseng
Number：1000 r/min of rotating speed, 30 s of time, 60 DEG C of 1 h of drying, then one layer of PVDF-TrFE of spin coating, spin coating parameters：Rotating speed
1000 r/min, 90 s of time dry 10 min.The Au gate electrodes of 50 nm are further deposited on laminated film, to complete
The preparation of device.Device is fixed on the panel of electric precise displacement platform, device is moved to by suitable position by controller,
Film is cut according to mask plate shape with glass cutter, marks active component.After sticking PDMS on effective film position, by it
24 h in 90 DEG C of pure water are soaked in, PVA sacrificial layers fully dissolve, and make to stick the film on PDMS and are taken off from glass substrate
It falls.The film to fall off is transferred on PDMS first, exposes gate electrode, the Ecoflex of ultraviolet irradiation pre-stretching, then will fall off
Film transfer to Ecoflex on, draw gate electrode.Finally, 2 h of close annealing is dried at 120 DEG C.Grid, source, drain electrode are connected
It is connected to characteristic of semiconductor analyzer corresponding port, the current-responsive under the conditions of test Mechanical loading, illumination etc..
Embodiment 2：
Configure PVA and PVDF-TrFE solution.On clean glass substrate, the PVA that 400 nm thickness are prepared with spin-coating method sacrifices
Layer, spin coating parameters：1500 r/min of rotating speed, 180 s of time.Using hot evaporation method, 0.5/s of evaporation rate, in PVA film
The Au electrodes of 40 nm thickness on upper vapor deposition.Then spin coating PVDF-TrFE functional layers, spin coating parameters：3000 r/min of rotating speed, when
Between 90 s, 60 DEG C drying 10 min.Device is fixed on the panel of electric precise displacement platform, is moved device by controller
Suitable position is moved, is moved by high-precision controllor for step-by-step motor part, glass cutter is used in combination to be cut into apart from equal on film
Line segment, and the PDMS sticked, then be soaked in 60 h in 92 DEG C of pure water, PVA sacrificial layers fully dissolve, and make to stick
Film on PDMS falls off from glass substrate.The Ecoflex of ultraviolet irradiation pre-stretching, then extremely by the film transfer to fall off
On Ecoflex, hearth electrode is drawn.Finally, 2 h of close annealing is dried at 120 DEG C.
Embodiment 3：
Configure PVA and P3HT solution.On clean glass substrate, the PVA sacrificial layers of 200 nm thickness, rotation are prepared with spin-coating method
Apply parameter：4000 r/min of rotating speed, 90 s of time.Then one layer of P3HT functional layer of spin coating, spin coating parameters：2000 r/ of rotating speed
Min, 30 s of time, 60 DEG C of 10 min of drying.Using hot evaporation method, 0.3/s of evaporation rate is placing mask plate
The Au that thickness 60 nm, 0.3 mm of diameter are deposited on PVA film justifies electrode.Then device is fixed on to the face of electric precise displacement platform
It on plate, is moved by controller plc part, film is divided equally into 4 fractions with glass cutter, and stick respectively
PDMS, then be soaked in 12 h in 90 DEG C of pure water, PVA sacrificial layers fully dissolve, and make to stick film on PDMS from glass
It falls off on glass substrate.The Ecoflex of ultraviolet irradiation pre-stretching, then will be on the film transfer to Ecoflex that fallen off.Finally, 125
DEG C dry close annealing 2 h.
Embodiment 4：
Configure PVA and PVDF-TrFE-CFE solution.On clean glass substrate, the PVA of 300 nm thickness is prepared with spin-coating method
Sacrificial layer, spin coating parameters：2000 r/min of rotating speed, 180 s of time.Upper 40 nm is deposited on PVA film using hot evaporation method
Thick Au electrodes, 0.5/s of evaporation rate.Then spin coating PVDF-TrFE-CFE functional layers, spin coating parameters：3000 r/ of rotating speed
Min, 90 s of time, 60 DEG C of 10 min of drying.Then device is fixed on the panel of electric precise displacement platform, passes through control
Device control device moves, the PDMS for being cut into equidistant line segment on film with glass cutter, and sticking, then is soaked in
48 h in 90 DEG C of pure water, PVA sacrificial layers fully dissolve, and make to stick the film on PDMS and fall off from glass substrate.Ultraviolet photograph
The Ecoflex of pre-stretching is penetrated, then by the film transfer to Ecoflex to fall off, draws hearth electrode.Finally, in 120 DEG C of baking ovens
2 h of middle annealing.
Claims (3)
1. a kind of extendable buckling structure organic film function element, it is characterised in that it is three-decker, top layer is Au electrodes,
Middle layer is organic function layer, and bottom is Au electrodes.
2. extendable buckling structure organic film function element as described in claim 1, it is characterised in that organic work(
Ergosphere is P3HT/PVDF-TrFE, PVDF-TrFE, P3HT or PVDF-TrFE-CFE.
3. the preparation method of extendable buckling structure organic film function element described in claim 1, it is characterised in that including
Following steps：
（1）Solution is prepared：Prepare PVA and organic function layer solution；
（2）It is prepared by sacrificial layer：On clean glass substrate, PVA layers are prepared with spin-coating method, 1000 ~ 3000 r/ of spin coating rotating speed
Min, 90 ~ 180 s of time so that PVA layers of thickness control is in 200 ~ 400 nm；
（3）It is prepared by bottom electrode：Using hot evaporation method, evaporation rate is 0.4 ~ 0.5/s, according to device on PVA film layer
It needs, the Au electrodes of different pattern is deposited, Au thickness of electrode is 40 ~ 60 nm；
（4）It is prepared by organic function layer：It is needed according to application, the corresponding organic function layer of spin coating on bottom Au electrodes, and to having
Machine functional layer is heat-treated；
（5）It is prepared by top layer electrode：The Au top layer electrodes for being prepared 40 ~ 60 nm using hot evaporation method on organic function layer, are obtained
Complete organic film function element；
（6）Device micro Process：Organic film function element is fixed on to the workbench of high precision position moving stage, is walked by high-precision
Stepper motor control platform moves along the x-axis, and is cut in Y direction with glass cutter, organic film function element is processed
For required structure；
（7）Device is removed：PDMS is sticked on the active position of organic film function element, is soaked in 90 ~ 95 DEG C super
In pure water；PVA sacrificial layers fully dissolve, and finally making to stick has the organic film function element of PDMS to fall off from glass substrate；
（8）Transfer：By the flexible substrate Ecoflex of pre-stretching ultraviolet lights 6 ~ 15 minutes, organic film function element
It is transferred on Ecoflex, extraction electrode, unloading can be obtained extendable buckling structure organic film function element.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109285946A (en) * | 2018-11-19 | 2019-01-29 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of the transferable electronic device of flexibility |
| CN110251281A (en) * | 2019-06-24 | 2019-09-20 | 华中科技大学 | A kind of preparation method and products thereof of flexible electronic skin |
| CN110620166A (en) * | 2019-08-26 | 2019-12-27 | 合肥工业大学 | Method for preparing ultra-flexible optical detector on neutral plane with zero stress |
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| CN105405983A (en) * | 2015-12-14 | 2016-03-16 | 吉林大学 | Stretching organic electroluminescence device with periodically regular crease structure |
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